Halogen Containing Compound Patents (Class 427/253)
  • Patent number: 6206967
    Abstract: A multiple step chemical vapor deposition process for depositing a tungsten film on a substrate. A first step of the deposition process includes a nucleation step in which a process gas including a tungsten-containing source, a group III or V hydride and a reduction agent are flowed into a deposition zone of a substrate processing chamber while the deposition zone is maintained at or below a first pressure level. During this first deposition stage, other process variables are maintained at conditions suitable to deposit a first layer of the tungsten film over the substrate. Next, during a second deposition stage after the first stage, the flow of the group III or V hydride into the deposition zone is stopped, and afterwards, the pressure in the deposition zone is increased to a second pressure above the first pressure level and other process parameters are maintained at conditions suitable for depositing a second layer of the tungsten film on the substrate.
    Type: Grant
    Filed: June 14, 2000
    Date of Patent: March 27, 2001
    Assignee: Applied Materials, Inc.
    Inventors: Alfred Mak, Kevin Lai, Cissy Leung, Dennis Sauvage
  • Patent number: 6207233
    Abstract: A process for forming an oxidation and corrosion resistant coating on selective surfaces of an airfoil providing a chamber having an external wall which receives a hollow sleeve for defining an internal space and an annular space between the external wall and sleeve. The airfoil to be coated is located within the internal space. An activator is provided in the internal space below the airfoil. The chemical coating composition is located in the annular space. The chamber is closed and heated to a desired temperature for a sufficient time to coat selective surfaces of the airfoil with the coated composition.
    Type: Grant
    Filed: November 23, 1998
    Date of Patent: March 27, 2001
    Assignee: United Technologies Corporation
    Inventors: Terry T. Perry, Krishnangshu Bose, David W LaFlamme, Lester J Magyar
  • Patent number: 6197436
    Abstract: A method for diffusion coating workpieces of ferrous base metals such as carbon steel and cast iron includes the step of weighing and mixing the following components, in powdered form: Chromium 40-50 wt % Ferrochromium 25-37 wt % Tantalum Carbide 0.40-0.65 wt % Vanadium 0.35-0.70 wt % Ammonium Halide 4-5 wt % Aluminum Oxide Remainder The workpieces are preferably degreased and then placed in a container with the mixed components. The container is sealed and heated to a temperature of 1000°-1050° C. The workpieces and the composition are kept at that temperature for a predetermined period, on the order of forty-five minutes or longer, to permit a surface layer of desired thickness to form. The container is then cooled in a conventional cooling chamber and the workpieces are removed. The method produces coatings having good wear and corrosion resistance.
    Type: Grant
    Filed: April 14, 1999
    Date of Patent: March 6, 2001
    Assignee: Jamar Venture Corporation
    Inventors: Inna I. Zayets, Lidia O. Chunayeva, Grigory A. Tkach
  • Patent number: 6194314
    Abstract: In chemical gaseous phase deposition (CVD=Chemical Vapor Deposition), there is frequently the problem of there still being an aggressive gas in the reaction chamber from the preceding layer production process. The aggressive gas can be a remainder of a process gas used for layer production or it can be a remainder gas produced by the reaction of the process gasses. The aggressive gas can cause undesirable reactions on the surface of the semiconductor product, which damage the semiconductor product. A process for layer production on a surface includes supplying at least one protective gas to the surface before and/or during the heating of the surface to the reaction temperature.
    Type: Grant
    Filed: February 6, 1998
    Date of Patent: February 27, 2001
    Assignee: Infineon Technologies AG
    Inventors: Wolfram Karcher, Lutz Labs
  • Patent number: 6187412
    Abstract: A silicon article including a silicon base and columns extending from the silicon base. The columns define a gap between the columns which is devoid of material so that the article can act as a filter or heat sink. Also disclosed is a method of making the silicon article.
    Type: Grant
    Filed: June 27, 1997
    Date of Patent: February 13, 2001
    Assignee: International Business Machines Corporation
    Inventors: Michael D. Armacost, Peter D. Hoh, Son V. Nguyen
  • Patent number: 6183811
    Abstract: A method for preventing the aluminizing of cooling holes and internal surfaces of an airfoil during vapor phase aluminizing. The method generally entails flowing a gas through internal cavities of the airfoil and out through the cooling holes, while the surfaces of the airfoil are aluminized by vapor phase deposition. As a result of the outward gas flow, volatile activators and aluminum compounds are prevented from flowing into the cooling holes and internal cavity, thereby preventing aluminizing of the cooling hole walls and internal surfaces of the airfoil and interactions with any oxide deposits on the surfaces of the cooling holes and internal cavities.
    Type: Grant
    Filed: December 15, 1998
    Date of Patent: February 6, 2001
    Assignee: General Electric Company
    Inventor: Jeffrey A. Conner
  • Patent number: 6180170
    Abstract: In a method for preparing and/or coating the surfaces of metallic hollow structural elements that have at least two connection openings between their outer and inner surfaces, first and second reaction gas mixtures (I, II) are prepared by reaction gas sources for treating the outer and inner surfaces of the hollow structural elements. The first reaction gas mixture (I) is guided over the outer surfaces and thereafter over the inner surfaces of the structural elements, and then the second reaction gas mixture (II) is guided over the inner surfaces and thereafter over the outer surfaces of the structural elements. An apparatus for carrying out the method includes a reaction vessel enclosing an outer reaction space, a central holding pipe arranged in the reaction vessel and enclosing an inner space, and hollow support arms removably attached on the holding pipe to extend radially outwardly therefrom.
    Type: Grant
    Filed: August 21, 1998
    Date of Patent: January 30, 2001
    Assignee: MTU Motoren- und Turbinen-Union Muenchen GmbH
    Inventors: Valentin Grossmann, Horst Pillhoefer, Martin Thoma
  • Patent number: 6177149
    Abstract: A Ti film is formed by CVD in holes formed in an insulating film formed on a Si substrate or on a Si film formed on a Si substrate by a method comprising the steps of: loading a Si substrate into a film forming chamber; evacuating the chamber at a predetermined vacuum; supplying TiCl4 gas, H2 gas, Ar gas and SiH4 gas into the film forming chamber; and producing a plasma in the film forming chamber to deposit a Ti film in the holes formed in the insulating film. The Si substrate is heated at 550° C. or above during the deposition of the Ti film, and the flow rates of the processing gases are regulated so that Si-to-insulator selectivity is not less than one. This method enables formation of a Ti film on a Si base at positions of holes in an insulating layer, with a good morphology of the interface between the Si base and the Ti film and with a good step coverage.
    Type: Grant
    Filed: December 21, 1998
    Date of Patent: January 23, 2001
    Assignee: Tokyo Electron Limited
    Inventors: Kunihiro Tada, Hayashi Otsuki
  • Patent number: 6171661
    Abstract: A method and apparatus for improving the adhesion of a copper layer to an underlying layer on a wafer. The layer of copper is formed over a layer of material on a wafer and the copper layer impacted with ions to improve its adhesion to the underlying layer.
    Type: Grant
    Filed: February 25, 1998
    Date of Patent: January 9, 2001
    Assignee: Applied Materials, Inc.
    Inventors: Bo Zheng, Ling Chen, Alfred Mak, Mei Chang
  • Patent number: 6169031
    Abstract: In-situ prepared TiCl2 and TiCl3 precursors to form titanium metal thin film by chemical vapor deposition at 350˜800° C. Due to the low decomposition temperature of TiCl2 and TiCl3, titanium metal thin films were obtained at very low temperature with the by-product, TiCl4, which could be reused to prepare TiCl2 and TiCl3.
    Type: Grant
    Filed: May 28, 1999
    Date of Patent: January 2, 2001
    Assignee: National Science Council
    Inventor: Chi-Young Lee
  • Patent number: 6156382
    Abstract: A multiple step chemical vapor deposition process for depositing a tungsten layer on a substrate. A first step of the deposition process includes a nucleation step in which WF.sub.6 and SiH.sub.4 are introduced into a deposition chamber. Next, the flow of WF.sub.6 and SiH.sub.4 are stopped and diborane is introduced into the chamber for between 5-25 seconds. Finally, during a bulk deposition step, the WF.sub.6 is reintroduced into the chamber along with H.sub.2 and B.sub.2 H.sub.6 flows to deposit a tungsten layer on the substrate. In a preferred embodiment, the bulk deposition step also introduces nitrogen into the process gas.
    Type: Grant
    Filed: May 16, 1997
    Date of Patent: December 5, 2000
    Assignee: Applied Materials, Inc.
    Inventors: Ravi Rajagopalan, Steve Ghanayem, Manabu Yamazaki, Keiichi Ohtsuka, Yuji Maeda
  • Patent number: 6146696
    Abstract: A process for simultaneously vapor phase aluminizing nickel-base and cobalt-base superalloys within a single process chamber using the same aluminum donor and activator, to yield diffusion aluminide coatings of approximately equal thickness. The process entails the use of an aluminum donor containing about 50 to about 60 weight percent aluminum, and an aluminum fluoride activator present in an amount of at least 1 gram per liter of coating chamber volume. Nickel-base and cobalt-base superalloys are simultaneously vapor phase aluminized for 4.5 to 5.5 hours at a temperature of about 1900.degree. F. to about 1950.degree. F. in an inert or reducing atmosphere. With these materials and process parameters, diffusion aluminide coatings are developed on both superalloys whose thicknesses do not differ from each other by more than about 30%.
    Type: Grant
    Filed: May 26, 1999
    Date of Patent: November 14, 2000
    Assignee: General Electric Company
    Inventors: Nripendra N. Das, Patricia A. Charles, Raymond W. Heidorn
  • Patent number: 6143361
    Abstract: Method and apparatus for controlling deposition from excess gaseous reactant in an exhaust conduit of a chemical vapor deposition apparatus involves introducing a gaseous chemical reactant in the exhaust stream effective to react with the excess gaseous reactant in the exhaust stream to form solid reaction product particulates in a manner that reduces harmful deposition of liquid and/or solid metal in the exhaust system.
    Type: Grant
    Filed: October 19, 1998
    Date of Patent: November 7, 2000
    Assignee: Howmet Research Corporation
    Inventors: Daniel L. Near, Bruce M. Warnes, Stephen M. Winters
  • Patent number: 6143362
    Abstract: A titanium layer is formed on a substrate with chemical vapor deposition (CVD). First, a seed layer is formed on the substrate by combining a first precursor with a reducing agent by CVD. Then, the titanium layer is formed on the substrate by combining a second precursor with the seed layer by CVD. The titanium layer is used to form contacts to active areas of substrate and for the formation of interlevel vias.
    Type: Grant
    Filed: February 25, 1998
    Date of Patent: November 7, 2000
    Assignee: Micron Technology, Inc.
    Inventors: Gurtej Singh Sandhu, Donald L. Westmoreland
  • Patent number: 6139922
    Abstract: A method for chemical vapor deposition of a film comprising tantalum onto a substrate includes introducing into a deposition chamber: (i) a substrate; (ii) a source precursor in the vapor state; and (iii) a reactant gas, and maintaining the temperature of the substrate within the chamber as from about 70.degree. C. to about 675.degree. C. for a period of time sufficient to deposit a film comprising tantalum on the substrate. The source precursor has a formula (I):Ta(F.sub.5-q-p)(X.sub.q-p)(R.sub.p) (I)wherein X is selected from the group consisting of bromine, iodine, chlorine, and combinations thereof; q is an integer from 0 to 4; p is an integer from 0 to 4; and R is selected from the group consisting of hydrogen and lower alkyl.
    Type: Grant
    Filed: May 18, 1999
    Date of Patent: October 31, 2000
    Assignees: Gelest, Inc., The Research Foundation of State University of New York
    Inventors: Alain E. Kaloyeros, Barry C. Arkles
  • Patent number: 6129991
    Abstract: High temperature oxidation resistance of an aluminide diffusion overcoated MCrAlY coating system is substantially improved by CVD over-aluminizing the MCrAlY type overlay coating under CVD conditions that result in reduced concentrations of such tramp impurities as S and P in the aluminized MCrAlY overlay coating region of the coating system. The CVD aluminizing conditions yield an outwardly grown aluminide over-coat on the underlying MCrAlY type coating.
    Type: Grant
    Filed: August 14, 1997
    Date of Patent: October 10, 2000
    Assignee: Howmet Research Corporation
    Inventors: Bruce M. Warnes, William J. Shriver, Ronald J. Honick, Jr., Nick S. DuShane
  • Patent number: 6120843
    Abstract: In a method for coating workpieces with a coating material by a gas phase diffusion coating process, the coating material is conveyed in the form of a metal halide compound from a coating material source (9A, 9B, 9C) to the workpiece (7) by means of a metal halide gas circulation flow (F). The gas circulation flow (F) is physically induced due to convection by establishing a temperature gradient between the workpiece (7) and the coating material source (9A, 9B, 9C), and is reinforced by the chemical reactions taking place. An apparatus for carrying out a gas phase diffusion process includes a reaction vessel (3) enclosing a reaction chamber (1) in which the workpiece (7) is arranged. The apparatus further includes a metal halide generator (9A, 9B, 9C) arranged in the reaction chamber (1), and a heater (5) as well as a cooling device (6) and a thermal conduction arrangement (8) for establishing a temperature gradient between the workpiece (7) and the metal halide generator (9A, 9B, 9C).
    Type: Grant
    Filed: July 13, 1998
    Date of Patent: September 19, 2000
    Assignee: MTU Motoren- und Turbinen-Union Muenchen GmbH
    Inventors: Horst Pillhoefer, Martin Thoma
  • Patent number: 6120842
    Abstract: A process for producing conformal and stable TiN+Al films, which provides flexibility in selecting the chemical composition and layering. In this new process, porous TiCN is first deposited, and then Al is incorporated by exposing the porous film to CVD aluminum conditions at low temperatures.
    Type: Grant
    Filed: October 21, 1997
    Date of Patent: September 19, 2000
    Assignee: Texas Instruments Incorporated
    Inventors: Jiong-Ping Lu, Wei-Yung Hsu, Qi-Zhong Hong
  • Patent number: 6117772
    Abstract: A method and apparatus for metal-organics chemical vapor deposition (MO CVD) of a metal layer upon a spherical substrate at atmospheric pressure are disclosed. The method includes pretreating the spherical substrate with a vapor of a first precursor in preparation for a deposition of a metal layer. The pretreated spherical substrate is then exposed to a thermally dissociated precursor of metal for depositing the metal layer onto the spherical substrate, wherein the exposure to the thermally dissociated precursor of metal provides a uniformly deposited metal layer coverage over the pretreated spherical substrate. The deposited metal layer is then annealed and cooled.
    Type: Grant
    Filed: July 10, 1998
    Date of Patent: September 12, 2000
    Assignee: Ball Semiconductor, Inc.
    Inventors: Ivan Herman Murzin, Toshiyuki Sakuma, Ajay Tapiawala
  • Patent number: 6113983
    Abstract: A new low temperature method for nanostructured metal and ceramic thin film growth by chemical vapor deposition (CVD) involves the use of a low pressure co-flow diffusion flame reactor to react alkali metal vapor and metal halide vapor to deposit metal, alloy and ceramic films. The reaction chemistry is described by the following general equation:(mn)Na+nMX.sub.m .fwdarw.(M).sub.n +(nm)NaXwhere Na is sodium, or another alkali metal (e.g., K, Rb, Cs), and MX.sub.m is a metal-halide (M is a metal or other element such as Si, B or C; X is a halogen atom, e.g., chlorine, fluorine or the like; and m and n are integers). This reaction chemistry is a viable technique for thin film growth. In one mode, using the precursors of sodium metal vapor, titanium tetrachloride (the limiting reagent), and either argon or nitrogen gases, titanium (Ti), titanium nitride (TiN), titanium dioxide (TiO.sub.2), and titanium silicide (TiSi, Ti.sub.5 Si.sub.3, TiSi.sub.2, Ti.sub.5 Si.sub.
    Type: Grant
    Filed: April 3, 1998
    Date of Patent: September 5, 2000
    Assignee: The United States of America as represented by the Secretary of Commerce
    Inventors: Michael R. Zachariah, Jay H. Hendricks
  • Patent number: 6110530
    Abstract: Copper films having improved properties are deposited by chemical vapor deposition from an organocopper precursor of a blend of copper hexafluoroacetylacetonate trimethylvinylsilane and from about 1.0 to 5.0 percent by weight of trimethylvinylsilane that is vaporized in a vaporizer, and passed into a chemical vapor deposition chamber. Separately up to about 2 percent by weight of the precursor blend of water vapor is added directly to the chamber.
    Type: Grant
    Filed: June 25, 1999
    Date of Patent: August 29, 2000
    Assignee: Applied Materials, Inc.
    Inventors: Ling Chen, Seshadri Ganguli, Bo Zheng, Samuel Wilson, Christophe Marcadal
  • Patent number: 6099904
    Abstract: A multiple step chemical vapor deposition process for depositing a tungsten film on a substrate. A first step of the deposition process includes a nucleation step in which a process gas including a tungsten-containing source, a group III or V hydride and a reduction agent are flowed into a deposition zone of a substrate processing chamber while the deposition zone is maintained at or below a first pressure level. During this first deposition stage, other process variables are maintained at conditions suitable to deposit a first layer of the tungsten film over the substrate. Next, during a second deposition stage after the first stage, the flow of the group III or V hydride into the deposition zone is stopped, and afterwards, the pressure in the deposition zone is increased to a second pressure above the first pressure level and other process parameters are maintained at conditions suitable for depositing a second layer of the tungsten film on the substrate.
    Type: Grant
    Filed: December 2, 1997
    Date of Patent: August 8, 2000
    Assignee: Applied Materials, Inc.
    Inventors: Alfred Mak, Kevin Lai, Cissy Leung, Dennis Sauvage
  • Patent number: 6086951
    Abstract: A method of forming metallic capacitor. The method includes forming a lower electrode for forming the capacitor and a metal conductive line over an inter-layer dielectric such that there are gaps between and on the sides of the lower electrode and the metal conductive line. Thereafter, a first oxide layer is formed that fills the gap, and then a second oxide layer is formed over the inter-layer dielectric. The second oxide layer is later patterned to form a cap oxide layer having an opening that exposes a portion of the lower electrode. Subsequently, a thin dielectric layer is formed over the lower electrode and the cap oxide layer. Finally, an upper electrode is formed over the thin dielectric layer filling the opening.
    Type: Grant
    Filed: June 14, 1999
    Date of Patent: July 11, 2000
    Assignee: United Microelectronics Corp.
    Inventors: Chen-Bin Lin, Cheng-Hui Chung, Yu-Ju Liu
  • Patent number: 6077571
    Abstract: The present invention relates to a process and apparatus for the formation of conformal pure aluminum and doped aluminum coatings on a patterned substrate. It is directed to the use of low temperature thermal and plasma-promoted chemical vapor deposition techniques with biased substrate to provide conformal layers and bilayers comprised of pure Al and/or doped Al (e.g., Al with 0.5 at % copper) on semiconductor device substrates with patterned holes, vias, and trenches with aggressive aspect ratios (hole depth/hole width ratios). The use of the plasma-promoted CVD (PPCVD) process, which employs low plasma power densities, allows the growth of aluminum films with the smooth surface morphology and small grain size necessary for ULSI applications, while substrate bias provides superior coverage and complete aluminum fill of features intrinsic in microelectronic device manufacture.
    Type: Grant
    Filed: December 19, 1995
    Date of Patent: June 20, 2000
    Assignee: The Research Foundation of State University of New York
    Inventors: Alain E. Kaloyeros, Jonathan Faltermeier
  • Patent number: 6074945
    Abstract: The present invention provides methods for the preparation of ruthenium metal films from liquid ruthenium complexes of the formula (diene)Ru(CO).sub.3 wherein "diene" refers to linear, branched, or cyclic dienes, bicyclic dienes, tricyclic dienes, fluorinated derivatives thereof, derivatives thereof additionally containing heteroatoms such as halide, Si, S, Se, P, As, N, or 0, or combinations thereof.
    Type: Grant
    Filed: August 27, 1998
    Date of Patent: June 13, 2000
    Assignee: Micron Technology, Inc.
    Inventors: Brian A. Vaartstra, Eugene P. Marsh
  • Patent number: 6066366
    Abstract: Within wafer and wafer-to-wafer uniformity of W layers deposited by CVD, employing N.sub.2 for increased reflectivity, is significantly improved by omitting N.sub.2 during at least a portion of deposition. Embodiments include depositing a W nucleation layer on a TiN layer employing gaseous WF.sub.6 during a nucleation phase, omitting WF.sub.6 during an interposition phase during which substantially no W deposition occurs, depositing a W layer employing gaseous WF.sub.6 during a main deposition phase, flowing N.sub.2 gas at least during the terminal portion of the main deposition phase and omitting N.sub.2 gas during at least a portion of the nucleation phase and/or interposition phase, e.g., omitting N.sub.2 gas during the entire interdeposition phase.
    Type: Grant
    Filed: July 22, 1998
    Date of Patent: May 23, 2000
    Assignee: Applied Materials, Inc.
    Inventors: Daniel Berenbaum, David A. Duke, Herald Hauf, Richard Petri, Jean-Christopher Favreau
  • Patent number: 6063442
    Abstract: A process for bonding a porous material having an opened porous cellular structure to a substrate material, the process including the steps of: conditioning the substrate with tantalum in a reactor at 925.degree. C. having a tantalum source pot at 550.degree. C.; affixing the porous material to the conditioned substrate to form an affixed composite structure by clamping the porous material to the conditioned substrate; and, subjecting the composite structure to a chemical vapor deposition process (CVD) which uses tantalum as a source material for a time sufficient to CVD bond the porous material to the conditioned substrate material.
    Type: Grant
    Filed: October 26, 1998
    Date of Patent: May 16, 2000
    Assignee: Implex Corporation
    Inventors: Robert C. Cohen, Joseph R. Vargas
  • Patent number: 6063705
    Abstract: A method is provided for forming a film of ruthenium or ruthenium oxide on the surface of a substrate by employing the techniques of chemical vapor deposition to decompose precursors of ruthenium having the formula: L.sub.y RuX.sub.z where L is a neutral or monoanionic ligand selected from the group consisting essentially of linear hydrocarbyls, branched hydrocarbyls, cyclic hydrocarbyls, cyclic alkenes, dienes, cyclic dienes, trienes, cyclic trienes, bicyclic alkenes, bicyclic dienes, bicyclic trienes, tricyclic alkenes, tricyclic dienes, tricyclic trienes; fluorinated derivatives thereof; derivatives thereof additionally containing heteroatoms such as a halide, Si, S, Se, P, As, N or O; and combinations thereof; where X is a pi-bonding ligand selected from the group consisting of CO, NO, CN, CS, nitriles, isonitriles, trialkylphosphines, trialkylphosphites, trialkylamines, and isocyanide, and where subscripts y and z have a value of from one (1) to three (3); or L.sub.1 Ru(CO).sub.
    Type: Grant
    Filed: August 27, 1998
    Date of Patent: May 16, 2000
    Assignee: Micron Technology, Inc.
    Inventor: Brian A. Vaartstra
  • Patent number: 6063453
    Abstract: An electron-emitting device having an electroconductive film including an electron-emitting region and arranged between a pair of electrodes is manufactured by forming an electroconductive film on a substrate and producing an electron-emitting region in the electroconductive film. The electroconductive film is formed on the substrate by heating the substrate in an atmosphere containing a gasified organic metal compound to a temperature higher than the decomposition of the gasified organic metal compound.
    Type: Grant
    Filed: October 30, 1997
    Date of Patent: May 16, 2000
    Assignee: Canon Kabushiki Kaisha
    Inventors: Yoshinori Tomida, Hisaaki Kawade, Masahito Niibe, Toshikazu Ohnishi, Yoshimasa Okamura
  • Patent number: 6051286
    Abstract: The present invention provides systems, methods and apparatus for depositing titanium films at rates up to 200 .ANG./minute on semiconductor substrates from a titanium tetrachloride source. In accordance with an embodiment of the invention, a ceramic heater assembly with an integrated RF plane for bottom powered RF capability allows PECVD deposition at a temperature of at least 400.degree. C. for more efficient plasma treatment. A thermal choke isolates the heater from its support shaft, reducing the thermal gradient across the heater to reduce the risk of breakage and improving temperature uniformity of the heater. A deposition system incorporates a flow restrictor ring and other features that allow a 15 liters/minute flow rate through the chamber with minimal backside deposition and minimized deposition on the bottom of the chamber, thereby reducing the frequency of chamber cleanings, and reducing clean time and seasoning. Deposition and clean processes are also further embodiments of the present invention.
    Type: Grant
    Filed: August 22, 1997
    Date of Patent: April 18, 2000
    Assignee: Applied Materials, Inc.
    Inventors: Jun Zhao, Lee Luo, Xiao Liang Jin, Jia-Xiang Wang, Stefan Wolff, Talex Sajoto
  • Patent number: 6051281
    Abstract: A method of forming a titanium film and a titanium nitride film on a substrate by lamination which method is capable of suppressing contamination of the substrate due to the by-product and of reducing a contact resistance value of the titanium film. By carrying out the step of forming a titanium film on a surface of a substrate, the step of subjecting the substrate to the plasma processing in an atmosphere of the mixed gas of nitrogen gas and hydrogen gas, thereby nitriding a surface layer of the titanium film to form thereon a nitride layer, and the step of forming a barrier film (e.g., a titanium nitride film) on the titanium film having the nitride layer formed thereon, both the titanium film and the titanium nitride film are formed on the substrate by lamination.
    Type: Grant
    Filed: September 30, 1997
    Date of Patent: April 18, 2000
    Assignee: Tokyo Electron Limited
    Inventors: Yasuo Kobayashi, Kunihiro Tada, Hideki Yoshikawa
  • Patent number: 6045863
    Abstract: The invention includes a low activity localized aluminide coating for a metallic article made by positioning a coating material, preferably in the form of a tape, on a portion of the article. The coating material comprises a binder, a halide activator, an aluminum source, and an inert ceramic material. The coating material and the article are heated in an inert atmosphere between about 1800.degree. F. (982.degree. C.) and about 2050.degree. F. (1121.degree. C.) for between about four and about seven hours thereby producing a low activity localized aluminide coating having an outward diffusion aluminide coating microstructure characterized by two distinct zones, an inner diffusion zone and an outer zone including between about 20-28 percent, by weight, aluminum.
    Type: Grant
    Filed: November 18, 1997
    Date of Patent: April 4, 2000
    Assignee: United Technologies Company
    Inventors: Walter E. Olson, Norman Pietruska, Peter Jon Draghi
  • Patent number: 6040010
    Abstract: Methods and apparatus for depositing films on semiconductor wafers in chemical vapor deposition processes employing a catalyst to provide one or more activated gases to reduce the surface temperature of the semiconductor wafer needed to form the film thereon. The activated gas precursors can include hydrogen or hydrogen-bearing gases. The catalysts can be selected from ruthenium, rhodium, palladium, osmium, iridium, platinum, gold, silver, mercury, rhenium, copper, tungsten, and combinations thereof.
    Type: Grant
    Filed: September 10, 1996
    Date of Patent: March 21, 2000
    Assignee: Micron Technology, Inc.
    Inventors: Anand Srinivasan, Gurtej S. Sandhu
  • Patent number: 6040021
    Abstract: A plasma CVD process for a metal film made from Ti or the like and a formation process of a metal nitride film made from TiN or the like. Each process solves problems on asymmetry of a film shape at an opening portion of a contact hole, corrosion of an underlaying material layer, remaining halogen in the film, and peeling of the film. In the plasma CVD using a mixed gas containing TiCl.sub.4, H.sub.2 and Ar, species for forming a Ti film is efficiently ionized and the Ti ions thus generated are made incident on a substrate to be processed in the direction substantially perpendicular to the substrate, to thus form a metal film being good in coverage. A metal nitride film having a specific thickness is formed by repeating the step of forming such a metal film and the step of nitriding the metal film by plasma nitriding.
    Type: Grant
    Filed: December 19, 1997
    Date of Patent: March 21, 2000
    Assignee: Sony Corporation
    Inventor: Takaaki Miyamoto
  • Patent number: 6033493
    Abstract: Surface preoxidation of the substrate is carried out by bringing the substrate into contact with an oxidizing gas excited by a cold plasma, the substrate being situated in the flowing afterglow of the cold plasma used to excite the oxidizing element and being heated to an oxidation temperature of less than 500.degree. C. A metal oxide is formed at the surface of the preoxidized substrate by heterogeneous oxidation of a metal halide with a gas mixture including an oxidizing element activated by a cold plasma. The oxidizing gas mixture is brought into contact with the halide as directly as possible in the vicinity of the substrate arranged in the far flowing afterglow of the cold plasma. The cold plasma is preferably generated by microwaves. The process can be used in particular for producing a protective coating on a cladding tube of a nuclear fuel rod.
    Type: Grant
    Filed: October 28, 1997
    Date of Patent: March 7, 2000
    Assignees: Framatome, Cogema Velizy
    Inventors: Dominique Hertz, Thierry Belmonte, Jerome Gavillet, Henri Michel
  • Patent number: 5972429
    Abstract: A method of diffusion coating a surface of an alloy product containing at least 5 wt. % iron with a chromium-silicon coating uses a dual activator containing a fluoride salt and a chloride salt, at least one of those salts particularly being ammonium chloride or another ammonium halide salt. The pack mix contain at least 20% chromium and a chromium to silicon ratio of at least 10 to 1. The workpiece is heated to at least 2050.degree. F. to obtain a coating of at least 10 mils which contains at least 30% chromium. Upon heating the ammonium salt will form a reducing environment containing molecular hydrogen. The presence of molecular hydrogen speeds up the chemical reactions by an additional reduction reaction to create the surface coating which enables the coating reactions to occur shorter hold times.
    Type: Grant
    Filed: November 3, 1997
    Date of Patent: October 26, 1999
    Assignee: Alon, Inc.
    Inventors: George T. Bayer, Kim A. Wynns
  • Patent number: 5958152
    Abstract: To provide heat-resistant alloy members that maintain the resistance to corrosion at high temperature of the chromized layer formed on Ni- or Co-base heat-resistant alloys and which yet are improved in various mechanical properties. The improved Ni- or Co-base heat-resistant alloy member having a chromized layer that is characterized by having a chromium concentration of 25-80% and a thickness of 10-100 .mu.m. This member is produced by controlling both the vapor pressure of a chromium halide being used in chromization and the temperature therefor in such a way that the chromized layer being formed is adjusted to have a chromium concentration and a thickness within the ranges specified above.
    Type: Grant
    Filed: May 23, 1997
    Date of Patent: September 28, 1999
    Assignees: Ebara Corporation, Tocalo Co., Ltd.
    Inventors: Shuhei Nakahama, Hisamichi Nagahara, Masamichi Kawasaki, Yoshio Harada
  • Patent number: 5942282
    Abstract: A first pre-coating film forming gas containing titanium is supplied into a process chamber in which a susceptor for supporting a wafer is located, at the same time heating the susceptor to thereby form, on the susceptor, a first pre-coating film containing titanium as a main component, and then a second pre-coating film forming gas containing titanium and nitrogen is supplied into the process chamber to thereby form, on the pre-coating first film, a second pre-coating film containing titanium nitride as a main component. The wafer is mounted on a part of the second pre-coating film susceptor. A first film forming gas containing titanium is supplied into the process chamber, at the same time heating the susceptor to thereby form, on the wafer, a first film containing titanium as a main component, and then a second film forming gas containing titanium and nitrogen is supplied into the process chamber to thereby form, on the first film on the wafer, a second film containing titanium nitride as a main component.
    Type: Grant
    Filed: May 4, 1998
    Date of Patent: August 24, 1999
    Assignee: Tokyo Electron Limited
    Inventors: Kunihiro Tada, Yoshihiro Tezuka, Kazuichi Hayashi
  • Patent number: 5939144
    Abstract: The present invention provides a composition and method for use in diffusion coating ceramic workpieces. In an especially preferred form, the composition comprises:Chromium 45-50 wt %Silicon Carbide 3.5-5.0 wt %Vanadium Boride 0.5-1.5 wt %Ammonium Halide 5.0-6.0 wt %Aluminum Oxide Remainder,the sum of all the components being 100 wt %. The components, in powdered form, are weighed and mixed in a container. The workpieces are placed in the container. The container is hermetically sealed and heated to a temperature of approximately 1000.degree. C. The workpieces and the composition are kept at approximately 1000.degree. C. for a predetermined period of time sufficient to permit a surface layer of desired thickness to form. The container is then cooled in a conventional cooling chamber down to approximately 300.degree.-350.degree. C. and air cooled to room temperature. The container is opened and the workpieces are removed.
    Type: Grant
    Filed: October 23, 1997
    Date of Patent: August 17, 1999
    Assignee: Jamar Venture Corporation
    Inventors: Inna I. Zayets, Lidia O. Chunayeva, Grigory A. Tkach
  • Patent number: 5925411
    Abstract: A platen supports a substrate on an interior platen region during the deposition of materials such as tungsten, metal nitrides, other metals, and silicides in a chemical vapor deposition ("CVD") reactor. A deposition control gas composed of a suitable inert gas such as argon or a mixture of inert and reactive gases such as argon and hydrogen is introduced into the CVD reactor. Deposition control gas is preferably introduced through a restrictive opening in a gas orifice surrounding the platen interior region and exits near an edge of the substrate. The restrictive opening accommodates a uniform deposition control gas flow proximate to an edge of the substrate at a pressure greater than reactor pressure near the substrate edge. The deposition control gas substantially prevents process gas access to the substrate edge and backside. In one embodiment, the restrictive opening is formed by placing a restrictive insert within a gas groove surrounding the platen interior region.
    Type: Grant
    Filed: June 7, 1995
    Date of Patent: July 20, 1999
    Assignee: Siliconix incorporated
    Inventors: Everhardus P. van de Ven, Eliot K. Broadbent, Jeffrey C. Benzing, Barry L. Chin, Christopher W. Burkhart
  • Patent number: 5919531
    Abstract: A method for chemical vapor deposition of a film comprising tantalum onto a substrate includes introducing into a deposition chamber: (i) a substrate; (ii) a source precursor in the vapor state; and (iii) at least one carrier gas, and maintaining the temperature of the substrate within the chamber as from about 70.degree. C. to about 675.degree. C. for a period of time sufficient to deposit a film comprising tantalum on the substrate. The source precursor has a formula (I):Ta(I.sub.5-m-n-p)(Br.sub.m- p)(Cl.sub.n- p)(R.sub.p) (I)wherein m is an integer from 0 to 5, n is an integer from 0 to 4, p is an integer from 0 to 4, and R is selected from the group consisting of hydrogen, and lower alkyl.
    Type: Grant
    Filed: March 26, 1997
    Date of Patent: July 6, 1999
    Assignees: Gelest, Inc., The Research Foundation of State University of New York
    Inventors: Barry C. Arkles, Alain E. Kaloyeros
  • Patent number: 5882439
    Abstract: To provide heat-resistant alloy members that maintain the resistance to corrosion at high temperature of the chromized layer formed on Ni- or Co-base heat-resistant alloys and which yet are improved in various mechanical properties. The improved Ni- or Co-base heat-resistant alloy member having a chromized layer that is characterized by having a chromium concentration of 25-80% and a thickness of 10-100 .mu.m. This member is produced by controlling both the vapor pressure of a chromium halide being used in chromization and the temperature therefor in such a way that the chromized layer being formed is adjusted to have a chromium concentration and a thickness within the ranges specified above.
    Type: Grant
    Filed: September 11, 1996
    Date of Patent: March 16, 1999
    Assignees: Ebara Corporation, Tocalo Co., Ltd.
    Inventors: Syuhei Nakahama, Hisamichi Nagahara, Masamichi Kawasaki, Yoshio Harada
  • Patent number: 5840366
    Abstract: A W film having good surface morphology and high reflectance is formed while avoiding any degradation of the characteristics such as specific resistivity. The method for forming a thin film is carried out by depositing a W film on a heated substrate using CVD. The raw material gas is WF.sub.6, and the reducing gases are SiH.sub.4 and H.sub.2. In the first stage of the film formation, the reaction between WF.sub.6 and SiH.sub.4 forms nuclei on the surface of the substrate. In the second stage, following the first stage, the reaction between WF.sub.6 and H.sub.2 forms the W film. The second stage is controlled to form crystal grains of a predetermined size. The first stage and the second stage are alternately repeated as many times as necessary.
    Type: Grant
    Filed: August 28, 1995
    Date of Patent: November 24, 1998
    Assignee: Anelva Corporation
    Inventors: Shigeru Mizuno, Akihiko Koura
  • Patent number: 5803991
    Abstract: In manufacturing a corrosion-resistant metallic porous member having high Cr content by diffusion process in which the material is heat-treated, a plurality of heat cycles are used to achieve uniform Cr content in the thickness direction. Metallic porous body of Ni, Fe, Ni-Cr or Fe-Cr is buried in a powder of Al, Cr and NH.sub.4 Cl. Inert gas such as Ar and H.sub.2 is introduced and the porous body is heat treated at 800.degree.-1100.degree. C. In the heat treatment, at least two temperature-increase and temperature-decrease steps are included.
    Type: Grant
    Filed: September 11, 1996
    Date of Patent: September 8, 1998
    Assignee: Sumitomo Electric Industries, Ltd.
    Inventors: Toshiyasu Tsubouchi, Satoru Okamoto, Tomohiko Ihara
  • Patent number: 5795824
    Abstract: A tungsten (W) film is formed on a surface of a semiconductor substrate by providing to that surface gas mixtures tailored for both reduced gas phase nucleation of particulates (GPN) and attack of exposed silicon (Si) or titanium (Ti) surfaces (Device Attack) while maintaining a high W deposition rate. An initiation step is performed where the surface is preconditioned with hydrogen (H.sub.2) and silane (SiH.sub.4). A subsequent nucleation step then uses a mixture of H.sub.2 and SiH.sub.4 to reduce tungsten hexafluoride (WF.sub.6) and thus form a first thickness of the W film. In some embodiments, an alternate gas mixture can be employed to form a second thickness of W on the surface of the semiconductor substrate.
    Type: Grant
    Filed: August 28, 1997
    Date of Patent: August 18, 1998
    Assignee: Novellus Systems, Inc.
    Inventor: Shawn Diane Hancock
  • Patent number: 5763008
    Abstract: This invention is directed to the creation of crystalline mullite coatings having uniform microstructure by chemical vapor deposition (CVD). The process comprises the steps of establishing a flow of reactants which will yield mullite in a CVD reactor, and depositing a crystalline coating from the reactant flow. The process will yield crystalline coatings which are dense and of uniform thickness.
    Type: Grant
    Filed: January 6, 1995
    Date of Patent: June 9, 1998
    Assignee: Trustees of Boston University
    Inventors: Vinod Sarin, Rao Mulpuri
  • Patent number: 5747112
    Abstract: A process for the production of a heat- and corrosion-resistant porous metal body which is made of a metal or whose surface layer is made of a metal, in which the porous metal body can be alloyed with chromium or a combination of chromium and aluminum uniformly throughout the entire thereof by adjusting the alloy composition in the following manner, i.e., (A) heat-treating the porous metal body in a mixed gas comprising a gas, generated by heating a powdered mixture comprising chromium or its compound and NH.sub.4 Cl at 950.degree. to 1100.degree. C., and a diluent reducing gas at 800.degree. to 1100.degree. C, or (B) heat-treating the porous metal body in a mixed gas comprising a gas, generated by heating a powdered mixture comprising aluminum or its compound, chromium or its compound and NH.sub.4 X, wherein X is I, F, Cl or Br, at a weight ratio of the chromium or its compound to the aluminum or its compound of 10 to 80 in terms of Cr and Al respectively at 950.degree. to 1100.degree. C.
    Type: Grant
    Filed: September 9, 1996
    Date of Patent: May 5, 1998
    Assignee: Sumitomo Electric Industries, Ltd.
    Inventors: Toshiyasu Tsubouchi, Satoru Okamoto, Tomohiko Ihara
  • Patent number: 5736192
    Abstract: An embedded electroconductive layer is disclosed which comprises an opening part or a depressed part 3 formed in an insulating film 2 on a substrate 1, a barrier layer for covering the opening part or the depressed part, a metal growth promoting layer 5 on the barrier layer, and an electroconductive layer 6 embedded in the opening part or the depressed part via the barrier layer 4 and the metal growth promoting layer 5.
    Type: Grant
    Filed: June 7, 1996
    Date of Patent: April 7, 1998
    Assignee: Fujitsu Limited
    Inventor: Shigeru Okamoto
  • Patent number: 5700519
    Abstract: A method is provided for depositing ultra high purity of greater than 99.998% titanium films which comprises generating gaseous TiI.sub.4 in situ by reacting titanium metal starting material with gaseous iodide in a reaction chamber, purifying the TiI.sub.4 by a double distillation process at reduced pressure to produce ultra high purity of greater than 99.998% TiI.sub.4, transferring the ultra high purity TiI.sub.4 in liquid form to a deposition chamber to vaporize the liquid TiI.sub.4 and contacting a heated titanium substrate with the TiI.sub.4 vapor, thereby depositing the ultra high purity Ti films on the substrate.
    Type: Grant
    Filed: January 6, 1995
    Date of Patent: December 23, 1997
    Assignees: Sony Corporation, Materials Research Corp.
    Inventor: Raymond K. F. Lam
  • Patent number: RE36330
    Abstract: The present invention provides an electroless process for making a catalyst in a liquid or gaseous medium comprising contacting a base metal with a chemical cleaning agent and simultaneously or sequentially treating said base metal under reducing conditions with a noble metal-containing material, the catalyst prepared using the process, and a method of using the catalyst.
    Type: Grant
    Filed: July 16, 1998
    Date of Patent: October 5, 1999
    Assignee: Witco Corporation
    Inventors: James S. Ritscher, Wei T. Yang, George M. Omietanski, Robert L. Ocheltree, Earl E. Malson