Establishment and maintenance of low gas pressure within interior spaces of temperature-stabilized storage systems

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Methods and apparatus described herein relate to establishing and maintaining low gas pressure within a gas-sealed device fabricated from heat sensitive materials. Methods include transferring activated getters within the interior of an apparatus from regions fabricated from heat-resistant materials to interior regions of the gas-sealed device fabricated from heat-sensitive materials.

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Description
CROSS-REFERENCE TO RELATED APPLICATIONS

The present application is related to and claims the benefit of the earliest available effective filing date(s) from the following listed application(s) (the “Related applications”) (e.g., claims earliest available priority dates for other than provisional patent applications or claims benefits under 35 USC §119(e) for provisional patent applications, for any and all parent, grandparent, great-grandparent, etc. applications of the Related application(s)). All subject matter of the Related applications and of any and all parent, grandparent, great-grandparent, etc. applications of the Related applications, including any priority claims, is incorporated herein by reference to the extent such subject matter is not inconsistent herewith.

RELATED APPLICATIONS

    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/001,757, entitled TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Dec. 11, 2007, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/006,088, entitled TEMPERATURE-STABILIZED STORAGE CONTAINERS WITH DIRECTED ACCESS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Dec. 27, 2007, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/006,089, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Dec. 27, 2007, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/008,695, entitled TEMPERATURE-STABILIZED STORAGE CONTAINERS FOR MEDICINALS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Jan. 10, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/012,490, entitled METHODS OF MANUFACTURING TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Jan. 31, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/077,322, entitled TEMPERATURE-STABILIZED MEDICINAL STORAGE SYSTEMS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William Gates; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Mar. 17, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/152,465, entitled STORAGE CONTAINER INCLUDING MULTI-LAYER INSULATION COMPOSITE MATERIAL HAVING BANDGAP MATERIAL AND RELATED METHODS, naming Jeffrey A. Bowers; Roderick A. Hyde; Muriel Y. Ishikawa; Edward K. Y. Jung; Jordin T. Kare; Eric C. Leuthardt; Nathan P. Myhrvold; Thomas J. Nugent Jr.; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood Jr. as inventors, filed May 13, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/152,467, entitled MULTI-LAYER INSULATION COMPOSITE MATERIAL INCLUDING BANDGAP MATERIAL, STORAGE CONTAINER USING SAME, AND RELATED METHODS, naming Jeffrey A. Bowers; Roderick A. Hyde; Muriel Y. Ishikawa; Edward K. Y. Jung; Jordin T. Kare; Eric C. Leuthardt; Nathan P. Myhrvold; Thomas J. Nugent Jr.; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood Jr. as inventors, filed May 13, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/220,439, entitled MULTI-LAYER INSULATION COMPOSITE MATERIAL HAVING AT LEAST ONE THERMALLY-REFLECTIVE LAYER WITH THROUGH OPENINGS, STORAGE CONTAINER USING SAME, AND RELATED METHODS, naming Roderick A. Hyde; Muriel Y. Ishikawa; Jordin T. Kare; and Lowell L. Wood, Jr. as inventors, filed Jul. 23, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/658,579, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William Gates; Zihong Guo; Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Feb. 8, 2010, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/927,981, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS WITH FLEXIBLE CONNECTORS, naming Fong-Li Chou; Geoffrey F. Deane; William Gates; Zihong Guo; Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Nov. 29, 2010, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/927,982, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS INCLUDING STORAGE STRUCTURES CONFIGURED FOR INTERCHANGEABLE STORAGE OF MODULAR UNITS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William Gates; Jenny Ezu Hu; Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Nov. 29, 2010, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 13/135,126, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS CONFIGURED FOR STORAGE AND STABILIZATION OF MODULAR UNITS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William Gates; Jenny Ezu Hu; Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Mark K. Kuiper; Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene; Mike Vilhauer; Charles Whitmer; Lowell L. Wood, Jr.; and Ozgur Emek Yildirim as inventors, filed Jun. 23, 2011, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.
    • For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 13/199,439, entitled METHODS OF MANUFACTURING TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Aug. 29, 2011, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.

The United States Patent Office (USPTO) has published a notice to the effect that the USPTO's computer programs require that patent applicants reference both a serial number and indicate whether an application is a continuation, continuation-in-part, or divisional of a parent application. Stephen G. Kunin, Benefit of Prior-Filed Application, USPTO Official Gazette Mar. 18, 2003. The present Applicant Entity (hereinafter “Applicant”) has provided above a specific reference to the application(s) from which priority is being claimed as recited by statute. Applicant understands that the statute is unambiguous in its specific reference language and does not require either a serial number or any characterization, such as “continuation” or “continuation-in-part,” for claiming priority to U.S. patent applications. Notwithstanding the foregoing, Applicant understands that the USPTO's computer programs have certain data entry requirements, and hence Applicant has provided designation(s) of a relationship between the present application and its parent application(s) as set forth above, but expressly points out that such designation(s) are not to be construed in any way as any type of commentary and/or admission as to whether or not the present application contains any new matter in addition to the matter of its parent application(s).

SUMMARY

Apparatus described herein include, but are not limited to: a structural region fabricated from a heat-sensitive material, the structural region including an outer wall and an inner wall with a gas-sealed gap between the outer wall and the inner wall; an activation region fabricated from a heat-resistant material, the activation region including one or more getters; a connector attached to the structural region and to the activation region, the connector including a flexible region and a region configured for sealing and detachment of the structural region from the activation region; and a vacuum pump operably attached to the connector.

Methods described herein include, but are not limited to: establishing vacuum within a gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions; heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established vacuum within the gas-sealed apparatus; allowing the at least one activation region and the one or more getters to cool to a temperature compatible with structural stability of the heat-sensitive material; transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the apparatus; and separating the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters. Methods of establishing and maintaining vacuum within a storage device also include, but are not limited to: assembling substantially all structural components of a storage device, including an outer wall and an inner wall substantially defining a gas-sealed gap; attaching the storage device to a gas-sealed apparatus, the gas-sealed apparatus including a getter activation region containing one or more getters, a vacuum pump, and a connector operably connecting the storage device to the gas-sealed apparatus; activating the vacuum pump to establish gas pressure below atmospheric pressure within the gas-sealed gap of the storage device; heating the storage device to a predetermined temperature for a predetermined length of time; heating the getter activation region and the one or more getters to an activation temperature for an activation time suitable to activate one or more getters within the at least one getter activation region, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device; allowing the getter activation region and the one or more getters to cool to a predetermined temperature; flexing the connector to move the storage device and the getter activation region into a relative position wherein the getter activation region is above the storage device and the connector is substantially linear; allowing the getters to fall along the connector interior into the gas-sealed gap in the storage device, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device; separating the connector at a location adjacent to the storage device while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. In addition to the foregoing, other method aspects are described in the claims, drawings, and text forming a part of the present disclosure.

In addition to the foregoing, other aspects are described in the claims, drawings, and text forming a part of the present disclosure. The foregoing summary is illustrative only and is not intended to be in any way limiting. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features will become apparent by reference to the drawings and the following detailed description.

BRIEF DESCRIPTION OF THE FIGURES

FIG. 1 is a schematic of an apparatus.

FIG. 2 is a schematic of an apparatus such as that illustrated in FIG. 1.

FIG. 3 is a schematic of an apparatus such as that depicted in FIGS. 1 and 2.

FIG. 4 is a schematic of an apparatus such as that depicted in FIGS. 1, 2 and 3.

FIG. 5 depicts a flowchart of a method.

FIG. 6 illustrates a flowchart of a method.

FIG. 7 shows a flowchart of a method such as illustrated in FIG. 6.

FIG. 8 depicts a flowchart of a method such as illustrated in FIG. 6.

FIG. 9 illustrates a flowchart of a method such as illustrated in FIG. 6.

FIG. 10 shows a flowchart of a method such as illustrated in FIG. 6.

FIG. 11 depicts a flowchart of a method such as illustrated in FIG. 6.

FIG. 12 illustrates a flowchart of a method such as illustrated in FIG. 6.

FIG. 13 shows a flowchart of a method such as illustrated in FIG. 6.

FIG. 14 depicts a flowchart of a method such as illustrated in FIG. 6.

FIG. 15 illustrates a flowchart of a method such as illustrated in FIG. 6.

FIG. 16 illustrates a flowchart of a method.

FIG. 17 shows a flowchart of a method such as illustrated in FIG. 16.

FIG. 18 depicts a flowchart of a method such as illustrated in FIG. 16.

FIG. 19 illustrates a flowchart of a method such as illustrated in FIG. 16.

FIG. 20 shows a flowchart of a method such as illustrated in FIG. 16.

FIG. 21 depicts a flowchart of a method such as illustrated in FIG. 16.

FIG. 22 illustrates a flowchart of a method such as illustrated in FIG. 16.

FIG. 23 is a schematic of a storage container.

 DETAILED DESCRIPTION

In the following detailed description, reference is made to the accompanying drawings, which form a part hereof. In the drawings, similar symbols typically identify similar components, unless context dictates otherwise. The illustrative embodiments described in the detailed description, drawings, and claims are not meant to be limiting. Other embodiments may be utilized, and other changes may be made, without departing from the spirit or scope of the subject matter presented here.

The use of the same symbols in different drawings typically indicates similar or identical items.

Methods and apparatus described herein are useful to establish and maintain a stable and extremely low gas pressure within an internal, gas-sealed region of a container. Methods and apparatus as described herein have a variety of potential uses in the manufacture of containers that include internal, gas-sealed regions with durable gas pressure below atmospheric pressure, such as near-vacuum gas pressure, without active pumping of gas out of the internal gas-sealed regions. Methods and apparatus described herein may be utilized to establish and maintain a durable low gas pressure region internal to a container structure, and may be particularly useful in regard to containers fabricated from materials that lose their structural stability at temperatures below the activation temperatures required by many getter materials. For example, the methods and apparatus as described herein may be utilized to establish and maintain a stable gas pressure below atmospheric pressure, such as near-vacuum gas pressure, within an internal, gas-sealed cavity within a portion of a larger device fabricated all or in part from aluminum. For example, the methods and apparatus as described herein may be useful in the manufacture and durability of containers fabricated out of plastic-metal composites that include internal, gas-impermeable spaces with gas pressure less than that of the environment surrounding the container, such as substantially evacuated, gas-impermeable internal spaces.

Internal, gas-sealed regions with low gas pressure may be incorporated into the structure of containers as part of the insulation for the container. Internal, gas-sealed regions of low gas pressure incorporated into the structure of containers as partial insulation for the container may include other materials or features, such as insulation materials, electronics or structural features of the container. For example, internal, gas-sealed regions of low gas pressure incorporated into the structure of a container may include multilayer insulation material (MLI). For example, internal, gas-sealed regions of low gas pressure incorporated into the structure of a container may include wires or conduits connecting electronic components operably attached to different regions of the container. Internal, gas-sealed regions of low gas pressure may also isolate electronics incorporated into the device from external factors, such as chemically active materials, magnetically active materials, water, heat and cold. For example, internal, gas-sealed regions of low gas pressure incorporated into the structure of a container may include structural elements such as flanges, supports, struts and other features improving the structural stability of the container. Internal, gas-sealed regions of low pressure may have advantages of low weight and cost in a finished, manufactured device. Methods and apparatus described herein may be used to manufacture substantially thermally sealed storage devices, such as those suitable for stable maintenance of stored materials within a predetermined temperature range without reliance on external power sources to maintain the temperature range within the storage area. For example, containers and devices such as those manufactured with the methods and apparatus described herein are suitable for maintenance of stored materials within a predetermined temperature range in locations with minimal municipal power, or unreliable municipal power sources, such as remote locations or in emergency situations. For example, containers and devices such as those manufactured with the methods and apparatus described herein may be useful for the transport and storage of materials that are sensitive to external temperature changes that can occur during shipment and storage. For example, the storage systems described herein are useful for the shipment and storage of medicinal agents, including vaccines.

Many medicinal agents, including vaccines, currently in regular use are highly sensitive to temperature variations, and must be maintained in a particular temperature range to preserve stability, as well as the potency and efficacy of the medicinal agents. The temperature range to maintain stability in storage is inherent to the particular formulation and medicinal agent. For example, many medicinal agents, including vaccines, must be stored in a predetermined temperature range, such as between 2 degrees Centigrade and 8 degrees Centigrade, or between 0 degrees Centigrade and 10 degrees Centigrade, or between 10 degrees Centigrade and 15 degrees Centigrade, or between 15 degrees Centigrade and 25 degrees Centigrade, or between −15 degrees Centigrade and −5 degrees Centigrade, or between −50 degrees Centigrade and −15 degrees Centigrade, to preserve efficacy of the medicinal agent. Storage and transport of medicinal agents, including vaccines, within a temperature range, such as between 2 degrees Centigrade and 8 degrees Centigrade, or between 0 degrees Centigrade and 10 degrees Centigrade, or between 10 degrees Centigrade and 15 degrees Centigrade, or between 15 degrees Centigrade and 25 degrees Centigrade, or between −15 degrees Centigrade and −5 degrees Centigrade, or between −50 degrees Centigrade and −15 degrees Centigrade, is often referred to as the “cold chain.”

Health care providers and clinics who use medicinal agents, such as vaccines, must follow established protocols and procedures for maintenance of the cold chain, including during transport and in times of emergency and in power failures, to ensure medicinal agent activity such as vaccine potency. See: Rodgers et al., “Vaccine Cold Chain Part 1 Proper Handling and Storage of Vaccine,” AAOHN Journal 58(8) 337-344 (2010); Rodgers et al., “Vaccine Cold Chain Part 2: Training Personnel and Program Management,” AAOHN Journal 8(9): 391-402 (2010); Magennis et al., “Pharmaceutical Cold Chain” A Gap in the Last Mile,” Pharmaceutical & Medical Packaging News, 44-50 (September 2010); and Kendal et al., “Validation of Cold Chain Procedures Suitable for Distribution of Vaccines by Public Health Programs in the USA,” Vaccine 15 (12/13): 1459-1465 (1997) which are each incorporated by reference. For example, failure to follow established protocols and procedures for maintenance of the cold chain, even during periods of normal use in developed countries, leads to significant levels of vaccine wastage due to exposure to both excessively high and excessively low temperatures. In some cases, a brief period outside of normal storage temperatures is sufficient to disrupt activity. See: Thakker and Woods, “Storage of Vaccines in the Community: Weak Link in the Cold Chain?” British Medical Journal 304: 756-758 (1992); Matthias et al., “Freezing Temperatures in the Vaccine Cold Chain: A Systematic Literature Review,” Vaccine 25: 3980-3986 (2007); Edsam et al., “Exposure of Hepatitis B Vaccine to Freezing Temperatures During Transport to Rural Health Centers in Mongolia,” Preventative Medicine 39: 384-388 (2004); Techathawat et al., “Exposure to Heat and Freezing in the Vaccine Cold Chain in Thailand,” Vaccine 25: 1328-1333 (2007); and Setia et al., “Frequency and Causes of Vaccine Wastage,” Vaccine 20: 1148-1156 (2002), which are each incorporated by reference. Although some breaks in cold chain maintenance, such as frozen vaccine vials and vials containing precipitants due to improper temperature exposure, may be readily apparent, medicinal agents such as vaccines with reduced potency due to breaks in cold chain maintenance may not be readily detectable. See: Chen et al., “Characterization of the Freeze Sensitivity of a Hepatitis B Vaccine,” Human Vaccines 5(1): 26-32 (2009), which is incorporated by reference. Medicinal agent stocks with reduced potency or efficacy due to exposure to excessively high temperatures may not be immediately identifiable. The temperature sensitivity of any given medicinal agent varies widely depending on the specific agent, or example the specific vaccine formulation. In some circumstances, a few minutes outside of the appropriate temperature range can significantly impact the biological effectiveness of a particular container of a medicinal agent. See: Kristensen and Chen, “Stabilization of Vaccines: Lessons Learned,” Human Vaccines 6(3): 229-230 (2010), which is incorporated by reference. Issues related to the maintenance of cold chain are even more significant in less well developed regions of the world. See: Wirkas et al., “A Vaccine Cold Chain Freezing Study in PNG Highlights Technology Needs for Hot Climate Countries,” Vaccine 25: 691-697 (2007); and Nelson et al., “Hepatitis B Vaccine Freezing in the Indonesian Cold Chain: Evidence and Solutions,” Bulletin of the World Health Organization, 82(2): 99-105 (2004), which are each incorporated by reference. In addition, approaches to the cold chain that require less energy may be desirable for ongoing cost and climate considerations. See Halldórsson and Kovacs, “The Sustainable Agenda and Energy Efficiency: Logistics Solutions and Supply Chains in Times of Climate Change,” International Journal of Physical Distribution & Logistics Management 40 (1/2): 5-13 (2010), which is incorporated by reference. Thermal stabilization of medicinal agents, such as vaccines, for use beyond the cold chain includes economic, logistical, regulatory, procurement and policy issues (see Kristensen and Chen, “Stabilization of vaccines: lessons learned,” Human Vaccines, vol. 6, no. 3, March 2010, pages 229-231, which is incorporated by reference).

Containers and storage devices such as those fabricated using methods and apparatus described herein may be designed in a variety of sizes and shapes, depending on the embodiment. For example, containers and storage devices may be fabricated in various sizes, shapes and materials depending on the intended use of the container or storage device. A representative example of a storage container is shown in FIG. 23 and described in the associated text (see below). For example, containers and storage devices manufactured using the methods and apparatus described herein may be of a shape and size for convenient portability, such as no more than 1 kilogram (kg), 2 kg, 5 kg, 7 kg or 10 kg. For example, containers and storage devices manufactured using the methods and apparatus described herein may be of a size and shape to be carried easily by an individual person, either directly or with a carrier, such as with a satchel, duffle bag, rucksack, carryall, handbag, haversack, knapsack, pack, pouch, suitcase, tote, travel bag or backpack. For example, containers and storage devices may be fabricated in a shape and size for transport using a small wheeled conveyance operated by a single person, such as with a mass of no more than 15 kg, 20 kg, or 25 kg. For example, containers and storage devices manufactured using the methods and apparatus described herein may be of a size and shape to be carried easily by a person using a handcart, a rickshaw, a gurney, a bicycle or a motorcycle, such as in a saddlebag, carrier or rack. For example, containers and storage devices may be fabricated in a shape and size for transport using a truck, wagon, pickup, van or other motorized delivery vehicle, such as with a mass of no more than 30 kg, 35 kg, 40 kg, 45 kg, 50 kg or 55 kg. For example, containers and storage devices may be fabricated in a shape and size for substantially stationary use, for example with a mass of greater than 100 kg.

Apparatus

With reference now to FIG. 1, shown is an example of an apparatus that may serve as a context for the subject matter described herein. FIG. 1 illustrates a schematic of an apparatus 185. The apparatus 185 includes a structural region 180, an activation region 100, a connector 120 attached to the structural region 180 and to the activation region 100, and a vacuum pump 130. Each of the structural region 180, the activation region 100, the connector, and the vacuum pump 130 includes an internal, gas-sealed region. For example, the structural region 180 includes a gas-sealed gap 145 between the outer wall 150 and the inner wall 155. The entire apparatus 185 includes an internal, gas-sealed region that is contiguous throughout the regions (e.g. 100, 120, 145) of the apparatus 185.

The structural region 180 is fabricated from a heat-sensitive material. The structural region 180 may be fabricated entirely or in part from a heat-sensitive material. The structural region 180 may be fabricated from a combination of materials. Wherein the structural region includes components fabricated from different materials, the material with the lowest heat tolerance will govern the heat-sensitivity of the entire structural region 180. The structural region 180 includes an outer wall 150 and an inner wall 155, with a gas-sealed gap 145 between the outer wall 150 and the inner wall 155. The activation region 100 is fabricated from a heat-resistant material. The activation region 100 is entirely fabricated from a heat-resistant material utilizing methods that are also heat-resistant. For example, any epoxy, seals, coatings or similar components within the activation region 100 structure will be heat-resistant. Wherein the activation region includes components fabricated from different materials, the material with the lowest heat tolerance will govern the heat-resistance of the entire activation region 100. The activation region 100 includes one or more getters 110.

The connector 120 is attached to both the structural region 180 and the activation region 100. The connector 120 is operably connected to both the structural region 180 and the activation region 100 with gas-impermeable connections to form a gas-sealed interior. For example, the connector 120 may be attached to the structural region 180 and the activation region 100 using gas-impermeable seals on the respective ends of the connector 120. For example, the connector 120 may be welded on to the structural region 180 and the activation region 100 on the respective ends of the connector 120 to form a gas-impermeable welding joint. The connector 120 includes a flexible region 125. The connector includes a region 127 configured for sealing and detachment of the structural region 180 from the activation region 100. The vacuum pump 130 is operably attached to the connector 120. The vacuum pump 130 is operably attached to the connector 120 to allow the vacuum pump 130 to substantially evacuate the gas within the gas-sealed interior of the apparatus 185 during utilization of the methods described herein. In some embodiments, the vacuum pump 130 may be operably attached to the connector 120 through a tube, duct, conduit or other structure that creates a gas-impermeable seal between the vacuum pump 130 and the connector 120. FIG. 1, for example, illustrates the vacuum pump 130 as operably attached to the connector 120 through a conduit 170.

The apparatus 185 includes a gas-sealed interior region throughout the structural region 180, the activation region 100, and the connector 120 attached to the structural region 180 and to the activation region 100. Gas-impermeable seals are located in each of the junctions between regions 180, 100 of the apparatus 185 and the connector. The vacuum pump 130 is also operably attached to the connector 120 with a gas-impermeable seal. See: Ishimaru, “Bakable aluminum vacuum chamber and bellows with an aluminum flange and metal seal for ultrahigh vacuum,” Journal of Vacuum Science and Technology, vol. A15, no. 6, November/December 1978, pages 1853-1854; and Jhung et al., “Achievement of extremely high vacuum using a cryopump and conflate aluminum gaskets,” Vacuum, vol. 43, no. 4, 1992, pages 309-311; which are each incorporated by reference. The vacuum pump 130 may be attached to the connector 120 through a through a structure, such as conduit 170, that includes a gas-impermeable seal between the vacuum pump 130 and the connector 120. The vacuum pump 130 included in a specific embodiment should have sufficient pumping capacity to substantially evacuate the entirety of the gas-sealed interior region throughout the structural region 180, the activation region 100, and the connector 120 attached to the structural region 180 and to the activation region 100.

A valve 135 may be operably attached to the connector 120, for example in the region of the connector 120 between the attached vacuum pump 130 and conduit 170 and the attached structural region 180. A valve 135 operably attached to the connector 120 may be configured to inhibit the flow of gas through the connector 120. A valve 135 operably attached to the connector 120 may be configured to block the flow of gas through the connector 120. A valve 135 operably attached to the connector 120 is configured to restrict gas flow through the interior of the connector 120 at a location along the length of the connector 120. For example, as illustrated in FIG. 1, a valve 135 may be configured to prevent gas flow between the gas-sealed gap 145 in the structural region 180 from the flexible region 125 of the connector 120, and the interior of the activation region 100. As an example, as illustrated in FIG. 1, a valve 135 may be integrated into the connector 120 and configured to reversibly prevent the flow of gas within the interior of the connector 120. A valve 135 may be configured to isolate gas present in one region of the interior of the apparatus 185 from another region of the interior of the apparatus 185. A valve 135 may be of a number of types, as appropriate to the embodiment and relative to factors such as cost, size, durability, structural strength, outgassing of fabrication materials, and sealing strength. A valve 135 may be a quarter-turn valve, such as a butterfly style valve. A valve 135 may be a ball valve. In some embodiments, there may be a plurality of valves. If a valve 135 includes organic materials, such as nitrile, in “O” rings or other components, the expected outgassing rate of the value components should be understood to effect the time required to achieve a target minimal gas pressure within the apparatus. See: L. de Csernatony, “The properties of Viton “A” elastomers II: the influence of permeation, diffusion and solubility of gases on the gas emission rate from an O-ring used as an atmospheric seal or high vacuum immersed,” Vacuum, vol. 16, no. 3, 1965, pages 129-134, which is incorporated by reference. In some embodiments, baking the value under vacuum conditions prior to assembly of the apparatus (e.g. see FIG. 5 and associated text) may reduce outgassing from organic materials within the valve. See: D. J. Crawley and L. de Csernatony, “Degassing characteristics of some ‘O’ ring materials,” Vacuum, vol. 14, 1964, pages 7-9; and S. Rutherford, “The benefits of Viton outgassing,” Duniway Stockroom Corp., 1997, pages 1-5, which are each incorporated by reference.

The structural region 180 fabricated from a heat-sensitive material includes a device configured for use independently from the remainder of the apparatus. For example, the structural region 180 may include a storage device (see, e.g. FIG. 23) configured for use independently from the remainder of the apparatus. For example, the structural region 180 may include a storage device (see, e.g. FIG. 23) configured for use independently from the connector 120, the vacuum pump 130 and the activation region 100. For example, the structural region 180 may include a substantially thermally sealed container configured for use independently from the connector 120, the vacuum pump 130 and the activation region 100. In some embodiments, the structural region 180 includes a device configured for detachment from the remainder of the apparatus. In some embodiments, the structural region 180 includes a storage device. In some embodiments, the structural region 180 includes a storage device configured for temperature-stabilized storage. In some embodiments, the structural region 180 includes a thermally-insulated device. The structural region 180 may include a storage device with an interior storage region 165 and an opening 160 in the structural region 180 of a suitable size and shape to maintain the thermal storage properties of the interior storage region 165 and to allow for the addition and removal of any stored material within the interior storage region 165. The interior storage region 165 is a substantially thermally sealed storage region containing an access opening 160 of minimal size and shape to allow insertion and removal of stored material from the interior storage region 165. The storage device may include a container, such as a thermally-stabilized container (see, e.g. FIG. 23) designed for storage of medicinal agents within the cold chain. As illustrated in FIG. 1, the structural region 180 may have an attached gas pressure gauge 140, configured to detect and signal the gas pressure within the gas-sealed gap 145. See: Mukugi et al., “Characteristics of cold cathode gauges for outgassing measurements in uhv range,” Vacuum, vol. 44, nos. 5-7, 1993, pages 591-593; and Saitoh et al., “Influence of vacuum gauges on outgassing rate measurements,” Journal of Vacuum Science and Technology, vol. A11, no. 5, September/October 1993, pages 2816-2821; Hong et al., “Investigation of gas species in a stainless steel ultrahigh vacuum chamber with hot cathode ionization gauges,” Meas. Sci. Technol., vol. 15, 2004, pages 359-364; which are each incorporated by reference. The gas pressure gauge 140 may be operably attached to the gas-sealed gap 145 through a tube or duct 175. Although not illustrated in FIG. 1, in some embodiments a valve may be included in or on the duct 175 to inhibit the flow of gas through the duct 175 and to isolate the gas-sealed gap 145 from the gas pressure gauge 140.

The structural region 180 fabricated from a heat-sensitive material may be fabricated from a variety of heat-sensitive materials, depending on the embodiment. The structural region 180 may be fabricated to include a single heat-sensitive material. The structural region 180 fabricated from a heat-sensitive material may be fabricated from a plurality of materials, one or more of which may be heat-sensitive, depending on the embodiment. For example, the structural region 180 may be fabricated partially or entirely from aluminum. The structural region 180 may include a plurality of materials in a particular embodiment. The structural region 180 may be fabricated from composite materials. For example, the structural region 180 may be fabricated partially or entirely from metalized plastic, such as polypropylene, PET, nylon or polyethylene completely covered with a layer of metal, such as aluminum, on the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145. For example, the structural region 180 may be fabricated partially or entirely from plastic with a metal coating, or from plastic with a metal liner, on the interior surface of the gas-sealed gap 145 (e.g. as illustrated as surfaces 190 in FIG. 1). For example, the structural region 180 may be fabricated partially or entirely from a composite material forming a plastic interior and a metal coating covering the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145. For example, the structural region 180 may be fabricated partially or entirely from a composite material forming a plastic interior and a metal liner covering the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145. For example, the structural region 180 may be fabricated partially or entirely from materials including carbon fibers. The structural region 180 may be fabricated from different materials in layers or areas of the structural region 180, as suitable for a given embodiment. For example, the structural region 180 may be fabricated partially or entirely from a plastic exterior region with a gas-impermeable metal liner covering the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145.

In order to maintain a low gas pressure within the gas-sealed gap 145, in some embodiments the structural region 180 is fabricated entirely or partially from low vapor emitting materials. For example, the structural region 180 may be fabricated from low vapor-emitting materials such as aluminum, stainless steel, or other metals. For example, the structural region 180 may be fabricated from low vapor-emitting materials such as glass or appropriate ceramics. In order to maintain a low gas pressure within the gas-sealed gap 145, in some embodiments the structural region 180 is fabricated with a layer of low vapor emitting materials on the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145. For example, the surfaces 190 may be covered with a layer of stainless steel, aluminum, or other low vapor emitting material. In some embodiments the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145 is cleaned and treated prior to assembly to reduce the sublimation of contaminants (e.g. water, oils, or plastics) from the surfaces 190 into the gas-sealed gap 145 (see FIG. 5 and associated text herein). The specific type of low vapor emitting material used in the fabrication may be selected based on factors such as cost, weight, durability, hardness, strength, and anticipated sublimation from the surface of the particular material at the gas pressures required within the gas-sealed gap 145 and at the expected temperatures of use in a given embodiment. See, for example, Adams, “A review of the stainless steel surface,” Journal of Vacuum Science and Technology, vol. A1, no. 1, January-March 1983, pages 12-18, which is incorporated by reference. For example, in some embodiments a manufactured storage device may include a gas-sealed gap 145 with an internal gas pressure less than or equal to 1×10−2 torr. For example, in some embodiments a manufactured storage device may include a gas-sealed gap 145 with an internal gas pressure less than or equal to 5×10−4 torr. For example, in some embodiments a manufactured storage device may include a gas-sealed gap 145 with an internal gas pressure less than or equal to 1×10−2 torr. For example, in some embodiments a manufactured storage device may include a gas-sealed gap 145 with an internal gas pressure less than or equal to 5×10−4 torr. For example, in some embodiments a manufactured storage device may include a gas-sealed gap 145 with an internal gas pressure less than 1×10−2 torr, for example, less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, 5×10−6 torr or 5×10−7 torr.

The materials used to fabricate the components of the apparatus 185, as well as any treatment of the components prior to assembly of the apparatus 185 (see, e.g., FIG. 5 and associated text) will influence the rate of reduction of gas pressure within the apparatus 185 during the steps of the methods as described herein (see, e.g., FIGS. 6-22 and associated text) as well as the maintenance of the low gas pressure over time. See: R. J. Elsey, “Outgassing of vacuum materials-I,” Vacuum, vol. 25, no. 7, 1975, pages 299-306; Yamazake et al., “High-speed pumping to UHV,” Vacuum, vol. 84, 2010, pages 756-759; Saito et al., “Measurement system for low outgassing materials by switching between two pumping paths,” Vacuum, vol. 47, nos. 6-8, 1996, pages 749-752; Watanabe et al, “Reduction in outgassing rate from residual gas analyzers for extreme high vacuum measurements,” Journal of Vacuum Science and Technology, vol. A14, no. 6, November/December 1996, pages 3261-3266; Chun et al., “Effect of the Cr-rich oxide surface on fast pumpdown to ultrahigh vacuum,” Journal of Vacuum Science and Technology, vol. A15, no. 5, September/October 1997, pages 2518-2520; and Nemanic and Setina, “Outgassing of a thin wall vacuum insulating panel,” Vacuum, vol. 49, no. 3, 1998, pages 233-237; Poole and Michaelis, “Hiavac and Teflon outgassing under ultra-high vacuum conditions,” Vacuum, vol. 30, no. 10, 1980, pages 415-417; and Ishikawa and Nemanic, “An overview of methods to suppress hydrogen outgassing rate from austenitic stainless steel with reference to UHV and EXV,” Vacuum, vol. 69, 2003, pages 501-512; which are each incorporated by reference. The term “outgassing,” as used herein, refers to the evolution of gas from a solid or liquid in a vacuum or low gas pressure environment. See: Redhead, “Recommended practices for measuring and reporting outgassing data,” Journal of Vacuum Science and Technology, vol. A20, no. 5, September/October 2002, pages 1667-1675, which is incorporated by reference. The structural stability and the expected outgassing properties of the materials used to fabricate the components of the apparatus 185 during expected use of the entire apparatus 185 and any independent use of all or part of the structural region 180 should be taken into account in material selection. See: S. Choi and B. V. Sankar, “Gas permeability of various graphite/epoxy composite laminates for cryogenic storage systems,” Composites: Part B 39, 2008, pages 782-791; Engelmann et al., “Vacuum chambers in composite material,” Journal of Vacuum Science and Technology, vol. A5, no. 4, July/August 1987, pages 2337-2341; Nemanic and Setina, “Experiments with a thin-walled stainless steel chamber,” Journal of Vacuum Science and Technology, vol. A18, no. 4, July/August 2000, pages 1789-1793; Halliday, “An introduction to materials for use in vacuum,” Vacuum, vol. 37, nos. 8/9, pages 583-585, 1987; Holtrop and Hansink, “High temperature outgassing test on materials used in DIII-D tokamak,” Journal of Vacuum Science and Technology, vol. A24, no. 4, July/August 2006, pages 1572-1577; Patrick, “Outgassing and the choice of materials for space instrumentation,” Vacuum, vol. 23, no. 11, 1973, pages 411-413; Ishimaru, “Ultimate pressure of the order of 10−13 Torr in an aluminum alloy vacuum chamber,” Journal of Vacuum Science and Technology, vol. A7, no. 3, May/June 1989, pages 2437-2442; Hirohata et al., “Hydrogen desorption behavior of aluminum materials used for extremely high vacuum chamber,” Journal of Vacuum Science and Technology, vol. A11, no. 54, September/October 1993, pages 2637-2641; Ishimaru, “Aluminum alloy-sapphire sealed window for ultrahigh vacuum,” Vacuum, vol. 33, no. 6, 1983, pages 339-340; and Nemanic and Setina, “Outgassing in thin wall stainless steel cells,” Journal of Vacuum Science and Technology, vol. A17, no. 3, May/June 1999, pages 1040-1046; which are each incorporated by reference. In embodiments wherein components of the apparatus 185, such as the connector 120 and/or the structural region 180, are fabricated from a composite, such as an epoxy-containing material, the outgassing rates and associated weight loss of the components should be taken into account in estimating the time required to produce a low gas pressure within the apparatus 185 using the methods described herein (see, e.g., FIGS. 6-22 and associated text). In some situations, materials may sublimate to the extent that their structural integrity is reduced at the low gas pressures required in a specific embodiment, and such factors should be taken into account in the design of the apparatus 185 and the structural region 180. See: R. D. Brown, “Outgassing of epoxy resins in vacuum,” Vacuum, vol. 17, no. 9, 1967, pages 505-509; J. Santhanam and P. Vijendran, “Outgassing rate of reinforced epoxy and its control by different pretreatment methods,” Vacuum, vol. 28, no. 8/9, 1978, pages 365-366; and Gupta et al., “Outgassing from epoxy resins and methods for its reduction,” Vacuum, vol. 27, no. 2, 1977, pages 61-63, which are each incorporated by reference.

The term “heat-sensitive,” as used herein, refers to materials that lose their structural integrity at temperatures below the activation temperature(s) and under the activation condition(s) for the types of getter(s) 110 used in the apparatus 185. The term “heat-sensitive,” as used herein, is relative to the activation temperature(s) and the pressure conditions used for the specific getters 110 included in a given embodiment. For example, in some embodiments the getters 110 included in the apparatus 185 may include zirconium-vanadium-iron getters (see U.S. Pat. No. 4,312,669 “Non-evaporable Ternary Gettering Alloy and Method of Use for the Sorption of Water, Water Vapor and Other Gasses,” to Boffito et al., which is incorporated by reference). For example, in some embodiments the getters 110 included in the apparatus 185 may include St707™ getters with 70% zirconium, 24.6% vanadium and 5.4% iron (for example, available from Getter Technologies International Ltd., China). See also Hobson and Chapman, “Pumping of methane by St707 at low temperatures,” Journal of Vacuum and Science Technology,” vol. A4, no. 3, May/June 1986, pages 300-302, which is incorporated by reference. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature of approximately 700 degrees Centigrade for at least 20 seconds and then reducing the temperature to between approximately 400 degrees Centigrade and approximately 25 degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. A “heat-sensitive material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would be a heat-sensitive material that is predicted to lose its structural integrity in a temperature of approximately 700 degrees Centigrade lasting for at least 20 seconds. A “heat-sensitive material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would lose its structural integrity at a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. For example, in some embodiments the structural region 180 is fabricated from a heat-sensitive material that includes aluminum, or aluminum alloy that loses its structural integrity at temperatures above 250 degrees Centigrade. See: Ishimaru et al., “New all aluminum alloy vacuum system for the TRISTAN e+e− storage accelerator,” IEEE Transactions on Nuclear Science, Vol. NS-28, no. 3, 1981, pages 3320-3322, which is incorporated by reference.

The term “structural integrity,” as used herein, refers to a structure maintaining its fabricated form in a set of given conditions. Loss of structural integrity, correspondingly, refers to the failure of a structure to maintain its fabricated form in a set of conditions. “Heat-sensitive” materials, as used herein, refers to materials that lose their structural integrity at temperatures below the activation temperature(s) and under the activation condition(s) for the types of getter(s) 110 used in an embodiment of an apparatus 185. Conditions affecting loss of structural integrity may include temperature ranges, such as excessively hot or cold temperatures, and gas pressures, such as minimal gas pressure within an interior region. Conditions affecting loss of structural integrity may include conditions of intended use, such as weight-bearing, erosion, compressive strength, or tensile strength. Loss of structural integrity may be overt or gross, such as when a structure in whole or part melts, deforms, distorts, implodes, or combusts. Loss of structural integrity may include a change the outgassing properties of a material used in fabrication of a structure, for example a plastic material with low outgassing properties may exhibit increased outgassing properties in a set of given conditions, such as temperature or gas pressure. Loss of structural integrity may also be inconspicuous or undetectable to a cursory inspection, such as in the formation of a small hole, surface thinning, alteration of a crystalline or other non-overt structure of a fabricated material, or loss of cohesion at a weld or joint. For example, in some embodiments, aluminum and aluminum alloys are “heat-sensitive,” as used herein, and may lose their structural integrity in some conditions required to activate some types of getters employed in the specific embodiment. For example, although aluminum and aluminum alloys may not completely melt into a liquid form at temperatures above 250 degrees Centigrade, in some instances they will begin to soften and, as such, lose their structural integrity. Similarly, copper and copper alloys may be considered heat-sensitive materials in some embodiments. See Koyatsu et al., “Measurements of outgassing rate from copper and copper alloy chambers,” Vacuum, vol. 47, no. 6-8, 1996, pages 709-711, which is incorporated by reference. When combined with the force of gravity on the structural region 180 and any force due to a low gas pressure within the gas-sealed gap 145, aluminum and aluminum alloys at temperatures above 250 degrees Centigrade may lose their structural integrity and manufactured form and compress, shift, or bend. Similarly, plastic and plastic composites used in some embodiments may be heat sensitive materials.

As illustrated in FIG. 1, in some embodiments the inner wall 155 and the outer wall 150 of the structural region 180 together substantially define the gas-sealed gap 145. For example, the gas-sealed gap 145 may be primarily defined by the boundaries of the inner wall 155 and the outer wall 150 of the structural region 180. For example, the gas-sealed gap 145 may be substantially established by the boundaries of the inner wall 155 and the outer wall 150 of the structural region 180. Junctions between the inner wall 155 and the outer wall 150 may be, for example, welds, bonds or seals that substantially isolate the gas-sealed gap 145 from the gas environment external to the structural region 180. In some embodiments, the junctions between the inner wall 155 and the outer wall 150 may include additional material, such as welding agents, solder, brazing material or other sealing materials to establish and maintain the isolation of the gas-sealed gap 145 from the gas environment external to the structural region 180.

In some embodiments, the gas-sealed gap 145 includes additional material. In some embodiments, the gas-sealed gap 145 includes additional material designed to improve the durability and stability of the structural region 180. For example, the gas-sealed gap 145 may include structural features, such as one or more flanges, struts, braces, crossbars, or posts that may be configured to maintain the stability of the structural region 180. For example, the gas-sealed gap 145 may include internal support structure, such as reinforced regions of the inner wall 155 and the outer wall 150.

In some embodiments, the gas-sealed gap 145 includes additional insulating material that improves the thermal properties of the structural region 180. For example, the gas-sealed gap 145 may include multilayer insulation material (MU). See: Wiedmann et al., “Multi Layer Insulation Literature,” DLR, Institute of Structural Mechanics, 20 pages total; Wei et al., “Effects of structure and shape on thermal performance of perforated multi-layer insulation blankets,” Applied Thermal Engineering, vol. 29, 2009, pages 1264-1266; Halaczek and Rafalowicz, “Heat transport in self-pumping multilayer insulation,” Cryogenics, vol. 26, 1986, pages 373-376; Shu et al., “Heat flux from 277 to 77 K through a few layers of multilayer insulation,” Cryogenics vol. 26, 1986, pages 671-677; Jacob et al., “Investigations into the thermal performance of multilayer insulation (300-77 K) Part 1: calorimetric studies,” Cryogenics, vol. 32, no. 12, 1992, pages 1137-1146; Jacob et al., “Investigations into the thermal performance of multilayer insulation (300-77 K) Part 2: Thermal analysis,” Cryogenics, vol. 32, no. 12, 1992, pages 1147-1153; Halaczek and Rafalowicz, “Unguarded cryostat for thermal conductivity measurements of multilayer insulations,” Cryogenics, vol. 25, 1985, pages 529-530; Mikhalchenko et al., “Theoretical and experimental investigation of radiative-conductive heat transfer in multilayer insulation,” Cryogenics, vol. 25, 1985, pages 275-278; Bapat et al., “Experimental investigations of multilayer insulation,” Cryogenics, vol. 30, 1990, pages 711-719; U.S. Pat. No. 5,590,054 to McIntosh, titled “Variable-density method for multi-layer insulation;” Zhitomirskil et al., “A theoretical model of the heat transfer process in multilayer insulation,” Cryogenics, 1979, pages 265-268; Shu, “Systematic study to reduce the effects of cracks in multilayer insulation Part 1: theoretical model,” Cryogenics, vol. 27, 1987, pages 249-256; Shu, “Systematic study to reduce the effects of cracks in multilayer insulation Part 2: experimental results,” Cryogenics, vol. 27, 1987, pages 298-311; Glassford and Liu, “Outgassing rate of multilayer insulation,” Lockheed Palo Alto Research Laboratory, pages 83-106; Halaczak and Rafalowicz, “Flat-plate cryostat for measurements of multilayer insulation thermal conductivity,” Cryogenics, vol. 25, 1985, pages 593-595; Matsuda and Yoshikiyo, “Simple structure insulating material properties for multilayer insulation,” Cryogenics, 1980, pages 135-138; Keller et al., “Application of high temperature multilayer insulations,” Acta Astronautica, vol. 26, no. 6, 1992, pages 451-458; Scurlock and Saull, “Development of multilayer insulations with thermal conductivities below 01. μW cm−1 K−1,” Cryogenics, May 1976, pages 303-311; Bapat et al., “Performance prediction of multilayer insulation,” Cryogenics vol. 30, 1990, pages 700-710; and Kropschot, “Multiple layer insulation for cryogenic applications,” Cryogenics, 1961, pages 171-177; which are each incorporated by reference.

In some embodiments, there is at least one section of ultra efficient insulation material within the gas-sealed gap 145. The term “ultra efficient insulation material,” as used herein, may include one or more type of insulation material with extremely low heat conductance and extremely low heat radiation transfer between the surfaces of the insulation material. The ultra efficient insulation material may include, for example, one or more layers of thermally reflective film, high vacuum, aerogel, low thermal conductivity bead-like units, disordered layered crystals, low density solids, or low density foam. In some embodiments, the ultra efficient insulation material includes one or more low density solids such as aerogels, such as those described in, for example: Fricke and Emmerling, Aerogels—preparation, properties, applications, Structure and Bonding 77: 37-87 (1992); and Pekala, Organic aerogels from the polycondensation of resorcinol with formaldehyde, Journal of Materials Science 24: 3221-3227 (1989), which are each herein incorporated by reference. As used herein, “low density” may include materials with density from about 0.01 g/cm3 to about 0.10 g/cm3, and materials with density from about 0.005 g/cm3 to about 0.05 g/cm3. In some embodiments, the ultra efficient insulation material includes one or more layers of disordered layered crystals, such as those described in, for example: Chiritescu et al., Ultralow thermal conductivity in disordered, layered WSe2 crystals, Science 315: 351-353 (2007), which is herein incorporated by reference. In some embodiments, the ultra efficient insulation material includes at least two layers of thermal reflective film surrounded, for example, by at least one of: high vacuum, low thermal conductivity spacer units, low thermal conductivity bead like units, or low density foam. See, for example, Mikhalchenko et al., “Study of heat transfer in multilayer insulation based on composite spacer materials,” Cryogenics, 1983, pages 309-311, which is incorporated by reference herein. In some embodiments, the ultra efficient insulation material may include at least two layers of thermal reflective material and at least one spacer unit between the layers of thermal reflective material. For example, the ultra-efficient insulation material may include at least one multiple layer insulating composite such as described in U.S. Pat. No. 6,485,805 to Smith et al., titled “Multilayer insulation composite,” which is herein incorporated by reference. For example, the ultra-efficient insulation material may include at least one metallic sheet insulation system, such as that described in U.S. Pat. No. 5,915,283 to Reed et al., titled “Metallic sheet insulation system,” which is herein incorporated by reference. For example, the ultra-efficient insulation material may include at least one thermal insulation system, such as that described in U.S. Pat. No. 6,967,051 to Augustynowicz et al., titled “Thermal insulation systems,” which is herein incorporated by reference. For example, the ultra-efficient insulation material may include at least one rigid multilayer material for thermal insulation, such as that described in U.S. Pat. No. 7,001,656 to Maignan et al., titled “Rigid multilayer material for thermal insulation,” which is herein incorporated by reference. See also: Li et al., “Study on effect of liquid level on the heat leak into vertical cryogenic vessels,” Cryogenics, vol. 50, 2010, pages 367-372; Barth et al., “Test results for a high quality industrial superinsulation,” Cryogenics, vol. 28, 1988, pages 607-609; and Eyssa and Okasha, “Thermodynamic optimization of thermal radiation shields for a cryogenic apparatus,” Cryogenics, 1978, pages 305-307; which are each incorporated by reference. For example, the ultra-efficient insulation material may include multilayer insulation material, or “MLI.” For example, an ultra efficient insulation material may include multilayer insulation material such as that used in space program launch vehicles, including by NASA. See, e.g., Daryabeigi, Thermal analysis and design optimization of multilayer insulation for reentry aerodynamic heating, Journal of Spacecraft and Rockets 39: 509-514 (2002), which is herein incorporated by reference. For example, the ultra efficient insulation material may include space with a gaseous pressure lower than atmospheric pressure external to the gas-sealed gap 145. See, for example, Nemanic, “Vacuum insulating panel,” Vacuum, vol. 46, nos. 8-10, 1995, pages 839-842, which is incorporated by reference. In some embodiments, the ultra efficient insulation material may substantially cover the inner wall 155 surface facing the gas-sealed gap 145. In some embodiments, the ultra efficient insulation material may substantially cover the outer wall 150 surface facing the gas-sealed gap 145.

In some embodiments, there is at least one layer of multilayer insulation material (“MLI”) within the gas-sealed gap 145. The at least one layer of multilayer insulation material may substantially surround the surface of the inner wall 155. In some embodiments, there are a plurality of layers of multilayer insulation material within the gas-sealed gap 145, wherein the layers may not be homogeneous. For example, the plurality of layers of multilayer insulation material may include layers of differing thicknesses, or layers with and without associated spacing elements. In some embodiments there may be one or more additional layers within or in addition to the insulation material, such as, for example, an outer structural layer or an inner structural layer. An inner or an outer structural layer may be made of any material appropriate to the embodiment, for example an inner or an outer structural layer may include: plastic, metal, alloy, composite, or glass. See, for example, U.S. Pat. No. 4,726,974 to Nowobilski et al., titled “Vacuum insulation panel,” which is incorporated by reference. In some embodiments, there may be one or more layers of high vacuum between layers of thermal reflective film. In some embodiments, the gas-sealed gap 145 includes a substantially evacuated gaseous pressure relative to the atmospheric pressure external to the structural region 180. A substantially evacuated gaseous pressure relative to the atmospheric pressure external to the structural region 180 may include substantially evacuated gaseous pressure surrounding a plurality of layers of MLI, for example between and around the layers. A substantially evacuated gaseous pressure relative to the atmospheric pressure external to the structural region 180 may include substantially evacuated gaseous pressure in one or more sections of the gas-sealed gap 145. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 1×10−2 torr. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 5×10−4 torr. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 1×10−2 torr in the gas-sealed gap 145. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 5×10−4 torr in the gas-sealed gap 145. In some embodiments, the gas-sealed gap 145 includes substantially evacuated space having a pressure less than 1×10−2 torr, for example, less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr. For example, in some embodiments the gas-sealed gap 145 includes a plurality of layers of multilayer insulation material and substantially evacuated space having a pressure less than or equal to 1×10−2 torr. For example, in some embodiments the gas-sealed gap 145 includes a plurality of layers of multilayer insulation material and substantially evacuated space having a pressure less than or equal to 5×10−4 torr.

As illustrated in FIG. 1, during some steps of the methods described herein, and when included with the apparatus 185, the gas-sealed gap 145 of the structural region 180 is open to the interior of the connector 120. The structural region 180 is joined to the connector 120 in a manner to form a substantially gas sealed space with the interior of the gas-sealed gap 145. The structural region 180 is operably attached to the connector 120 with a seal sufficient to maintain low gas pressure within the gas-sealed gap 145, such as through action of the vacuum pump 130. The structural region 180 is operably attached to the connector 120 with a seal sufficient to maintain minimal gas pressure within the gas-sealed gap 145, such as through action of the vacuum pump 130. For example, the structural region 180 may be operably attached to the connector 120 with a seal sufficient to maintain gas pressure less than or equal to 1×10−2 torr within the gas-sealed gap 145 through action of the vacuum pump 130. As illustrated in FIG. 1, some embodiments may include a valve 135 integral to the connector 120 and adjacent to the outer wall 150 of the structural region 180, wherein the valve 135 is operably attached in an orientation to isolate the interior of the connector 120 on the opposing ends of the valve 135.

The apparatus 185 includes an activation region 100 fabricated from a heat-resistant material, the activation region 100 including one or more getters 110. Although a single activation region 100 is depicted in FIGS. 1-4, in some embodiments there may be a plurality of activation regions that may be fabricated from the same or different heat-resistant materials and may contain either the same or different types of getters. In embodiments with a plurality of activation regions, each region may be independently operably attached to a connector. In embodiments with a plurality of activation regions, there may be one or more valves operably attached between one or more of the plurality of activation regions and the associated connector.

As used herein, the term “heat-resistant material” refers to materials that maintain their structural integrity at temperatures and conditions above the activation temperature(s) and within the condition(s) for the types of getter(s) 110 used in the apparatus 185. The term “heat-resistant,” as used herein, is relative to the activation temperature(s) and gas pressure conditions used for the specific getters 110 included in a given embodiment. For example, in some embodiments the getters 110 included in the apparatus 185 may include zirconium-vanadium-iron getters (see U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein). For example, in some embodiments the getters 110 included in the apparatus 185 may include St707™ getters with 70% zirconium, 24.6% vanadium and 5.4% iron (for example, available from Getter Technologies International Ltd., China). See: Gunter et al., “Microstructure and bulk reactivity of the nonevaporable getter Zr57V36Fe7,” Journal of Vacuum Science Technology, Vol. A16, no. 6, November/December 1998, pages 3526-3535, which is incorporated by reference. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature of approximately 700 degrees Centigrade for at least 20 seconds and then reducing the temperature to between approximately 400 degrees Centigrade and approximately 25 degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. A “heat-resistant material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would be a heat-resistant material that is predicted to maintain its structural integrity in a temperature of approximately 700 degrees Centigrade lasting for at least 20 seconds. A “heat-resistant material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would conserve its structural integrity at a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. For example, in some embodiments the getters 110 included in the apparatus 185 may include getters fabricated from a titanium-zirconium-vanadium getter material. See: Matolin and Johanek, “Static SIMS study of TiZrV NEG activation,” Vacuum, vol. 67, 2002, pages 177-184, which is incorporated by reference. A “heat-resistant material,” as used herein, for use with an embodiment incorporating getters fabricated from a titanium-zirconium-vanadium getter material, would conserve its structural integrity at a temperature less of approximately 300 degrees Centigrade with a gas pressure within the interior of approximately 5×10−11 mbar (see Matolin and Johanek, ibid, which is incorporated by reference). For example, in some embodiments the structural region 180 is fabricated from a heat-resistant material that includes stainless steel, or stainless steel alloys. For example, in some embodiments the structural region 180 is fabricated from a heat-resistant material that includes titanium alloy.

Getters of a variety of types may be used in different embodiments. The getters may be fabricated from a variety of getter materials. For example, the getters may be fabricated from non-evaporatable getter material. The selection of getters may depend, for example, on the availability, cost, mass, chemical composition, toxicity and durability of the getter material employed in a given embodiment. The selection of getters may depend, for example, on the activation temperature and conditions for a particular getter material. Some types of getters are activatable at different temperatures and gas pressure conditions for different lengths of time (see, e.g. U.S. Pat. No. 4,312,669 “Non-evaporable Ternary Gettering Alloy and Method of Use for the Sorption of Water, Water Vapor and Other Gasses,” to Boffito et al., which is incorporated by reference), and for such getter materials the selection of the materials may depend on the range of potential temperatures, gas pressure conditions, and times, or one or more combinations of activation temperatures, gas pressure conditions and times for a specific getter material. Some getters may require gas pressure conditions less than atmospheric pressures, such as near-vacuum conditions, during activation at particular temperatures (see Matolin and Johanek, ibid, and U.S. Pat. No. 4,312,669, ibid., which are each incorporated by reference). The selection of getters may depend, for example, on the operational temperature of a given getter material, such as within ambient temperatures (i.e. substantially between 20 degrees Centigrade and 30 degrees Centigrade), within refrigeration temperatures (i.e. substantially between 2 degrees Centigrade and 10 degrees Centigrade) or within freezing temperatures (for example, substantially between 0 degrees Centigrade and −10 degrees Centigrade, or substantially between −15 degrees Centigrade and −25 degrees Centigrade). Some embodiments may include a single type of getters, for example getters fabricated from substantially the same active getter material. Some embodiments may include a plurality of types of getters fabricated from substantially distinct getter materials. More information regarding types of getters and getter materials suitable for various embodiments of the invention may be found in: Tripathi et al., “Hydrogen intake capacity of ZrVFe alloy bulk getters,” Vacuum, vol. 48, no. 12, 1997, pages 1023-1025; Benvenuti et al., “Nonevaporable getter films for ultrahigh vacuum applications,” Journal of Vacuum and Science Technology, vol. A16, no. 1, January/February 1998, pages 148-154; Benvenuti et al., “Decreasing surface outgassing by thin film getter coatings,” Vacuum, vol. 50, nos. 1-2, 1998, pages 57-63; Boffito et al., “A nonevaporable low temperature activatable getter material,” Journal of Vacuum and Science Technology, vol. 18, no. 3, May/June 1981, pages 1117-1120; della Porta, “Gas problem and gettering in sealed-off vacuum devices,” Vacuum, vol. 47, nos 6-8, 1996, pages 771-777; Benvenuti and Chiggiato, “Obtention of pressures in the 10-14 torr range by means of a Zr—V—Fe non evaporable getter,” Vacuum, vol. 44, nos. 5-7, 1993, pages 511-513; Londer et al., “New high capacity getter for vacuum insulated mobile LH2 storage tank systems,” Vacuum, vol. 82, 2008, pages 431-434; Li et al., “Design and pumping characteristics of a compact titanium-vanadium non-evaporable getter pump,” Journal of Vacuum and Science Technology, vol. A16, no. 3, May/June 1998, pages 1139-1144; Chiggiato, “Production of extreme high vacuum with non evaporable getters,” Physica Scripta, vol. T71, 1997, pages 9-13; Benvenuit and Chiaggiato, “Pumping characteristics of the St707 nonevaporable getter (Zr 70 V 24.6-Fe 5.4 wt %),” Journal of Vacuum and Science Technology, vol. A14, no. 6, November/December 1996, pages 3278-3282; Day, “The use of active carbons as cryosorbent,” Colloids and Surfaces A: Physicochem. Eng. Aspects 187-188, 2001, pages 187-206; U.S. Pat. No. 4,312,669 “Non-evaporable Ternary Gettering Alloy and Method of Use for the Sorption of Water, Water Vapor and Other Gasses,” to Boffito et al.; Hobson and Chapman, “Pumping of methane by St707 at low temperatures,” Journal of Vacuum and Science Technology, vol. A4, no. 3, May/June 1986, pages 300-302; and Matolin and Johanek, “Static SIMS study of TiZrV NEG activation,” Vacuum, vol. 67, 2002, pages 177-184; which are each incorporated by reference.

As illustrated in FIG. 1, the activation region 100 includes walls forming a gas-sealed interior. The gas-sealed interior of the activation region 100 encloses one or more getters 110. Also as illustrated in FIG. 1, the activation region 100 includes a gas-sealed interior enclosing one or more getters 110, wherein the gas-sealed interior of the activation region 100 is open to the interior of the connector 120. The gas-sealed interior of the activation region 100 is configured to maintain a reduced gas pressure as established by the vacuum pump 130. Although not illustrated in FIG. 1, some embodiments may include a valve (e.g. as valve 135) located integral to the connector 120 at a location adjacent to the activation region 100, the valve configured to isolate the gas pressure within the connector 120 at the opposite sides of the valve.

As noted herein, the apparatus 185 is configured to establish and maintain a reduced gas pressure environment within the gas-sealed gap 145 of the structural region 180. Accordingly, the one or more getters 110 may include non-evaporatable getter material. The one or more getters 110 may include zirconium, vanadium and iron. For example, the one or more getters 110 may include 70% zirconium, 24.6% vanadium and 5.4% iron. For example, the one or more getters 110 may include St707 getters (available, for example, from SAES Getters Group, with corporate headquarters in Lainate, Italy; see attached online brochure downloaded on Sep. 21, 2011, which is incorporated by reference herein). Similar getter materials are also available from other sources, such as Getter Technologies International Ltd., China.

As illustrated in FIG. 1, the apparatus 185 includes a connector 120 attached to the structural region 180 and to the activation region 100, the connector 120 including a flexible region 125 and a region 127 configured for sealing and detachment of the structural region 180 from the activation region 100. The connector 120 may be fabricated, for example, from stainless steel or stainless steel alloy. The connector 120 may be fabricated, for example, from different materials in different regions, as appropriate to the embodiment. Generally, the connector 120 is fabricated from material(s) with low vapor emission on the surface within the connector 120 as well as sufficient strength, durability, and heat tolerance for a specific embodiment and associated methods (as described further in the section below). Cost, weight, and flexibility may also be factors in the selection of material(s) for fabrication of the connector 120. See, for example, Nemanic and Setina, “A study of thermal treatment procedures to reduce hydrogen outgassing rate in thin wall stainless steel cells,” Vacuum, vol. 53, 1999, pages 277-280; and Koyatsu et al., “Measurements of outgassing rate from copper and copper alloy chambers,” Vacuum, vol. 47, no. 6-8, 1996, pages 709-711, which are each incorporated by reference.

The connector may include a valve 135 configured to inhibit the flow of gas within the connector 120. Some embodiments may include more than one valve. As illustrated in FIG. 1, a valve 135 may be operably attached to the connector 120 at a location between the vacuum pump 130 and the outer wall 150 of the structural region. The valve 135 may be operably attached to the connector 120 at a location between the vacuum pump 130 and the region 127 configured for sealing and detachment of the structural region 180 from the activation region 100.

As illustrated in FIG. 1, in some embodiments the flexible region 125 of the connector 120 is adjacent to the activation region 100 of the apparatus 185. The flexible region 125 is configured to allow the activation region 100 to shift orientation relative to the remainder of the apparatus 185 (see also FIGS. 2-4) while retaining the low gas pressure within the connector as established and maintained by the vacuum pump 130. As illustrated in FIG. 1, the flexible region 125 is configured in an arc forming approximately a right angle, with the result that the activation region 100 and the structural region 180 are not in a horizontally linear alignment. As illustrated in FIGS. 1-4, in some embodiments the flexible region 125 of the connector 120 is configured to flex along the long axis of the connector 120 (i.e. as depicted by the double headed arrow in FIG. 1). The change in configuration of the flexible region 125 results in the change in relative orientation of the activation region 100 and the structural region 180, as illustrated in FIGS. 1-4. The flexible region 125 may be flexible due to the combination of the material from which it is fabricated as well as the configuration of that material. For example, the flexible region 125 of the connector 120 may be fabricated from stainless steel in a bellows-type configuration. A bellows-type configuration would be fabricated from suitable material and configured to allow for flexibility in the flexible region 125 of the connector 120. For example, the flexible region 125 of the connector 120 may be fabricated from stainless steel and configured in a corrugated, channeled, grooved or ridged shape to allow for flexibility of the flexible region 125 of the connector 120.

As illustrated in FIG. 1, the apparatus 185 includes a vacuum pump 130 operably attached to the connector 120. The vacuum pump 130 has sufficient pumping strength to establish a gas pressure within the apparatus 185 less than the gas pressure in the environment adjacent to the apparatus 185. In some embodiments, the vacuum pump 130 has sufficient pumping strength to establish a gas pressure that is substantially evacuated. In some embodiments, the vacuum pump 130 has sufficient pumping strength to establish a gas pressure that is near vacuum. For example, in some embodiments the vacuum pump 130 has sufficient pumping strength to evacuate the gas-sealed gap 145 in the interior of the structural region 180, the interior of the activation region 100 and the interior of the connector 120 to a gas pressure less than or equal to 1×10−2 torr. For example, in some embodiments the vacuum pump 130 has sufficient pumping strength to evacuate the gas-sealed gap 145 in the interior of the structural region 180, the interior of the activation region 100 and the interior of the connector 120 to a gas pressure less than or equal to 5×10−3 torr, 5×10−4 torr, 5×10−5 torr, 5×10−6 torr or 5×10−7 torr. The vacuum pump 130 may be a rotary vane style vacuum pump. Suitable vacuum pumps for some embodiments are manufactured, for example, by Pfeiffer Balzers Company, (Pfeiffer Vacuum GmbH, Germany). Suitable vacuum pumps for some embodiments are manufactured, for example, by the Edwards Vacuum Company (US Headquarters Tewksbury Mass.; Global Headquarters United Kingdom). Vacuum pumps suitable in some embodiments include Pfeiffer Balzers model TSH060 and Edwards model RV12.

The apparatus 185 includes a region 127 of the connector 120 configured for sealing and detachment of the structural region 180 from the activation region 100. In some embodiments, the apparatus 185 includes a region 127 of the connector 120 configured for sealing and detachment of the connector 120 adjacent to the structural region 180 along the length of the connector 120. As illustrated in FIG. 1, the region 127 of the connector 120 configured for sealing and detachment of the structural region 180 from the remainder of the apparatus 185 may be located in a region of the connector 120 adjacent to the outer wall 150 of the structural region 180. The apparatus 185 includes a region 127 of the connector 120 configured for sealing and detachment configured to allow for the gas-sealed gap 145 within the structural region 180 to maintain its low gas pressure (e.g. less than or equal to 1×10−2 torr) during detachment of the structural region 180 from the remainder of the apparatus 185. The region 127 of the connector 120 configured for sealing and detachment of the structural region 180 from the activation region 100 may be, for example, a section of aluminum tubing. In embodiments using aluminum tubing for the region 127 of the connector 120 configured for sealing and detachment of the structural region 180 from the activation region 100, the aluminum tube may be, for example, one half inch in diameter and 0.035 inches thick tubing, such as model 3003-O available from Aircraft Spruce and Specialty Company (Corona, Calif.). In embodiments including aluminum tubing for the region 127 of the connector 120 configured for sealing and detachment of the structural region 180 from the activation region 100, the aluminum tube may be, for example, collapsed on itself (i.e. “pinched off”) and the edges sealed together using a pinch and crimp instrument. For example, an ultrasonic welder may be used to seal and detach the sections of aluminum tubing.

The apparatus 185, as illustrated in FIGS. 1-4 and as described in the associated methods herein, is designed and fabricated to allow activated getters 110 to be moved within the apparatus 185 from the activation region 100 through the connector 120 into the gas-sealed gap 145 within the structural region 180. The activated getters 110 are moved within the apparatus 185 while the interior spaces of the activation region 100, the connector 120 and the gas-sealed gap 145 within the structural region 180 include gas pressure lower than that in the environment surrounding the apparatus 185. The activated getters 110 are moved within the apparatus 185 while the interior spaces of the activation region 100, the connector 120 and the gas-sealed gap 145 within the structural region 180 are being actively evacuated by the vacuum pump 130. Further aspects of the apparatus 185 are shown in FIGS. 2-4. FIGS. 2-4 illustrate additional aspects of the apparatus 185 shown in FIG. 1, particularly in relation to the design and fabrication of the apparatus 185 to allow the activated getters 110 to move within the interior of the connector 120 between the activation region 100 and the gas-sealed gap 145.

FIG. 2 depicts the apparatus 185 with the flexible region 125 of the connector 120 moved so that the activation region 100 is directly above the structural region 180. As shown in FIG. 2, the flexible region 125 of the connector 120 is fabricated and configured to allow it to bend into a substantially straight configuration. As is apparent from the combination of FIGS. 1 and 2, the flexible region 125 of the connector 120 is fabricated and configured to allow it to bend from a substantially right angle (as shown in FIG. 1) to a substantially linear configuration (as shown in FIG. 2). This motion is depicted by the double-headed arrow in FIG. 2. The apparatus 185 depicted in FIG. 2 is oriented with the flexible region 125 of the connector 120 so that the activation region 100 is directly above the structural region 180 to allow for the getters 110 A, 110 B, 110 C, to fall with the force of gravity (depicted by the single headed arrows) through the connector 120 and into the gas-sealed gap 145.

FIG. 2 also depicts the motion of the activated getters 110 A, 110 B, 110 C, from the activation region 100 through the connector 120 (e.g. illustrated with single-headed arrows). For purposes of illustration, the getters 110 as shown in FIG. 1 are given individual identifiers A, B and C in FIG. 2; however, the individual getters 110 A, 110 B, 110 C are intended to be equivalent to the group of getters 110 shown in FIGS. 1, 3, 4 and 5. Although three individual getters 110 A, 110 B, 110 C in a substantially oval shape are shown, the specific number and shape of the getters 110 would depend on the specific embodiment. As illustrated in FIG. 2, the apparatus 185 is fabricated from material configured to allow the getters 110 A, 110 B, 110 C to move from the activation region 100 through the connector 120. The getters 110 selected for a particular embodiment should be of a size and shape to move out of the activation region 100, through the connector 120, and into the gas-sealed gap 145 of the structural region 180. Getters in a form with rounded edges are well-suited for this purpose, but getters of varying shapes may be used in different embodiments. Getters formed as granules may be utilized in some embodiments, however getters formed as granular shapes may become stuck within the connector 120 and not move easily into the gas-sealed gap 145. Preferably, the entirety of the getters 110 should be located within the gas-sealed gap 145 at the end of the method steps. Preferably, no getters 110 should remain in the connector 120 during sealing of the connector 120. For example, the getter material may reduce the integrity of the sealed region of the connector 120.

Correspondingly, the activation region 100 should be operably attached to the connector 120 in a manner to minimally impede the movement of the getters 110 out of the activation region 100 and into the internal region within the connector 120. The attachment should provide a sufficient seal to allow for the establishment and maintenance of a reduced gas pressure (e.g. less than or equal to 1×10−2 torr) within the interior of the apparatus 185 by the vacuum pump 130. For example, in embodiments where the apparatus is fabricated from metal, the activation region 100 may be attached to the connector 120 by weld junctions. These weld junctions should be sufficiently smooth and minimally facing on the interior of the apparatus 185 to provide minimal impedance of the getters 110 through the connector 120. Similarly, the structural region 180 should be operably attached to the connector 120 in a manner to minimally impede the movement of the getters 110 out of the interior of the connector 120 and into the gas-sealed gap 145 within the structural region 180.

The interior diameter of the connector 120, including within its own regions 125 and 127, as well as the interior diameter of any valve(s) (e.g. 135) opening(s) should be suitable for the passage of the getters 110 through the apparatus 185 between the activation region 100 and the gas-sealed gap 145 in the structural region 180. The size and shape of any particular getters 110 used should be less than the interior diameter of the connector 120 and any valve(s) (e.g. 135) utilized within the apparatus 185. The interior of the connector 120 and any valve(s) (e.g. 135) incorporated into the apparatus 185 should include minimal surfaces which may impede the movement of the getters 110 through the apparatus 185. For example, the interior of the connector 120 and any valve(s) (e.g. 135) should be substantially smooth, without sharp, jutting, or rough edges that may impede the getters 110. For example, the interior of the connector 120 and any valve(s) (e.g. 135) should be substantially free of internal elements, such as struts or braces, which may inhibit getters 110 travelling through the interior. Generally, the interior of the apparatus 185 should be designed and fabricated to allow for the direct movement of the getters 110 from the interior of the activation region 100 through the connector 120 and into the gas-sealed gap 145 in the structural region 180 when the activation region 100, connector 120 and the structural region 180 are appropriately oriented (i.e. as depicted in FIG. 2). In some embodiments, the interior of the apparatus 185 should be designed and fabricated to allow for the direct movement of the getters 110 from the interior of the activation region 100 through the connector 120 and into the gas-sealed gap 145 in the structural region 180, such as through the force of gravity, when the activation region 100, connector 120 and the structural region 180 are appropriately positioned (i.e. as depicted in FIG. 2). In some embodiments, the interior of the apparatus 185 should be designed and fabricated to allow for the direct movement of the getters 110 through mechanical transfer from the interior of the activation region 100 through the connector 120 and into the gas-sealed gap 145 in the structural region 180.

FIG. 2 depicts the flexible region 125 of the connector 120 in a substantially straight configuration, and with the activation region 100 of the apparatus 185 positioned above the structural region 180. The apparatus is fabricated to allow the flexible region 125 of the connector to move the relative positioning of the apparatus 185, as illustrated in the double-headed arrow, between the position shown in FIG. 1 and that shown in FIG. 2. FIG. 2 depicts getter 110 A in a position to soon fall through the force of gravity (depicted by downward facing arrows) through the connector 120 and into the gas-sealed gap 145 of the structural region 180. FIG. 2 also depicts getter 110 B positioned within the connector 120 and moving through the force of gravity through the connector 120 towards the structural region 180. FIG. 2 depicts getter 110 C in the junction between the gas-sealed gap 145 of the structural region 180 and the connector 120 adjacent to the outer wall 150.

FIG. 3 illustrates the apparatus 185 positioned similarly to that shown in FIG. 2, at a later stage (see methods described herein). In the view illustrated in FIG. 3, the activated getters 110 are all positioned within the gas-sealed gap 145 of the structural region 180. Although the activated getters 110 are illustrated in a cluster in FIG. 3, they may also be distributed within the gas-sealed gap 145. In some embodiments, structural elements within the gas-sealed gap 145 confine some or all of the activated getters 110 into a defined region of the gas-sealed gap 145. For example, the gas-sealed gap 145 may include internal braces or struts that restrict the mobility of the getters 110 within the gas-sealed gap 145. For example, the gas-sealed gap 145 may include wire netting material configured to restrict the movement of the getters 110 within the gas-sealed gap 145.

FIG. 3 depicts that the connector 120 includes a crimped area 300 with the opposing faces of the connector brought together to form a gas-impermeable seal. The crimped area 300 is within the region 127 configured for sealing and detachment of the connector 120. As shown in FIG. 3, the crimped area 300 may be positioned adjacent to the outer wall 150 of the structural region 180, but with a length 320 of the connector 120 between the crimped area 300 and the surface of the outer wall 150. Also as shown in FIG. 3, there may be a length 310 of the connector 120 between the crimped area 300 and a valve 135. As illustrated by the double-headed arrows in FIG. 3, after the crimped area 300 is formed, the structural region 180 is detached from the remainder of the apparatus 185. In order to detach the structural region 180 from the remainder of the apparatus 185, the connector 120 is separated at the crimped area while maintaining the reduced gas pressure (e.g. less than or equal to 1×10−2 torr) within the gas-sealed gap 145. In some embodiments, a gas-impermeable seal may be formed in the connector 120 substantially simultaneously as the separation at the sealed site. For example, the connector 120 may be sealed and separated with an ultrasonic welding device.

FIG. 4 shows the apparatus 185 positioned similarly to that shown in FIG. 3, at a later stage (see methods described herein). In FIG. 4, the activated getters 110 are within the gas-sealed gap 145. Also as shown in FIG. 4, the connector 120 has been separated at the crimped area 300. The separation of the connector 120 at the crimped area 300 results in the detachment of the structural region 180 from the remainder of the apparatus 185 (double headed arrows). FIG. 4 also shows a sealing agent 400 applied to the surface of the crimped area 300 adjacent to the structural region 180. The sealing agent 400 is positioned and applied to ensure that the crimped area 300 adjacent to the structural region 180 maintains its structural integrity and does not include any holes or spaces that would permit gas from the environment external to the outer wall 150 to enter the gas-sealed gap 145. The sealing agent 400, if included in a particular embodiment, adheres to the surface of the separated crimped area 300 to form a gas-tight seal on the interior of the connector length 310 adjacent to the outer wall 150. For example, the sealing agent may include epoxy material.

FIG. 23 depicts a cross-section view of a substantially thermally sealed storage container, such as may be included in a structural region 180 of an apparatus (not depicted in FIG. 23). The cross-section view is presented to illustrate various aspects of the container that are not visible in an external view. The cross-section presented is approximately half of the container, with the omitted region being substantially similar to the illustrated region. FIG. 23 is an example of an embodiment of a unit included in a structural region 180 of an apparatus (not depicted in FIG. 23), although other embodiments are within the scope of the disclosure herein. The substantially thermally sealed storage container depicted in FIG. 23 includes an outer wall 150 and an inner wall 155. The inner wall 155 substantially defines a storage region 165 within the container. The outer wall 150 and the inner wall 155 are separated by a gas-sealed gap 145.

The container depicted in FIG. 23 also includes an access tube 2340 between the interior storage region 165 and the exterior of the container. The access tube 2340 is attached to the inner wall 155 with a gas-impermeable seal 2320. For example, the access tube 2340 and the inner wall 155 may both be fabricated from stainless steel, and the gas-impermeable seal 2320 may be a suitable weld joint. The interior of the access tube 2340 forms an opening 160 between the exterior of the container and the interior storage region 165. The opening 160 is of a sufficient size and shape to allow stored material to be placed within and removed from the interior of the interior storage region 165, while substantially maintaining the storage and thermal properties of the interior storage region 165. The container also includes a neck region 2330 in a substantially tubular structure surrounding the access tube 2340. The neck region 2330 is attached to the outer wall 150 with a gas-impermeable seal 2360. For example, the neck region 2330 and the outer wall 150 may both be fabricated from stainless steel, and the gas-impermeable seal 2360 may be a suitable weld joint. The end of the access tube 2340 distal to the inner wall 155 and the end of the neck region 2330 distal to the outer wall 150 are connected with an end seal 2310. Although the end seal 2310 depicted is a discrete unit joining the gap between the surfaces of the access tube 2340 and the neck region 2330, the end seal 2310 may also include a crimp or other form of a gas-impermeable seal. As shown in FIG. 23, the gas-sealed gap 145 may be coextensive with the region 2350 between the neck region 2330 and the access tube 2340.

FIG. 23 also depicts two ducts 175 attached to the outer wall 150. These ducts 175 may be suitable for the attachment of a gas pressure gauge (such as identified as 140 in FIGS. 1-4) or other device as suitable to the embodiment. In the embodiment illustrated in FIG. 23, the ends of the ducts 175 are closed with barrier units 2300 secured with a gas-impermeable seal, such as welds or rivets. As the ducts 175 are coextensive with the gas-sealed gap 145, the ducts 175 should be similarly gas-sealed to preserve the reduced gas pressure (e.g. less than or equal to 1×10−2 torr) within the gas-sealed gap 145.

A storage container such as depicted in FIG. 23 may include phase-change material within the interior storage region 165. Generally speaking, specific properties of the materials, including durability, mass, corrosiveness, toxicity, and cost, should be taken into account in the selection of the materials used in fabricating a storage container. See, for example, Nemanic and Setina, “A study of thermal treatment procedures to reduce hydrogen outgassing rate in thin wall stainless steel cells,” Vacuum, vol. 53, 1999, pages 277-280; and Koyatsu et al., “Measurements of outgassing rate from copper and copper alloy chambers,” Vacuum, vol. 47, no. 6-8, 1996, pages 709-711, which are each incorporated by reference. In embodiments including phase change materials, the specific properties of the phase change materials, including durability, mass, corrosiveness, toxicity, and cost, should be taken into account in the selection of the materials used in fabricating the storage container. For example, the inner wall 155 should be fabricated from a material that retains its structural stability in the presence of the specific phase change material utilized under the expected use conditions. See: Zalba et al., “Review on thermal energy storage with phase change: materials, heat transfer analysis and applications,” Applied Thermal Engineering, vol. 23, 2003, pages 251-283; and Bo et al., “Tetradecane and hexadecane binary mixtures as phase change materials (PCMs) for cool storage in district cooling systems,” Energy, vol. 24, 1000, pages 1015-1028; which are each incorporated by reference.

Methods

FIG. 5 illustrates an optional method of preparation of the metallic system components of the apparatus prior to assembly of the apparatus. In order to establish and maintain a substantially reduced gas pressure (e.g. less than or equal to 1×10−2 torr) within the apparatus, the metallic surfaces of the components of the apparatus may optionally be cleaned and prepared to minimize outgassing from surface contaminants on the metallic surfaces. FIG. 5 depicts, as an example, a flowchart of a method that may be used in some embodiments to prepare the metallic system components of the apparatus as described herein prior to assembly of the apparatus. See also Y. T. Sasaki, “A survey of vacuum material cleaning procedures: A subcommittee report of the American Vacuum Society Recommended Practices Committee,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 9, May. 1991, p. 2025, which is incorporated by reference.

FIG. 5 illustrates a flowchart of a method to prepare metallic system components prior to assembly 500 of an apparatus. Block 510 depicts cleaning components with denatured alcohol. This step may reduce grease, oil and similar contaminants on the surfaces of the components. The flowchart also includes optional block 520, illustrating mechanically polishing the components. See, for example, Kato et al., “Achievement of extreme high vacuum in the order of 10−10 Pa without baking of test chamber,” Journal of Vacuum Science and Technology, vol. A8, no. 3, May/June 1990, pages 2860-2864, which is incorporated by reference. This step may be omitted, for example wherein the components already are sufficiently smooth. See: S. Okamura, “Outgassing measurement of finely polished stainless steel,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 9, July 1991, p. 2405; M. Suemitsu et al., “Ultrahigh-vacuum compatible minor-polished aluminum-alloy surface: Observation of surface-roughness-correlated outgassing rates,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 10, 1992, pp. 570-572; M. Suemitsu et al., “Development of extremely high vacuums with mirror-polished AL-alloy chambers,” Vacuum, vol. 44, nos. 5-7, 1993, pages 425-428; H. F. Dylla, “Correlation of outgassing of stainless steel and aluminum with various surface treatments,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 11, September 1993, p. 2623; Mohri et al., “Surface study of Type 6063 aluminum alloys for vacuum chamber materials,” Vacuum, vol. 34, no. 6, 1984, pages 643-647; and Y. T. Sasaki, “Reducing SS 304316 hydrogen outgassing to 2×10 [sup−15] torr 1/cm[sup 2] s,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 25, 2007, p. 1309, which are all incorporated by reference. If the components are mechanically polished, they may be subsequently cleaned an additional time with denatured alcohol (not illustrated in FIG. 5).

Block 530 illustrates washing the components with detergents and water. A detergent washing step may reduce the presence of fine contaminants such as hydrocarbon oils and solvents, which may contribute to undesirable outgassing within the finished apparatus. See: R. Elsey, “Outgassing of vacuum materials-II,” Vacuum, vol. 25, 1975, pp. 347-361, which is incorporated by reference. As an example, hand dishwashing detergent (i.e. Dawn Advanced Power Dish Soap, manufactured by the Procter & Gamble Company) may be used to hand wash the components in warm tap water and a standard soft sponge. As an additional example, the detergent Alconox® may be used to clean the components in tap water (available from Alconox Inc., White Plains N.Y.). Optional block 540 depicts rinsing the washed components with deionized water (DI water). Optional block 550 illustrates blowing the components dry with dehumidified nitrogen gas, or a comparable inert gas. This step may reduce non-visible water molecules adhering to the surface of the components. See, for example: A. Berman, “Water vapor in vacuum systems,” Vacuum, vol. 47, no. 4, 1996, pages 327-332; J.-R. Chen et al., “Outgassing behavior of A6063-EX aluminum alloy and SUS 304 stainless steel,” Journal of Vacuum Science and Technology, vol. A5, no. 6, November/December 1987, pages 3422-3424; Y. C. Liu et al., “Thermal outgassing study on aluminum surfaces,” Vacuum, vol. 44, nos. 5-7, 1993, pages 435-437; Chen and Liu, “A comparison of outgassing rate of 304 stainless steel and A6063-EX aluminum alloy vacuum chamber after filling with water,” Journal of Vacuum Science and Technology, vol. A5, no. 2, March/April 1987, pages 262-264; Ishimaru et al., “Fast pump-down aluminum ultrahigh vacuum system,” Journal of Vacuum Science and Technology, vol. A10, no. 3, May/June 1992, pages 547-552; Miki et al., “Characteristics of extremely fast pump-down process in an aluminum ultrahigh vacuum system,” Journal of Vacuum Science and Technology, vol. A12, no. 4, July/August 1994, pages 1760-1766; and Chen et al., “Outgassing behavior on aluminum surfaces: water in vacuum systems,” Journal of Vacuum Science and Technology, vol. A12, no. 4, July/August 1994, pages 1750-1754, which are each incorporated by reference. In some embodiments, treatment with different types of gas may be included. See: Tatenuma et al., “Quick acquisition of clean ultrahigh vacuum by chemical process technology,” Journal of Vacuum Science and Technology, vol. All, no. 4, July/August 1993, pages 1719-1724; Tatenuma et al., “Acquisition of clean ultrahigh vacuum using chemical treatment,” Journal of Vacuum Science and Technology, vol. A16, no. 4, July/August 1998, pages 2693-2697; and L. C. Beavis, “Interaction of hydrogen with the surface of type 304 stainless steel,” Journal of Vacuum Science and Technology, vol. 10, no. 2, March/April 1973, pages 386-390; which are incorporated by reference. Block 560 depicts baking the components under vacuum conditions. See, for example: H. Ishimaru, “Fast pump-down aluminum ultrahigh vacuum system,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 10, May 1992, p. 547, which is incorporated by reference.

Baking components under vacuum conditions has been demonstrated to be useful for reducing outgassing from some materials, for example, for aluminum and stainless steel components. See: J. Young, “Outgassing Characteristics of Stainless Steel and Aluminum with Different Surface Treatments,” Journal of Vacuum Science and Technology, 1969; Odaka and Ueda, “Dependence of outgassing rate on surface oxide layer thickness in type 304 stainless steel before and after surface oxidation in air,” Vacuum, no. 47, nos. 6-8, 1996, pages 689-692; Odaka et al., “Effect of baking temperature and air exposure on the outgassing rate of type 316L stainless steel,” Journal of Vacuum Science and Technology, vol. A5, no. 5, September/October 1987, pages 2902-2906; Zajec and Nemanic, “Hydrogen bulk states in stainless-steel related to hydrogen release kinetics and associated redistribution phenomena,” Vacuum, vol. 61, 2001, pages 447-452; Bernardini et al., “Air bake-out to reduce hydrogen outgassing from stainless steel,” Journal of Vacuum Science and Technology, vol. A16, no. 1, January/February 1998, pages 188-193; Nemanic et al., “Anomalies in kinetics of hydrogen evolution from austenitic stainless steel from 300 to 1000° C.,” Journal of Vacuum Science and Technology, vol. A19, no. 1, January/February 2001, pages 215-222; Nemanic and Bogataj, “Outgassing of thin wall stainless steel chamber,” Vacuum, vol. 50, no. 3-4, 1998, pages 431-437; Cho et al., “Creation of extreme high vacuum with a turbomolecular pumping system: a baking approach,” Journal of Vacuum Science and Technology, vol. A13, no. 4, July/August 1995, pages 2228-2232; and Y. Ishikawa and K. Odaka, “Reduction of outgassing from stainless surfaces by surface oxidation,” Vacuum, vol. 41, 1990, pp. 1995-1997; which are incorporated by reference. For example, stainless steel components may be baked for 30 hours at 250 degrees Centigrade in a chamber with a gas pressure of approximately 1×10−2 torr. As an additional example, aluminum components or composite components may be baked at 150 degrees Centigrade for 60-70 hours in a chamber with a gas pressure of approximately 1×10−2 torr. See also: Chen et al., “An aluminum vacuum chamber for the bending magnet of the SRRC synchrotron light source,” Vacuum, vol. 41, nos. 7-9, 1990, pages 2079-2081; Burns et al., “Outgassing test for non-metallic materials associated with sensitive optical surfaces in a space environment,” Materials and Processes Laboaratory, George C. Marshall Space Flight Center, 1987; and Chen et al., “Thermal outgassing from aluminum alloy vacuum chambers,” Journal of Vacuum Science and Technology, vol. A3, no. 6, November/December 1985, pages 2188-2191, which are each incorporated by reference. In addition or alternately, baking components in the presence of inert gas has been demonstrated to be useful for reducing outgassing from some materials. In some embodiments, as an alternate to near-vacuum gas pressure conditions, the components are baked in the presence of inert gas, such as nitrogen.

After the components are cleaned and prepared, the components of the apparatus are assembled. A helium leak check may be performed to ensure that seals and/or junctions are sufficient to maintain reduced gas pressure conditions within the interior of the apparatus. In addition, the apparatus may be purged with dehydrated nitrogen gas during the check of the final assembly. See: K. Yamazaki, et al., “High-speed pumping to UHV,” Vacuum, vol. 84, December 2009, pp. 756-759; and Chun et al., “outgassing rate characteristic of a stainless-steel extreme high vacuum system,” Journal of Vacuum Science and Technology, vol. A14, no. 4, July/August 1996, pages 2636-2640; which are incorporated by reference.

FIG. 6 illustrates a flowchart of a method utilizing an apparatus such as those described herein (as above). FIG. 6 depicts a method 600, including steps depicted as blocks 610, 620, 630, 640 and 650. Block 610 illustrates establishing vacuum within a gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions. As used herein, “vacuum” refers to the gas pressure in substantially evacuated space. As used herein, “vacuum” refers to a low gas pressure relative to the gas pressure in the environment external to the apparatus. Different levels of vacuum may be suitable in different embodiments. For example, as used herein, “vacuum” refers to substantially evacuated space that may have a gas pressure less than 1×10−2 torr, less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr. Different gas pressures may be desirable depending on the specific embodiment, including factors such as durability, cost, components, fabrication, structure and expected duration of use. The vacuum may be established within an interior of the at least one activation region, within an interior of the at least one structural region, and within an interior of the connector of the gas-sealed apparatus. The vacuum may be established utilizing a vacuum pump operably connected to the gas-sealed apparatus. Suitable vacuum pumps for some embodiments are manufactured, for example, by Pfeiffer Balzers Company, (Pfeiffer Vacuum GmbH, Germany). Suitable vacuum pumps for some embodiments are manufactured, for example, by the Edwards Vacuum Company (US Headquarters Tewksbury Mass.; Global Headquarters United Kingdom). Vacuum pumps suitable in some embodiments include Pfeiffer Balzers model TSH060 and Edwards model RV12. See also Ishimaru and Hismatsu, “Turbomolecular pump with an ultimate pressure of 10−12 Torr,” Journal of Vacuum Science and Technology, vol. A12, no. 4, July/August 1994, pages 1695-1698; and Jhung et al., “Achievement of extremely high vacuum using a cryopump and conflate aluminum gaskets,” Vacuum, vol. 43, no. 4, 1992, pages 309-311, which are each incorporated by reference.

In some embodiments, heating the apparatus components while establishing the vacuum may reduce the time required to establish vacuum, for example by increasing the rate of evaporation of traces of water on the surfaces of the interior of the apparatus. In order to heat the apparatus components while establishing the vacuum, the apparatus may be placed within an oven of suitable size and operating conditions. In addition or alternately, in order to heat the apparatus components while establishing the vacuum, the exterior surfaces of the apparatus may be wrapped with heat tape, and the base of the apparatus may be placed on a hot plate. Suitable heat tape for some embodiments includes, for example, insulated heat tapes and may include fiberglass heavy insulated heat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, Stafford Tex.). The gas-sealed apparatus may be heated, for example, in temperature increments to ensure even heating, to allow time to monitor the apparatus, to allow for maintenance of the low gas pressure within the interior, and to ensure that the apparatus does not over-heat. The apparatus may be heated, as an example, to approximately 130-150 degrees Centigrade in approximately 50 degree increments during establishment of vacuum within the gas-sealed apparatus. The apparatus may be heated, as an example, to approximately 180-220 degrees Centigrade in approximately 20 degree increments during establishment of vacuum within the gas-sealed apparatus. Depending on the embodiment, establishing the vacuum may take several days, even with heating of the apparatus components assisting in a reduction of the time required. For example, establishing the vacuum may take a time on the order of 5-7 days of continual action by the vacuum pump and heating of the apparatus components. Even after suitable cleaning and other preparation, outgassing of volatile materials from the internal surfaces of the gas-sealed apparatus is expected, and will increase the time required to reach a suitably low gas pressure for a given embodiment. For example, heating the gas-sealed apparatus will increase outgassing of material from the internal surfaces of the gas-sealed apparatus. Suitable gas pressure within the interior of the apparatus is established when a gas pressure gauge operably attached to the apparatus displays a reading in the range appropriate for the embodiment (e.g. a gas pressure less than 1×10−2 torr, less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr).

The method flowchart depicted in FIG. 6 also includes block 620, showing heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established vacuum within the apparatus. As noted above, the activation temperature for a particular embodiment is dependent on the specific getters included in that embodiment. Heating of an activation region includes heating the getters within the activation region to a suitable temperature. Getters suitable for some embodiments include zirconium-vanadium-iron getters, as described in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature of approximately 700 degrees Centigrade for at least 20 seconds and then reducing the temperature to between approximately 400 degrees Centigrade and approximately 25 degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. In some embodiments, the activation region may be heated to a temperature of approximately 400 degrees Centigrade for at least 45 minutes. In some embodiments, the activation region may be heated in intervals of approximately 50 degrees Centigrade.

Heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region while maintaining the established vacuum within the apparatus may include heating the activation region independently from the remainder of the apparatus while the vacuum pump attached to the apparatus is operating. For example, the activation region may be heated with a heat source external to the apparatus. In some embodiments, in order to heat the activation region, the activation region exclusively to the remainder of the apparatus may be placed within an oven of suitable size, shape and properties. In some embodiments, in order to heat the activation region, the exterior surfaces of the activation region may be wrapped with heat tape. Suitable heat tape for some embodiments includes, for example, insulated heat tapes and may include fiberglass heavy insulated heat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, Stafford Tex.). Heating the activation region may include heating with a heat source in direct thermal contact with the activation region and not in direct thermal contact with the structural region and the connector of the gas-sealed apparatus. For example, if heat tape is used, a specific section of heat tape may be wrapped around the outer surface of the activation region and set to a temperature higher than any temperature setting for the remainder of the apparatus.

The method flowchart depicted in FIG. 6 also includes block 630, illustrating allowing the at least one activation region and the getters to cool to a temperature compatible with structural stability of the heat-sensitive material. The activation region may be cooled through radiative heat loss. For example, in embodiments where heat tape is used to heat the external surface of the activation region, the heat tape may be removed and the activation region allowed to cool by heat radiation into the external environment. In some embodiments, the activation region may be allowed to cool to a specific temperature, or temperature range, such as approximately 100 degrees Centigrade, approximately 150 degrees Centigrade, approximately 200 degrees Centigrade, approximately 250 degrees Centigrade, approximately 300 degrees Centigrade, or approximately 350 degrees Centigrade.

As shown in FIG. 6, the method flowchart also includes block 640, depicting transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the gas-sealed apparatus. For example, the cooled getters may be transferred through the gas-sealed apparatus by gravitational transfer, such as through reorienting the relative positions of the activation region and the structural region and allowing the getters to move through gravity through the apparatus (see FIGS. 1-4 and associated text, above). For example, the cooled getters may be transferred through the apparatus through a mechanical transfer, such as with an internal trowel, scoop, ladle, or fork configured to transfer the cooled getters within the gas-sealed apparatus.

The flowchart depicted in FIG. 6 also includes block 650, illustrating separating the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters. For example, the connector may be separated at a region adjacent to the surface of the outer wall of the structural region by crimping the connector sufficiently to establish a gas-tight seal, and separating the connector into two parts at the crimped region. An ultrasonic welder may be utilized to separate the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters. A specialized crimping device may be used to separate the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters.

FIG. 7 illustrates additional aspects of the method illustrated in the flowchart of FIG. 6. FIG. 7 shows block 610, which illustrates establishing vacuum within a gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions. Optional blocks 700, 710 and 720 illustrate optional aspects of the method. Block 700 illustrates establishing vacuum within an interior of the at least one activation region, within an interior of the at least one structural region, and within an interior of the connector of the gas-sealed apparatus. For example, vacuum may be established using a vacuum pump operably attached to the apparatus and the methods described herein. In some embodiments, additionally heating the apparatus may decrease the time required to establish vacuum within the gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions. Block 710 depicts utilizing a vacuum pump operably connected to the gas-sealed apparatus. For example, some embodiments may utilize a rotary vane style vacuum pump. Suitable vacuum pumps for some embodiments are manufactured, for example, by Pfeiffer Balzers Company, (Pfeiffer Vacuum GmbH, Germany). Suitable vacuum pumps for some embodiments are manufactured, for example, by the Edwards Vacuum Company (US Headquarters Tewksbury Mass.; Global Headquarters United Kingdom). Vacuum pumps suitable in some embodiments include Pfeiffer Balzers model TSH060 and Edwards model RV12. FIG. 7 includes block 720, depicting establishing gas pressure less than or equal to 1×10−2 torr within the gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions. In some embodiments, the gas pressure established within the gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions may be less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr.

FIG. 8 illustrates additional aspects of the method flowchart depicted in FIG. 7. Flowchart block 620 depicts heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established vacuum within the apparatus. Flowchart block 620 may include one or more of optional blocks 800 and 810. Block 800 depicts heating the activation region to a temperature of approximately 400 degrees Centigrade for at least 45 minutes. The activation region should be heated to a temperature and for a duration sufficient to activate the particular type of getters within the activation region given the conditions of a particular embodiment, such as the size, shape and position of the getters as well as the gas pressure within the activation region. As described herein, the activation temperature and activation conditions (e.g. time and gas pressure) of the particular type of getters used in a particular embodiment is the basis for determining the heating temperature and time of the activation region. Block 810 illustrates heating the activation region with a heat source external to the apparatus. For example, exclusively of the remainder of the apparatus the activation region may be placed within an oven of suitable size, shape and operating parameters. For example, the outer surface of the activation region may be heated with a heat tape wrapped around the activation region of the apparatus. Suitable heat tape for some embodiments includes, for example, insulated heat tapes and may include fiberglass heavy insulated heat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, Stafford Tex.). Heating the activation region may include heating with a heat source in direct thermal contact with the activation region and not in direct thermal contact with the structural region and the connector of the gas-sealed apparatus.

FIG. 9 illustrates aspects of the method flowchart as illustrated in FIG. 6. Flowchart block 620 depicts heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established vacuum within the apparatus. Flowchart block 620 may include one or more of optional blocks 900 and 910. Block 900 depicts heating the activation region with a heat source in direct thermal contact with the activation region and not in direct thermal contact with the structural region and the connector of the gas-sealed apparatus. For example, heat tape may be wrapped around the exterior surface of the activation region and not other regions of the apparatus, and the heat tape specifically controlled independently of any other controls. Block 910 illustrates heating the at least one activation region in intervals of approximately 50 degrees Centigrade. For example, if the at least one activation region is initially at a temperature of approximately 25 degrees Centigrade, the at least one activation region may be heated to approximately 75 degrees Centigrade, then 125 degrees Centigrade, then 175 degrees Centigrade, and so on until the final desired activation temperature is reached.

FIG. 10 depicts aspects of the method flowchart illustrated in FIG. 6. Block 630 shows allowing the at least one activation region and the getters to cool to a temperature compatible with structural stability of the heat-sensitive material. Flowchart block 630 may include one or more of optional blocks 1000 and 1010. Block 1000 illustrates allowing the at least one activation region to cool to an ambient temperature through radiative heat loss. For example, any heat tape may be turned off, allowed to cool, and then removed from the exterior surface of an activation region. The activation region then is allowed to cool to either a predetermined temperature or an ambient temperature through radiative heat loss. Block 1010 depicts allowing the at least one activation region to cool to approximately 250 degrees Centigrade. For example, approximately 250 degrees Centigrade may be a temperature compatible with structural stability of a heat-sensitive material such as aluminum.

FIG. 11 shows aspects of the method flowchart illustrated in FIG. 6. Block 640 shows transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the apparatus. Block 640 may include one or more of optional blocks 1100 and 1110. Block 1100 depicts bending the connector to allow the cooled one or more getters to move from the cooled at least one activation region to the at least one structural region through the connector. For example, the method may include bending a flexible region of the connector to place the activation region in a position substantially above the structural region, allowing the getters to fall through the force of gravity from the one activation region to the structural region through the connector. The vacuum pump may be operational during the getter transfer to maintain the established vacuum within the apparatus. Block 1110 illustrates bending the connector to alter the relative positioning of the cooled at least one activation region to the at least one structural region in relation to the connector. For example, the method may include bending the connector to alter the relative position of the at least one activation region relative to the structural region.

FIG. 12 depicts aspects of the method flowchart illustrated in FIG. 6. Block 640 shows transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the apparatus. Block 640 may include optional block 1200. Block 1200 shows transferring the cooled one or more getters into a gas-sealed gap between an inner wall and an outer wall of the structural region. For example, the activation region may be positioned so that the connector is in a substantially linear configuration, and oriented so that the opening of the activation region attached to the connector is approximately directly above an opening into the gas-sealed gap that is operably attached to the connector. Block 650 shows separating the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters. For example, the connector may be crimped and separated at a region adjacent to the outer surface of the structural region. Block 650 may include optional block 1210. Block 1210 depicts sealing the connector at a position adjacent to the structural region. For example, as illustrated in FIGS. 1-4, the connector may include a region configured for sealing and detachment of the structural region from the activation region in a location adjacent to the structural region. The region configured for sealing and detachment of the structural region from the activation region need not be directly next to the exterior surface of the structural region; as shown in FIGS. 1-4, there may be a section of the connector between the exterior surface of the structural region and the position where the connector is sealed and detached.

FIG. 13 shows aspects of the method flowchart illustrated in FIG. 6. Block 650 shows separating the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters. For example, the connector may be welded together and then disconnected using an ultrasonic welding device. Block 650 may include optional block 1300. Block 1300 depicts crimping the connector; and breaking the connector at the crimp location. For example, an ultrasonic welder may be used to weld to opposite faces of the connector together, and then to break the connector at the weld joint. For example, a crimping device specialized to crimp the connector sufficiently to form a gas-impermeable seal may be used, and the connector then broken at the seal location. As shown in FIG. 13, the method flowchart may also include optional block 1310. Block 1310 depicts adding sealing material to a surface of the separated connector adjacent to the structural region including the cooled one or more getters. Sealing material, such as epoxy material, may be added to the surface of the separated connector, such as over the crimp or weld site. See also FIG. 4 and associated text.

FIG. 14 depicts aspects of the method flowchart shown in FIG. 6. FIG. 14 illustrates that the flowchart may include one or more of optional blocks 1400 and 1410. Block 1400 may include block 1410. Block 1400 shows heating the structural region to a preset temperature for a predetermined time after establishing vacuum within the structural region and before heating the activation region. For example, the structural region may be heated to approximately 150 degrees to facilitate establishment of a durable vacuum within the apparatus. For example, the structural region may be heated with heat tape placed on the external surface of the structural region. For example, the structural region may be placed on a heat plate. Block 1410 depicts heating the structural region to the preset temperature by intervals of approximately 50 degrees Centigrade. For example, if starting at an ambient temperature of approximately 25 degrees Centigrade, the structural region may be heated to approximately 75 degrees Centigrade, then to approximately 125 degrees Centigrade, then to approximately 175 degrees Centigrade, then to approximately 225 degrees Centigrade, and so on until the desired temperature is reached. The heating series may be held at any or all of the series of temperatures for a given time period, for example for 10 minutes, 1 hour, 5 hours, or 1 day.

FIG. 15 illustrates aspects of the method flowchart shown in FIG. 6. FIG. 15 illustrates that the flowchart may include optional block 1500. Block 1500 depicts heating the structural region to a preset temperature prior to transferring the cooled one or more getters; and maintaining the preset temperature while separating the connector. For example, the structural region may be placed on a hot plate heated to a preset temperature before the transfer of the cooled one or more getters, and the structural region maintained on the hot plate set to a constant temperature during transfer of the getters. For example, the structural region may be wrapped with heat tape and heated to a preset temperature prior to the transfer of the getters, and the temperature maintained during the transfer. For example, the structural region may be heated to a predetermined temperature between approximately 125 degrees Centigrade and approximately 175 degrees Centigrade, and this temperature maintained during the getter transfer. For example, the structural region may be heated to a predetermined temperature between approximately 175 degrees Centigrade and approximately 225 degrees Centigrade, and this temperature maintained during the getter transfer. For example, the structural region may be heated to a predetermined temperature between approximately 200 degrees Centigrade and approximately 250 degrees Centigrade, and this temperature maintained during the getter transfer.

FIG. 16 illustrates a flowchart of a method. Block 1600 of the flowchart illustrates that the method is of establishing and maintaining vacuum within a storage device. Block 1600 includes blocks 1610, 1620, 1630, 1640, 1650, 1660, 1670, 1680 and 1690. Block 1610 illustrates assembling the components of a storage device, including an outer wall and an inner wall substantially defining a gas-sealed gap. Block 1620 depicts attaching the storage device to an apparatus, the apparatus including a getter activation region containing one or more getters, a vacuum pump, and a connector operably connecting the storage device to the apparatus. Block 1630 shows activating the vacuum pump to establish gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. Block 1640 illustrates heating the storage device to a predetermined temperature for a predetermined length of time. Block 1650 shows heating the getter activation region and the one or more getters to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. Block 1660 illustrates allowing the getter activation region and the one or more getters to cool to a predetermined temperature. Block 1670 shows flexing the connector to move the storage device and the getter activation region into a relative position wherein the getter activation region is above the storage device and the connector is substantially linear. Block 1680 depicts allowing the getters to fall along the connector interior into the gas-sealed gap in the storage device, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. Block 1690 shows separating the connector at a location adjacent to the storage device while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device.

Block 1620 depicts attaching the storage device to an apparatus, the apparatus including a getter activation region containing one or more getters, a vacuum pump, and a connector operably connecting the storage device to the apparatus. For example, the assembled device may be attached to an apparatus with a substantially gas-impermeable junction to form an apparatus such as illustrated in FIGS. 1-4. As shown in FIGS. 1-4, the interior of the apparatus includes a gas-sealed space within the getter activation region, the connector and the gas-sealed gap of the storage device. The gas-sealed gasp within a storage device may be connected to an apparatus through a conduit, for example with one or more ducts as illustrated as 175 in FIG. 23.

FIG. 17 illustrates aspects of the flowchart depicted in FIG. 16. FIG. 17 illustrates that block 1610 may include optional block 1700. Block 1610 illustrates assembling the components of a storage device, including an outer wall and an inner wall substantially defining a gas-sealed gap. For example, the components of a storage device may be assembled into a device as illustrated in FIGS. 1-4 and in FIG. 23. As shown in FIG. 17, block 1610 may include optional block 1700. Block 1700 depicts assembling the components of the storage device to form a gas-sealed gap within the storage device. For example, there may be joints, welds or seals included in the assembled components to create a gas-impermeable seal around the perimeter of the gas-sealed gap within the storage device.

FIG. 17 shows further aspects of the flowchart depicted in FIG. 16. FIG. 17 illustrates that block 1630 may include optional block 1710. Block 1630 depicts activating the vacuum pump to establish gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. For example, one or more vacuum pumps may be utilized to establish substantially evacuated space within the gas-sealed gap of the storage device. For example, one or more vacuum pumps may be utilized to establish an extremely low gas pressure within the gas-sealed gap of the storage device. Block 1710 illustrates establishing a gas pressure of less than or equal to 1×10−2 ton. For example, one or more vacuum pumps may be utilized to establish a gas pressure less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr within the gas-sealed gap of the storage device.

FIG. 18 illustrates additional aspects of the flowchart shown in FIG. 16. Block 1640 illustrates heating the storage device to a predetermined temperature for a predetermined length of time. For example, the storage device may be heated with an external heat source to a predetermined temperature for a length of time estimated to be required to evaporate any surface contaminants on the interior surface of the gas-sealed gap of the storage device. For example, the storage device may be heated with an external heat source to a predetermined temperature for a length of time estimated to be required to dehydrate the interior surface of the gas-sealed gap of the storage device. The heating temperature and time will depend on the specific embodiment, for example the type of material used to fabricate the storage device, the prior surface treatment of the material (for example as described in relation to FIG. 5, text above), and the desired final gas pressure within the gas-sealed gap of the storage device. FIG. 18 illustrates that block 1640 may include one or more of optional blocks 1800 and 1810. Block 1800 illustrates heating the storage device in increments of approximately 50 degrees Centigrade. For example, in an embodiment where heat tape wrapped around the exterior of the storage device is implemented to heat the storage device, the controller for the heat tape may be set to warm the heat tape in approximately 50 degree Centigrade increments. Warming the storage device in increments may be desirable, for example, to avoid overheating, or to ensure that the storage device is heated evenly throughout the surface, or to confirm that the junctions between the storage device and the connector are retaining a gas seal during the process. Warming the storage device in increments may be desirable, for example, to allow for time to check the gas pressure internal to the apparatus during the process. Block 1810 illustrates heating the storage device to between approximately 130 degrees Centigrade and approximately 150 degrees Centigrade for at least 100 hours. The specific time and temperature will depend on the embodiment, and the time required to reduce the internal gas pressure of the apparatus to a target gas pressure. For example, the specific time and temperature will depend on factors including the material used to fabricate the storage device, any pretreatment of the components, the size and shape of the gas-sealed gap, the size and shape of the interior of the apparatus, and the pumping capacity of the vacuum pump in a given embodiment. In some embodiments, the storage device may be heated to between approximately 150 degrees Centigrade and approximately 200 degrees Centigrade. In some embodiments, the storage device may be heated for approximately 75 hours. In some embodiments, the storage device may be heated for approximately 100 hours, or approximately 125 hours.

FIG. 19 shows additional aspects of the flowchart shown in FIG. 16. Block 1650 illustrates heating the getter activation region and the one or more getters to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. As discussed above, the activation temperature and time required in a specific embodiment depends on the getters used. For example, as noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. Also relevant is the material used in the fabrication of the activation region including the getters, clearly a user of the apparatus and method would not heat the getter activation region to a temperature predicted to compromise the structural integrity of the activation region. For example, a user of the apparatus and method would not heat the getter activation region to a temperature wherein the getter activation region could not maintain its shape and structure in response to the internal force of the low gas pressure. For example, a user of the apparatus and method would not heat the getter activation region to a temperature wherein the getter activation region would be predicted to melt, implode or deform based on the material and fabrication of the structure.

FIG. 19 illustrates that the flowchart of FIG. 16 may also include one or more of optional blocks 1900 and 1910 within block 1650. Block 1900 depicts heating the activation region to a temperature of approximately 400 degrees Centigrade for at least 45 minutes. For example, in embodiments employing a zirconium-vanadium-iron getter material, the getter material may be activated at approximately 400 degrees Centigrade for a duration of at least 45 minutes (see U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein). Block 1910 illustrates heating the getter activation region with a heat source external to the getter activation region. For example, the getter activation region may be wrapped with heat tape on the external surface of the getter activation region as a heat source. For example, the getter activation region may be placed in direct contact with a hot plate or similar heating surface as a heat source.

FIG. 20 depicts aspects of the method flowchart shown in FIG. 16. The flowchart shown in FIG. 20 depicts the method of establishing and maintaining vacuum within a storage device 1600 as illustrated in FIG. 16, as well as flowchart blocks 1610, 1620, 1630, 1640, 1650, 1660, 1670, 1680, 190 and optional blocks 2000 and 2010. The flowchart shown in FIG. 20 includes block 1660, showing allowing the getter activation region and the one or more getters to cool to a predetermined temperature. For example, after heating (as illustrated in block 1650), the getter activation region and the one or more getters may be cooled to a temperature compatible with further steps of the method. For example, after heating (as illustrated in block 1650), the getter activation region and the one or more getters may be cooled to a temperature compatible with allowing the getters to fall along the connector interior into the gap in the storage device (as shown in block 1680). For example, the getter activation region and the getters may be cooled to a temperature compatible with the structural integrity of the connector). For example, the getter activation region and the getters may be cooled to a temperature compatible with the structural integrity of the storage device. The predetermined temperature(s) will depend on factors including the material used to fabricate the regions of the apparatus, as well as safe and desirable handling temperatures for the apparatus in a given embodiment. Temperatures of the activation region may be determined through means suitable to a given embodiment, such as estimates based on the external surface conditions of the activation region. In some embodiments, there may be an embedded temperature sensor within the activation region.

FIG. 20 illustrates that the flowchart depicted in FIG. 16 may include optional block 2000 within block 1660. Block 2000 shows allowing the getter activation region to cool to approximately 250 degrees Centigrade through radiative heat loss. For example, in embodiments using heat tape on the exterior surface of the activation region to heat the activation region, the heat tape may be entirely or partially removed and the activation region allowed to cool through radiative heat loss from the external surface. For example, in embodiments wherein the activation region is placed in direct physical contact with a surface of a heat source (e.g. a hot plate), the activation region may be removed from the heat source and allowed to cool. The temperature of the surface of the activation region may be used as an approximation for the temperature of the entire activation region and its contents (e.g. the one or more getters). In some embodiments, there may be a temperature sensor within the interior of the activation region and the reading of that temperature sensor may be utilized in the method.

As shown in FIGS. 16 and 20, the flowchart includes block 1670, which depicts flexing the connector to move the storage device and the getter activation region into a relative position wherein the getter activation region is above the storage device and the connector is substantially linear. For example, as illustrated in FIGS. 1-4, the shape of the connector may be altered to allow the getter activation region to be moved to a position substantially above an opening in the gap in the storage device and for the connector to be substantially straight. The connector may be flexed into a position that allows for the activated getters to fall from an opening in the getter activation region through the interior of the connector and into the gap in the storage device. As shown in FIG. 20, block 1670 may include optional block 2010. Block 2010 shows flexing the connector to move the storage device and the getter activation region into a relative position wherein the getter activation region is above the storage device and the connector is substantially linear by flexing a region of the connector adjacent to the getter activation region. For example, as illustrated in FIGS. 1-4 and described in the associated text (see above), the connector may include a flexible region, such as a region in a corrugated or bellows-type configuration, adjacent to the activation region. The flexible portion of the connector adjacent to the activation region may be flexed to move the storage device and the getter activation region into a relative position wherein the getter activation region is substantially above the storage device.

FIG. 21 illustrates aspects of the flowchart depicted in FIG. 16. FIGS. 16 and 21 include block 1690, depicting separating the connector at a location adjacent to the storage device while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. For example, the connector may be sealed at a location adjacent to the storage device and then two sections of the connector separated either at the seal site or adjacent to the seal site in a manner to maintain the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. FIG. 21 shows that block 1690 of the flowchart may include one or more of optional blocks 2100 and 2110. Block 2100 depicts physically crimping the connector; and breaking the connector at the crimp location. For example, the connector may be flattened at a location adjacent to the storage device by physically pressing together the sides of the connector with a crimping device sufficient to create a gas-sealed region in the connector at the crimp site. After the connector is sufficiently crimped to create a gas-tight seal in the connector, the connector may be physically broken into two pieces at the crimp location. If desired, an additional sealing or stabilization material (e.g. epoxy) may be added to the external surface of the connector to stabilize the sealed surface (see also item 400 in FIG. 4). Block 2110 depicts separating the connector at a location adjacent to the storage device while maintaining the established gas pressure utilizing an ultrasonic welding device.

FIG. 22 depicts further aspects of the flowchart as shown in FIG. 16. FIG. 22 shows that block 1600, the method of establishing and maintaining vacuum within a storage device, may include one or more of optional blocks 2200, 2210, 2220 and 2230. Block 2200 illustrates heating the storage device to a predetermined temperature for a predetermined time after establishing gas pressure below atmospheric pressure within the gap of the storage device. For example, it may be desirable in some embodiments to dehydrate the interior surfaces of the gas-sealed gap in the storage device (e.g. item 190 in FIG. 1) through heating prior to the connector being sealed. For example, it may be desirable in some embodiments to heat the storage device to a temperature similar to the temperature of the getters when they are placed within the gas-sealed gap to ensure even heating and associated expansion of the storage device prior to addition of the heated getters. Block 2210 illustrates monitoring gas pressure within the gas-sealed gap of the storage device. For example, it may be desirable in some embodiments to attach a gas pressure gauge to the storage device. FIG. 23, for example, illustrates two ducts 175 attached to the outer wall 150 of the structural region 180 including a storage device. A gas pressure gauge could be attached to one of the ducts 175 if desired in a specific embodiment. Block 2220 shows monitoring gas pressure within the connector. A gas pressure gauge, for example, may be operably attached to the connector through a duct or a similar structure and used to monitor gas pressure within the connector during one or more steps of the method. Block 2230 shows adding sealing material to the surface of the separated connector adjacent to the storage device. For example, an epoxy compound may be added to the surface of the separated connector adjacent to the storage device (see also item 400 in FIG. 4).

One skilled in the art will recognize that the herein described components (e.g., operations), devices, objects, and the discussion accompanying them are used as examples for the sake of conceptual clarity and that various configuration modifications are contemplated. Consequently, as used herein, the specific exemplars set forth and the accompanying discussion are intended to be representative of their more general classes. In general, use of any specific exemplar is intended to be representative of its class, and the non-inclusion of specific components (e.g., operations), devices, and objects should not be taken limiting.

The herein described subject matter sometimes illustrates different components contained within, or connected with, different other components. It is to be understood that such depicted architectures are merely exemplary, and that in fact many other architectures may be implemented which achieve the same functionality. In a conceptual sense, any arrangement of components to achieve the same functionality is effectively “associated” such that the desired functionality is achieved. Hence, any two components herein combined to achieve a particular functionality can be seen as “associated with” each other such that the desired functionality is achieved, irrespective of architectures or intermedial components. Likewise, any two components so associated can also be viewed as being “operably connected”, or “operably coupled,” to each other to achieve the desired functionality, and any two components capable of being so associated can also be viewed as being “operably couplable,” to each other to achieve the desired functionality. Specific examples of operably couplable include but are not limited to physically mateable and/or physically interacting components, and/or wirelessly interactable, and/or wirelessly interacting components, and/or logically interacting, and/or logically interactable components.

While particular aspects of the present subject matter described herein have been shown and described, it will be apparent to those skilled in the art that, based upon the teachings herein, changes and modifications may be made without departing from the subject matter described herein and its broader aspects and, therefore, the appended claims are to encompass within their scope all such changes and modifications as are within the true spirit and scope of the subject matter described herein. It will be understood by those within the art that, in general, terms used herein, and especially in the appended claims (e.g., bodies of the appended claims) are generally intended as “open” terms (e.g., the term “including” should be interpreted as “including but not limited to,” the term “having” should be interpreted as “having at least,” the term “includes” should be interpreted as “includes but is not limited to,” etc.). It will be further understood by those within the art that if a specific number of an introduced claim recitation is intended, such an intent will be explicitly recited in the claim, and in the absence of such recitation no such intent is present. For example, as an aid to understanding, the following appended claims may contain usage of the introductory phrases “at least one” and “one or more” to introduce claim recitations. However, the use of such phrases should not be construed to imply that the introduction of a claim recitation by the indefinite articles “a” or “an” limits any particular claim containing such introduced claim recitation to claims containing only one such recitation, even when the same claim includes the introductory phrases “one or more” or “at least one” and indefinite articles such as “a” or “an” (e.g., “a” and/or “an” should typically be interpreted to mean “at least one” or “one or more”); the same holds true for the use of definite articles used to introduce claim recitations. In addition, even if a specific number of an introduced claim recitation is explicitly recited, those skilled in the art will recognize that such recitation should typically be interpreted to mean at least the recited number (e.g., the bare recitation of “two recitations,” without other modifiers, typically means at least two recitations, or two or more recitations). Furthermore, in those instances where a convention analogous to “at least one of A, B, and C, etc.” is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., “a system having at least one of A, B, and C” would include but not be limited to systems that have A alone, B alone, C alone, A and B together, A and C together, B and C together, and/or A, B, and C together, etc.). In those instances where a convention analogous to “at least one of A, B, or C, etc.” is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., “a system having at least one of A, B, or C” would include but not be limited to systems that have A alone, B alone, C alone, A and B together, A and C together, B and C together, and/or A, B, and C together, etc.). It will be further understood by those within the art that typically a disjunctive word and/or phrase presenting two or more alternative terms, whether in the description, claims, or drawings, should be understood to contemplate the possibilities of including one of the terms, either of the terms, or both terms unless context dictates otherwise. For example, the phrase “A or B” will be typically understood to include the possibilities of “A” or “B” or “A and B.”

With respect to the appended claims, those skilled in the art will appreciate that recited operations therein may generally be performed in any order. Also, although various operational flows are presented in a sequence(s), it should be understood that the various operations may be performed in other orders than those which are illustrated, or may be performed concurrently. Examples of such alternate orderings may include overlapping, interleaved, interrupted, reordered, incremental, preparatory, supplemental, simultaneous, reverse, or other variant orderings, unless context dictates otherwise. Furthermore, terms like “responsive to,” “related to,” or other past-tense adjectives are generally not intended to exclude such variants, unless context dictates otherwise.

With respect to the use of substantially any plural and/or singular terms herein, those having skill in the art can translate from the plural to the singular and/or from the singular to the plural as is appropriate to the context and/or application. The various singular/plural permutations are not expressly set forth herein for sake of clarity.

All of the above U.S. patents, U.S. patent application publications, U.S. patent applications, foreign patents, foreign patent applications and non-patent publications referred to in this specification and/or listed in any Application Data Sheet, are incorporated herein by reference, to the extent not inconsistent herewith.

While various aspects and embodiments have been disclosed herein, other aspects and embodiments will be apparent to those skilled in the art. The various aspects and embodiments disclosed herein are for purposes of illustration and are not intended to be limiting, with the true scope and spirit being indicated by the following claims.

Claims

1. An apparatus comprising:

a structural region fabricated from a heat-sensitive material, the structural region including an outer wall and an inner wall with a gas-sealed gap between the outer wall and the inner wall;
an activation region fabricated from a heat-resistant material, the activation region including one or more getters;
a connector attached to the structural region and to the activation region, the connector including a flexible region and a region configured for sealing and detachment of the structural region from the activation region; and
a vacuum pump operably attached to the connector.

2. The apparatus of claim 1, wherein the structural region comprises:

a storage device.

3. (canceled)

4. The apparatus of claim 1, wherein the structural region comprises:

a thermally-insulated device.

5. The apparatus of claim 1, wherein the structural region comprises:

a device configured for detachment from a remainder of the apparatus.

6. (canceled)

7. The apparatus of claim 1, wherein the heat-sensitive material comprises:

aluminum.

8.-11. (canceled)

12. The apparatus of claim 1, wherein the gas-sealed gap comprises:

multilayer insulation material.

13. The apparatus of claim 1, wherein the gas-sealed gap comprises:

gas at a pressure less than or equal to 1×10−2 torr.

14. The apparatus of claim 1, wherein the gas-sealed gap is open to an interior of the connector.

15. The apparatus of claim 1, wherein the heat-resistant material comprises:

stainless steel.

16. (canceled)

17. The apparatus of claim 1, wherein the activation region comprises:

a gas-sealed interior, wherein the one or more getters are enclosed within the gas-sealed interior.

18. The apparatus of claim 17, wherein the gas-sealed interior is open to an interior of the connector.

19. The apparatus of claim 1, wherein the one or more getters comprise:

non-evaporatable getter material.

20.-21. (canceled)

22. The apparatus of claim 1, wherein the connector comprises:

stainless steel.

23. The apparatus of claim 1, wherein the connector comprises:

a valve configured to inhibit the flow of gas within the connector.

24. (canceled)

25. The apparatus of claim 1, wherein the flexible region of the connector has a bellows configuration.

26. The apparatus of claim 1, wherein the vacuum pump is sufficient to evacuate an interior of the structural region, the activation region and the connector to a gas pressure less than or equal to 1×10−2 torr.

27. (canceled)

28. The apparatus of claim 1, comprising:

a gas-sealed, connected space interior to each of the structural region, the activation region and the connector.

29. (canceled)

30. The apparatus of claim 1, further comprising:

a pressure gauge operably connected to the connector.

31. The apparatus of claim 1, further comprising:

one or more seals between the structural region, the activation region and the connector, the seals sufficient to maintain a vacuum within the structural region, the activation region and the connector.

32. A method comprising:

establishing vacuum within a gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions;
heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established vacuum within the gas-sealed apparatus;
allowing the at least one activation region and the one or more getters to cool to a temperature compatible with structural stability of the heat-sensitive material;
transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the gas-sealed apparatus; and
separating the connector between the regions while maintaining the established vacuum within the structural region including the cooled one or more getters.

33. The method of claim 32, wherein the establishing vacuum comprises:

establishing vacuum within an interior of the at least one activation region, within an interior of the structural region, and within an interior of the connector of the gas-sealed apparatus.

34. (canceled)

35. The method of claim 32, wherein the establishing vacuum comprises:

establishing gas pressure less than or equal to 1×10−2 torr.

36. (canceled)

37. The method of claim 32, wherein the heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region comprises:

heating the at least one activation region with a heat source external to the apparatus.

38. The method of claim 32, wherein the heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region comprises:

heating the at least one activation region with a heat source in direct thermal contact with the at least one activation region and not in direct thermal contact with the structural region and the connector of the gas-sealed apparatus.

39. (canceled)

40. The method of claim 32, wherein the allowing the at least one activation region and the one or more getters to cool to a temperature compatible with structural stability of the heat-sensitive material comprises:

allowing the at least one activation region to cool to an ambient temperature through radiative heat loss.

41.-42. (canceled)

43. The method of claim 32, wherein the transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the gas-sealed apparatus comprises:

bending the connector to alter the relative positioning of the cooled at least one activation region to the structural region in relation to the connector.

44. The method of claim 32, wherein the transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the gas-sealed apparatus comprises:

transferring the cooled one or more getters into a gas-sealed gap between an inner wall and an outer wall of the structural region.

45.-46. (canceled)

47. The method of claim 32, further comprising:

adding sealing material to a surface of the separated connector adjacent to the structural region including the cooled one or more getters.

48. The method of claim 32, further comprising:

heating the structural region to a preset temperature for a predetermined time after establishing vacuum within the structural region and before heating the at least one activation region.

49. (canceled)

50. The method of claim 32, further comprising:

heating the structural region to a preset temperature prior to transferring the cooled one or more getters; and
maintaining the preset temperature while separating the connector.

51. A method of establishing and maintaining a vacuum within a storage device, comprising:

assembling substantially all structural components of a storage device, including an outer wall and an inner wall substantially defining a gas-sealed gap;
attaching the storage device to a gas-sealed apparatus, the gas-sealed apparatus including a getter activation region containing one or more getters, a vacuum pump, and a connector operably connecting the storage device to the gas-sealed apparatus;
activating the vacuum pump to establish a gas pressure below atmospheric pressure within the gas-sealed gap of the storage device;
heating the storage device to a predetermined temperature for a predetermined length of time;
heating the getter activation region and the one or more getters to an activation temperature for an activation time suitable to activate the one or more getters within the getter activation region, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device;
allowing the getter activation region and the one or more getters to cool to a predetermined temperature;
flexing the connector to move the storage device and the getter activation region into a relative position wherein the getter activation region is above the storage device and the connector is substantially linear;
allowing the one or more getters to fall along the connector interior into the gas-sealed gap in the storage device, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device;
separating the connector at a location adjacent to the storage device while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device.

52. (canceled)

53. The method of claim 51, wherein the activating the vacuum pump to establish a gas pressure below atmospheric pressure within the gas-sealed gap of the storage device comprises:

establishing a gas pressure of less than or equal to 1×10−2 torr.

54.-56. (canceled)

57. The method of claim 51, wherein the heating the getter activation region and the one or more getters to an activation temperature for an activation time suitable to activate the one or more getters comprises:

heating the getter activation region with a heat source external to the getter activation region.

58. (canceled)

59. The method of claim 51, wherein the flexing the connector comprises:

flexing a region of the connector adjacent to the getter activation region.

60. The method of claim 51, wherein the separating the connector at a location adjacent to the storage device while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device comprises:

physically crimping the connector; and
breaking the connector at the location of the physical crimping.

61. The method of claim 51, wherein the separating the connector at a location adjacent to the storage device comprises:

utilizing an ultrasonic welding device.

62. The method of claim 51, further comprising:

heating the storage device to a predetermined temperature for a predetermined length of time after establishing the gas pressure below atmospheric pressure within the gas-sealed gap of the storage device.

63. The method of claim 51, further comprising:

monitoring the gas pressure within the gas-sealed gap of the storage device.

64. The method of claim 51, further comprising:

monitoring the gas pressure within the connector.

65. The method of claim 51, further comprising:

adding sealing material to a surface of the separated connector adjacent to the storage device.
Patent History
Publication number: 20120085070
Type: Application
Filed: Sep 23, 2011
Publication Date: Apr 12, 2012
Applicant:
Inventors: Fong-Li Chou (Issaquah, WA), William Gates (Redmond, WA), Roderick A. Hyde (Redmond, WA), Edward K.Y. Jung (Bellevue, WA), Nathan P. Myhrvold (Bellevue, WA), Clarence T. Tegreene (Bellevue, WA), Charles Whitmer (North Bend, WA), Lowell L. Wood, JR. (Bellevue, WA)
Application Number: 13/200,555
Classifications
Current U.S. Class: Including Evacuating (53/408); Gas Filling And/or Evacuating Of Receptacle And Closing (53/79)
International Classification: B65B 31/04 (20060101);