Manganese (e.g., Manganate, Etc.) Patents (Class 423/599)
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Patent number: 6207130Abstract: A method has been developed for the solution-based metal exchange of carboxylato-alumoxanes [Al(O)x(OH)y(O2CR)z]n with a wide range of metal cations. Metal-exchanged carboxylato-alumoxanes are new, particularly those in which about 10% to about 50% or more of the Al ions are exchanged for other metal ions. Additionally, the carboxylic acid ligands can be stripped from the boehmite core of metal-exchanged carboxylato-alumoxanes at low temperature leading to the formation of metal-exchanged boebmite particles. These new material phases can be used as intermediates for preparation of mixed metal aluminum oxide materials. Thermolysis of the metal-exchanged carboxylato-alumoxanes or metal-exchanged boehmite particles results in doped aluminas (M/Al2O3), binary (MAlOx), ternary (MM′AlOx) and even more complex metal aluminum oxide compounds, where M and M′ are metal ions other than those of aluminum and are preferably those of Lanthanide metals or transition metals.Type: GrantFiled: April 10, 1998Date of Patent: March 27, 2001Assignees: Rice University, TDA Research, Inc.Inventors: Aivaras Kareiva, Chuansheng Bai, Charles Jeffrey Harlan, D. Brent MacQueen, Andrew R. Barron, Ronald L. Cook
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Patent number: 6197719Abstract: A process for the activation of perovskite-type oxide by increasing its surface area and/or catalytic activity, which comprises: (i) treating perovskite-type oxide hydrothermally with liquid water with water/perovskite-type oxide ratio of above 0.1 at temperature of 50°-500° C. and period of 0.1-100 h under autogeneous pressure and drying the resulting mass or treating perovskite-type oxide hydrothermally with water vapors with or without any inert gas at space velocity of above 100 h−1, temperature of 200°-1000° C. and a period of 0.1-100 h and (ii) calcining the hydrothermally treated perovskite-type oxide in air or inert gas or under vacuum at temperature of 300°-1000° C. for a period of 0.1-100 h.Type: GrantFiled: April 1, 1999Date of Patent: March 6, 2001Assignee: Council of Scientific and Industrial ResearchInventors: Vasant Ramchandra Choudhary, Subhabrata Banerjee
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Patent number: 6193946Abstract: Lithium composite metal oxides prepared by mixing at least one type of hydroxides, oxides, and carbonates of a metal selected from the group of transition metal, IIA metal, and IIIA metal, and a lithium compound of which the D50 value is in the range 5 to 50 &mgr;m, the D90 value is 90 &mgr;m or smaller, and in which particles 100 &mgr;m or greater do not exist, and calcining in the temperature range 700 to 1000° C. for 2 to 30 hours, and grinding, are used as the active material of a positive electrode which is laminated with a negative electrode with a separator interposed and spirally wound thereby forming an electrode group. By using the positive active materials prepared in this manner, discharge capacity and cycle characteristic of a non-aqueous electrolyte secondary cell can be improved.Type: GrantFiled: March 1, 1999Date of Patent: February 27, 2001Assignee: Matsushita Electric Industrial Co., Ltd.Inventors: Tomoko Kawano, Shigeo Kobayashi, Shoichiro Watanabe, Takafumi Fujiwara, Akira Hashimoto, Yasuhiko Syoji
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Patent number: 6193947Abstract: Hydrothermal treatment of at least one manganese source material, for example, an oxide of manganese, such as Mn2O3, MnO, or MnO2, in an aqueous solution containing at least one water-soluble lithium salt, such as lithium hydroxide, lithium chloride, lithium nitrate, lithium fluoride, or lithium bromide, and an alkaline metal hydroxide, such as potassium hydroxide, at 130 to 300° C. can realize the preparation of a lithium manganese oxide (LiMnO2) having a layered rock-salt structure in a single stage.Type: GrantFiled: June 29, 1998Date of Patent: February 27, 2001Assignee: Agency of Industrial Science and TechnologyInventors: Mitsuharu Tabuchi, Kazuaki Ado, Hironori Kobayashi, Hiroyuki Kageyama
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Patent number: 6190800Abstract: A lithiated manganese dioxide for use in primary lithium electrochemical cells. The lithiated manganese dioxide is prepared by stepwise treatment with a liquid source of lithium cations that can include an aqueous solution of a lithium base or a low melting point lithium salt resulting in formation of a lithiated manganese dioxide product. Lithium cations in the lithium base or molten lithium salt can be ion-exchanged with hydrogen ions in the manganese dioxide crystal lattice and additional lithium ions reductively inserted into the lattice during subsequent heat-treatment to form the lithiated manganese dioxide product LiyMnO2−&dgr;. The primary lithium cell utilizing the lithiated manganese dioxide product as active cathode material exhibits increased operating voltage and enhanced high rate, low temperature, and pulse discharge performance compared with untreated manganese dioxide.Type: GrantFiled: February 1, 2000Date of Patent: February 20, 2001Assignee: The Gillette CompanyInventors: Nikolay Iltchev, Paul A. Christian, William L. Bowden, Peter R. Moses, Klaus Brandt
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Patent number: 6183718Abstract: A method for forming the composition stabilized against capacity degradation comprises particles of spinel lithium manganese oxide (LMO) enriched with lithium by a decomposition product of lithium carbonate forming a part of each said particle and characterized by a reduced surface area and increased capacity expressed in milliamp hours per gram as compared to non-enriched spinel.Type: GrantFiled: May 7, 1999Date of Patent: February 6, 2001Assignee: Valence Technology, Inc.Inventors: Jeremy Barker, M. Yazid Saidi, Chariclea A. Scordilis-Kelley
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Patent number: 6183717Abstract: Mixed-metal oxide-based solids composed of a linked array of a plurality of vanadium oxide building blocks wherein a vanadium and oxygen shell cluster encapsulate a central X unit, where X is at least one species selected from the group consisting of VO4, SO4, Cl, Br, I, H2O, HCOO and NO2 and associated methods of synthesis are provided.Type: GrantFiled: February 3, 1999Date of Patent: February 6, 2001Assignee: Illinois Institute of TechnologyInventor: M. Ishaque Khan
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Patent number: 6183910Abstract: Suitable as active cathode material for an electrochemical lithium secondary cell are oxygen-deficient spinels Li1+xMn2−xO4−&dgr; , where 0≦x≦0.33 and 0.01≦&dgr;≦0.5. Their region of existence in a phase diagram laid out between the corner points MnO, MnO2 and Li2MnO3 for lithium manganese oxide compounds is defined by the corner compounds LiMn2O4, Li2Mn4O7, Li8Mn10O21 and Li4/3Mn5/3O4, all the compounds along the lines LiMn2O4—Li4/3Mn5/3O4 and LiMn2O4—Li2Mn2O4 being excepted. The spinels are produced by a modified ceramic process from a mixture of Li-containing and Mn-containing starting substances whose reaction product is reduced by roasting in an Ar/H2 atmosphere. The Li components x can be replaced partially or completely by foreign monovalent or multivalent cations from the series consisting of Co, Mg, Zn, Ni, Ca, Bi, Ti, V, Rh or Cu.Type: GrantFiled: October 24, 1997Date of Patent: February 6, 2001Assignee: Varta Batterie AktiengesellschaftInventors: Hans-Walter Praas, Sibylle Kemmler-Sack, Peter Endres
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Patent number: 6180764Abstract: A process for producing high-purity hydrotalcites by reacting alcohols or alcohol mixtures with at least one or more divalent metal(s) and at least one or more trivalent metal(s) and hydrolysing the resultant alcoholate mixture with water. The corresponding metal oxides can be produced by calcination.Type: GrantFiled: April 30, 1999Date of Patent: January 30, 2001Assignee: RWE-DEA Aktiengesellschaft fur Mineraloel und ChemieInventors: Klaus Noweck, Klaus Diblitz, Jan Sohiefler, Andrea Brasch
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Patent number: 6174835Abstract: An exhaust gas purifying catalyst for use in an oxygen surplus atmosphere, includes a brown millerite composite oxide for directly decomposing and absorbing nitrogen oxide (NOx), and a noble metal-series reducing catalyst disposed on the surface of said brown millerite composite oxide. The brown millerite composite oxide is represented by one of the following formulae: A3-aBaC4-bDbO9, A2-aBaC2-bDbO5, and A1-aBaC2-bDbO4 where A and B are elements selected from the group consisting of Ba, Ca, Sr, Mg and Ce, C and D are elements selected from the group consisting of Y, Dy, Zn, Ti, Mn, Fe, Co, Ni, Cu, Sn, Zr and Nd, a is within the range 0≦a<1, and b is within the range 0≦b<2.Type: GrantFiled: June 10, 1999Date of Patent: January 16, 2001Assignee: Isuzu Ceramics Research Institute Co., Ltd.Inventors: Isao Naito, Kazuo Oosumi, Yasuaki Unno
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Patent number: 6168888Abstract: A high-performance spinel-type lithium-manganese oxide for use as a material for a positive electrode of a Li secondary battery with inhibited Mn dissolution in an organic electrolyte, which is represented by the following formula: {Li}[Lix.My.Mn(2−x−y)]O4+d wherein { } represents the oxygen tetrahedral sites in the spinel structure and [ ] represents the oxygen octahedral sites in the spinel structure, 0<x≦0.33, 0<y≦1.0, −0.5<d<0.8, and M represents at least one heteroelement other than Li and Mn, is disclosed.Type: GrantFiled: June 18, 1998Date of Patent: January 2, 2001Assignee: Tosoh CorporationInventors: Eiichi Iwata, Ken-ichi Takahashi, Takashi M{overscore (o)}ri
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Patent number: 6156456Abstract: A positive electrode active material, includes a .beta.-Ni(OH).sub.2 type nickel oxide (including hydroxide) containing Mn in the state of solid solution or coprecipitated state with an average valence of Mn being 3.3 valences or more and preferably with a ratio A2/A1 being 1.25 or less which is a ratio of integrated intensity A2 of a peak present at 2.theta.=18-21.degree. to integrated intensity A1 of a peak present at 2.theta.=37-40.degree. of powder X-ray diffraction using CuK.alpha. ray.Type: GrantFiled: August 6, 1998Date of Patent: December 5, 2000Assignee: Matsushita Electric Industrial Co., Ltd.Inventors: Yoichi Izumi, Hiroyuki Sakamoto, Hidekatsu Izumi, Isao Matsumoto
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Patent number: 6153334Abstract: The energy density of active materials for a positive electrode comprising an oxide containing Ni as a main metallic element is enhanced, and, moreover, a method for manufacturing them is provided. The oxide includes Ni as a main metallic element and contains at least Mn in the state of solid solution or eutectic mixture, wherein the average valence of Mn is 3.3 valences or more, the tap density is 1.7 g/cc or more, the half width of a peak at around 2.theta.=37-40.degree. of X-ray diffraction using CuK.alpha. ray is 1.2 deg or less, the ratio B/A of integrated intensity B of a peak at around 2.theta.=18-21.degree. to integrated intensity A of a peak at around 2.theta.=37-40.degree. is 1.25 or less, and the volume of pores having a pore radius of 40 .ANG. or less is 60% or more of the total pore volume. The oxide is obtained by growing in the state of keeping the dissolved oxygen concentration in the aqueous solution in the reaction vessel and then oxidizing the oxide.Type: GrantFiled: August 6, 1998Date of Patent: November 28, 2000Assignee: Matsushita Electric Industrial Co., Ltd.Inventors: Hiroyuki Sakamoto, Hidekatsu Izumi, Yoichi Izumi, Isao Matsumoto
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Patent number: 6136287Abstract: Lithium manganese oxide particles have been produced with an average diameter less than about 250 nm. The particles have a high degree of uniformity. The particles are formed by the heat treatment of nanoparticles of manganese oxide. The lithium manganese oxide particles are useful as active materials in the positive electrodes of lithium based batteries. Improved batteries result from the use of the uniform nanoscale lithium manganese oxide particles.Type: GrantFiled: December 2, 1998Date of Patent: October 24, 2000Assignee: NanoGram CorporationInventors: Craig R. Horne, Sujeet Kumar, Hariklia Dris Reitz, James T. Gardner, Xiangxin Bi
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Patent number: 6129902Abstract: A process for producing positive electrode active material includes feeding an aqueous nickel salt solution, aqueous solutions of different kinds of metals, aqueous solution containing ammonium ions and aqueous alkali solution each independently and simultaneously into a reaction vessel such that the amount of alkali metal is 1.9-2.3 moles relative to 1 mole of the total amount of nickel and different kinds of metals and the amount of ammonium ions is 2 moles or more relative to 1 mole of the total amount of nickel and different kinds of metals, the pH in the vessel is 11-13, the temperature in the vessel is 30-60.degree. C. and the average residence time is 20-50 hours.Type: GrantFiled: February 2, 1998Date of Patent: October 10, 2000Assignee: Matsushita Electric Industrial Co., Ltd.Inventors: Hiroyuki Sakamoto, Hidekatsu Izumi, Hirokazu Kimiya, Yoichi Izumi, Isao Matsumoto
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Patent number: 6123911Abstract: A process for producing a lithium manganate for lithium secondary batteries comprising mixing a manganese compound and a lithium compound, firing the mixture at 1000 to 1500.degree. C., mixing the resulting complex oxide with a lithium compound, and firing the mixture at 600 to 800.degree. C.Type: GrantFiled: September 10, 1998Date of Patent: September 26, 2000Assignee: Mitsui Mining & Smelting Company, Ltd.Inventors: Munetoshi Yamaguchi, Koichi Numata
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Patent number: 6117410Abstract: A process for producing lithiated manganese oxide having a layered rock-salt structure, which comprises burning lithium and manganese materials or pretreated materials thereof at a temperature needed to synthesize LiMnO.sub.2, and then quenching the burnt materials.Type: GrantFiled: May 29, 1998Date of Patent: September 12, 2000Assignee: Showa Denko Kabushiki KaishaInventors: Takashi Ogihara, Hiroyuki Takahashi, Masahiro Ohmori, Katsutoshi Tamura
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Patent number: 6114064Abstract: A novel method of preparing a spinel Li.sub.1+x Mn.sub.2-x O.sub.4 intercalation compound with low lattice distortion and a highly ordered and homogeneous structure for 4 V secondary lithium and lithium ion cells is provided. The method of preparing the spinel Li.sub.1+x Mn.sub.2-x O.sub.4 intercalation compound comprises mixing at least one manganese compound with at least one lithium compound and firing the mixture at three different temperature ranges with corresponding gas flow rates to form the spinel Li.sub.1+x Mn.sub.2-x O.sub.4 intercalation compounds. The spinel Li.sub.1+x Mn.sub.2-x O.sub.4 intercalation compounds have a mean X value of between about 0.01 and 0.05 and a full width at half maximum of the x-ray diffraction peaks at a diffraction angle 2.theta. of planes (400) and (440) using CuK.alpha..sub.1 rays of between about 0.10.degree. and 0.15.degree.. The spinel Li.sub.1+x Mn.sub.2-x O.sub.Type: GrantFiled: June 2, 1997Date of Patent: September 5, 2000Assignee: FMC CorporationInventors: Vesselin Manev, Titus Faulkner
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Patent number: 6110441Abstract: A method of producing a homogeneous metal oxide fiber having high denseness and free of voids that may adversely affect the electro-optic characteristic of the fiber, and a metal oxide fiber produced according to the method. The method comprises:a first step of forming a gel-form fiber from a sol obtained by concentrating a solution composed of a metallic compound, water and a solvent to the extent that the solution exhibits a spinnable behavior;a second step of decomposing and eliminating organic components out of the gel-form fiber obtained at the first step; anda third step of solidifying the gel-form fiber obtained at the second step;the second step and/or the third step being carried out while heating is made in a water vapor atmosphere.Type: GrantFiled: May 12, 1998Date of Patent: August 29, 2000Assignee: Minolta Co., Ltd.Inventor: Kenji Kitaoka
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Patent number: 6110442Abstract: A method of preparing Li.sub.x Mn.sub.2 O.sub.4 for a secondary battery includes mixing lithium nitrate, magnanese nitrate and citric acid. A complex citrate solution is formed in the substantial absence of a polyhydroxyl alcohol. The complex citrate solution is dehydrated to produce a precursor. The precursor is then heated at a substantially constant rate and then calcined to provide a spinel compound.Type: GrantFiled: May 30, 1997Date of Patent: August 29, 2000Assignee: Hughes Electronics CorporationInventors: Dinggue Xia, Qingguo Liu
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Patent number: 6103422Abstract: The powdery cathode active material of the present invention for use in a nonaqueous electrolyte secondary battery comprises as the active ingredient a lithium manganese composite oxide and at least one nonmanganese metal element selected from the group consisting of aluminum, magnesium, vanadium, chromium, iron, cobalt, nickel, and zinc, provided that the nonmanganese metal element exists in the surface portions of fine particles constituting the powdery cathode active material.A nonaqueous electrolyte secondary battery comprising such a cathode active material, an anode active material and a nonaqueous electrolytic solution containing a lithium salt has a large charge-and-discharge capacity and a stable charge-and-discharge cycle durability, and can be prepared inexpensively.Type: GrantFiled: June 24, 1998Date of Patent: August 15, 2000Assignee: Kao CorporationInventor: Hiroyuki Kanai
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Patent number: 6087042Abstract: Disclosed is a positive electrode material for a secondary lithium battery excellent in high temperature cycle characteristics which is a lithium manganese oxyfluoride having a spinel structure, wherein the oxyfluoride has a composition represented by the composition formula:Li.sub.1+x Mn.sub.2-x O.sub.4-y F.sub.zwherein x represents a number of from 0.0133 to 0.3333; y represents a number of from 0 to 0.2 (exclusive of 0); and z represents a number of from 0.01 to 0.2 (exclusive of 0.01), with the proviso that (y-z) is more than 0 but not more than 0.07. The positive electrode material for a secondary lithium battery of the present invention exhibits not only a high cycle durability of charge/discharge but also a minimum drop of a charge/discharge initial capacity to provide a high energy density.Type: GrantFiled: February 23, 1999Date of Patent: July 11, 2000Assignee: Kabushiki Kaisha Toyota Chuo KenkyushoInventors: Jun Sugiyama, Tsuyoshi Sasaki, Tatsuya Hatanaka, Tatsuo Noritake, Tatsumi Hioki
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Patent number: 6083474Abstract: There are disclosed lithium-iron oxide particles having an excellent properties such as electrochemical reversibility and suitable as a material for cathode active material for lithium ion batteries, which have a corrugated layer crystal structure and are represented by the general formula (1):Li.sub.x (Fe.sub.(1-y) M.sub.y)O.sub.2 (1)wherein x is more than 0 and not more than 1; y is 0.005 to 0.1; and M is at least one metal selected from the group consisting of Co, Ni, Mn and Al.Type: GrantFiled: August 22, 1997Date of Patent: July 4, 2000Assignee: Toda Kogyo CorporationInventors: Tatsuya Nakamura, Ryoji Kanno, Mikio Takano
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Patent number: 6083643Abstract: A process for preparing an active material for a cathode of a lithium ion battery comprising the steps of: dissolving lithium hydroxide, manganese acetate as starting materials into water to form a solution; adding a chelating agent into the solution; producing gel or liquid phase by evaporating the solution; and producing a powder by raising temperature at the rate of 5.about.20 .degree. C./min, combusting and calcinating the gel or liquid phase at 300.about.400 .degree. C. during 2.about.3 hours is disclosed.Type: GrantFiled: November 24, 1997Date of Patent: July 4, 2000Assignee: Samsung Display Devices Co., Inc.Inventors: Jae-phil Cho, Geun-bae Kim
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Patent number: 6083475Abstract: The present invention is a simple and reliable method for producing lithiated metal oxides such as those useful as cathode materials in lithium ion electrochemical cells. The method is based on the use of an organic solvent that dissolves both lithium sulfide and elemental sulfur without dissolving the metal oxide or the lithiated product. Lithium sulfide and the metal oxide as a powder are refluxed in the organic solvent under an inert atmosphere. The organic solvent dissolves the lithium sulfide and the dissolved sulfide reduces the metal oxide allowing the intercalation of lithium. At the same time the sulfur that results from the oxidation-reduction reaction is carried away by the solvent thereby promoting the reaction and preventing contamination of the product with sulfur.Type: GrantFiled: April 2, 1999Date of Patent: July 4, 2000Assignee: Rentech, Inc.Inventors: Dale R. Shackle, Benjamin Chaloner-Gill
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Patent number: 6080510Abstract: Ternary lithium mixed oxides having a spinel-type crystal structure and the general formula (I) Li.sub.y Me.sub.x Mn.sub.2-x O.sub.4 are disclosed. In this formula (I), Me represents a metal cation from groups IIa, IIIa, Iva, IIb, IIIb, IVb, IVb, VIIb, and VIII of the Periodic Table of Elements, x is in a range between 0 and 1, and y is in a range of greater than zero and not more than 1.2. The ternary mixed lithium oxide is obtainable by reacting reaction components in the form of hydroxides and/or water-soluble metal salts dissolved in a basic aqueous medium to form a homogenous suspension of the hydroxylic reaction products, removing water and optionally further solvents from the suspension, and subjecting the dried reaction products to heat treatment by heating them to temperatures between 500.degree. C. and 900.degree. C. at a heating speed of between 1 K/min and 20 K/min. The respective mixed oxides obtained are in a form which has no phase having a radiographic effect.Type: GrantFiled: June 30, 1997Date of Patent: June 27, 2000Assignee: Zentrum fur Sonnenenergie-und Wasserstoff Forshung Baden Wurttemberg Gemeinnultzige StiftungInventors: Reinhard P. Hemmer, Rudiger Oesten, Margret Wohlfahrt-Mehrens, Gisela Arnold
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Patent number: 6077626Abstract: In an alkali storage battery comprising a positive electrode, a negative electrode and an alkali electrolyte in a battery can, .alpha.-nickel hydroxide containing manganese is used as a cathode active material for the positive electrode, and the difference between a charging potential and an oxygen gas evolution potential at the positive electrode is increased, to suppress oxygen gas evolution during the charging, and the volume percentage of the cathode active material and an anode active material is set to not less than 75% in the battery can, to obtain a large battery capacity.Type: GrantFiled: April 22, 1999Date of Patent: June 20, 2000Assignee: Sanyo Electric Co., Ltd.Inventors: Mitsuzou Nogami, Mutsumi Yano, Mitsunori Tokuda, Syuichi Suzuki, Shin Fujitani, Reizo Maeda, Ikuo Yonezu, Koji Nishio
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Patent number: 6076965Abstract: A nickel-cobalt-manganese oxide monocrystal having a cubic spinel structure over a broad concentration range of manganese/cobalt/nickel, including the entire possible range of manganese to nickel ratios, provided that the resulting monocrystal has a cubic spinel structure. A flux method is described for producing the monocrystals. Also disclosed are sensors, based on the monocrystals, having desirable electrical properties In particular, the sensors of the present invention are highly accurate temperature sensors or thermistors having high sensitivity, good reproducibility and improved aging characteristics. Performance of a sensor based on the monocrystal permits the preparation of a thermistor standard which can be used to evaluate the performance of ceramic devices.Type: GrantFiled: June 17, 1997Date of Patent: June 20, 2000Assignee: Therometrics, Inc.Inventors: Carol Zwick Rosen, Donald G. Wickham
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Patent number: 6077496Abstract: The mixed powders of a lithium compound and a transition metal based compound are formed into shaped parts, which are packed to form a bed 6 on a porous plate 5 in the bottom of a reaction vessel 7 placed on a support 10 in a firing furnace 8 equipped with an electric heater; the packed parts are fired with an oxidizing gas such as air being forced through the bed 6 at a superficial velocity higher than a specified value via a gas feed pipe 3 connecting an air pump 1, a flow regulator 2 and a preheater 4 and the gas emerging from the bed 6 is discharged into the air atmosphere through a ventilation port 9. Even if increased amounts of the mixed powders have to be fired, the invention process enables the production of a lithium complex oxide as an active material that is homogeneous and which features excellent cell characteristics.Type: GrantFiled: September 8, 1997Date of Patent: June 20, 2000Assignee: Dowa Mining Co., Ltd.Inventors: Yuichi Ito, Yukio Hiraoka, Akinobu Iikawa, Masaru Nishisako, Choju Nagata, Kenichi Harigae
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Patent number: 6071489Abstract: The Li.sub.x Mn.sub.2 O.sub.4 powder for cathode active material of a lithium secondary battery of the present invention is prepared by a method of comprising the steps of mixing an acetate aqueous solution using Li acetate and Mn acetate as metal precursors, and a chelating agent aqueous solution using PVB, GA, PAA or GC as a chelating agent; heating the mixed solution at 70.about.90.degree. C. to form a sol; further heating the sol at 70.about.90.degree. C. to form a gel precursor; calcining the produced gel precursor at 200 .about.900.degree. C. for 5.about.30 hours under atmosphere. The cathode active material, Li.sub.x Mn.sub.2 O.sub.4 powder for a lithium secondary battery in accordance with the present invention has a uniform particle size distribution, a high crystallinity and a pure spinel-phase, and a particle size, a specific surface area, a lattice of a cubic structure and the like can be controlled upon the preparing conditions. The present invention also provides a method of preparing LiNi.sub.Type: GrantFiled: December 2, 1997Date of Patent: June 6, 2000Assignee: Samsung Display Device Co., Ltd.Inventors: Yang-Kook Sun, Young-Roak Kim, Kyu-Sung Kim, Dong-Won Kim
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Patent number: 6071647Abstract: The invention relates to a method of preparing an oxide of formula Li.sub.x Mn.sub.y O.sub.z, in which x lies in the range 0 to 2, y lies in the range 1 to 3, and z lies in the range 3 to 4.5, x, y, and z being such that the oxide has a composition close to LiMn.sub.2 O.sub.4. According to the invention, the method comprises the following steps:a) a polymer complex of lithium and of manganese is prepared in the form of a gel or of a xerogel by causing a reducing polymer, copolymer or polymer mixture possessing complexing functions for lithium and manganese to react in a common solvent with an oxidizing lithium salt and with an oxidizing manganese salt, and by evaporating off the solvent, partially or in full; andb) the resulting lithium and manganese polymer complex is mineralized by the explosive oxidation-reduction technique to recover fine amorphous particles of the oxide of formula Li.sub.x Mn.sub.y O.sub.z.Type: GrantFiled: October 17, 1997Date of Patent: June 6, 2000Assignee: France TelecomInventors: Nadine Treuil, Josik Portier, Guy Campet, Josette Ledran, Jean-Claude Frison
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Patent number: 6051339Abstract: A cathode for use in an electrochemical cell comprising a lithiated isopolyvanadate or heteropolyvanadate wherein the isopolyvanadate or heteropolyvanate has a cage structure, and an electrochemical battery comprising an alkali metal anode, an ionically conductive electrolyte and a cathode which comprises a lithiated isopolyvanadate or heteropolyvanadate having a cage structure, are described.Type: GrantFiled: May 26, 1998Date of Patent: April 18, 2000Assignee: Rentech, Inc.Inventors: Dale R. Shackle, Benjamin Chaloner-Gill
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Patent number: 6027246Abstract: Monocrystalline nickel-cobalt-manganese-copper oxide having a cubic spinel structure over a broad range of concentration ratios of manganese/cobalt/nickel/copper, including methods of producing such monocrystals, particularly those having a quaternary cubic spinel structure. Sensors having desirable electrical properties are disclosed, which sensors comprise at least a portion of such monocrystals. In particular, such sensors are highly accurate temperature sensors or thermistors having high sensitivity, good reproducibility and improved aging characteristics.Type: GrantFiled: December 16, 1997Date of Patent: February 22, 2000Assignee: Thermometrics, Inc.Inventors: Carol Zwick Rosen, Donald G. Wickham
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Patent number: 6024934Abstract: Lithium compound and nickel oxyhydroxide containing a transition metal (Me) such as V, Cr, Mn, Fe, Zn and Co are suspended in water or in an organic solvent, and the solution is reacted with each other in an autoclave by a hydrothermal method to thereby synthesize transition metal-containing lithium nickelate.Type: GrantFiled: September 24, 1997Date of Patent: February 15, 2000Assignee: Japan Storage Battery Co., Ltd.Inventors: Khalil Amine, Hideo Yasuda, Yuko Fujita
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Patent number: 6017504Abstract: Perovskite-type structure compounds having the general empirical formula ABO.sub.3 are prepared by a process comprising subjecting a mixture of starting powders formulated to contain the components represented by A and B in the formula to a high energy milling sufficient to induce chemical reaction of the components and thereby synthesize a mechanically-alloyed powder comprising the perovskite in the form of nanostructural particles. The process according to the present invention is simple, efficient, not expensive and does not require any heating step for producing a perovskite that may easily show a very high specific surface area. Another advantage is that the perovskite obtained according to the present invention also has a high density of lattice defects thereby showing a higher catalytic activity, a characteristic which is highly desirable in their eventual application as catalysts and electronic conductors.Type: GrantFiled: July 16, 1998Date of Patent: January 25, 2000Assignee: Universite LavalInventors: Serge Kaliaguine, Andre Van Neste
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Patent number: 6004696Abstract: An air electrode for a solid oxide fuel cell having high conductivity and low interfacial resistance is disclosed. Said air electrode is composed of an Ag-perovskite cermet.Type: GrantFiled: March 22, 1995Date of Patent: December 21, 1999Assignee: Northwestern UniversityInventors: Scott Alexander Barnett, Li-Shun Wang
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Patent number: 6004469Abstract: A process for the decomposition of hydrogen peroxide wherein aqueous streams containing 1 to 500,000 ppm H.sub.2 O.sub.2 are contacted with a Mn/Cu catalyst component on a monolith carrier to eliminate the H.sub.2 O.sub.2 by decomposition to water and oxygen.Type: GrantFiled: January 28, 1998Date of Patent: December 21, 1999Assignee: Advanced Catalyst Systems, Inc.Inventors: Michele W. Sanders, Larry E. Campbell
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Patent number: 6004697Abstract: A method of improving certain vanadium oxide formulations is presented. The method concerns fluorine doping formulations having a nominal formula of LiV.sub.3 O.sub.8. Preferred average formulations are provided wherein the average oxidation state of the vanadium is at least 4.6. Herein preferred fluorine doped vanadium oxide materials, electrodes using such materials, and batteries including at least one electrode therein comprising such materials are provided.Type: GrantFiled: December 5, 1997Date of Patent: December 21, 1999Assignees: Minnesota Mining & Manufacturing Co., Hydro-Quebec CorporationInventors: Michael M. Thackeray, Arthur J. Kahaian, Donald R. Visser, Dennis W. Dees, Roy Benedek
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Patent number: 5997839Abstract: The invention is directed to making a lithiated manganese dioxide using low and high temperature calcination steps.Type: GrantFiled: June 2, 1998Date of Patent: December 7, 1999Assignee: Carus Chemical CompanyInventor: G. Chithambarathanu Pillai
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Patent number: 5993998Abstract: A positive active material for lithium battery, includes a lithium-containing amorphous nickel oxide represented by a chemical composition formula of Li.sub.x NiO.sub.2 ; wherein x is from greater than 0.25 to 2. Preferably, x is from greater than 1 to 2. More preferably, x is from greater than 1.4 to 2. The positive active material may contains cobalt from 2 to 60 mol % {(Co/(Ni+Co)}.Type: GrantFiled: December 19, 1997Date of Patent: November 30, 1999Assignee: Japan Storage Battery Co., Ltd.Inventor: Hideo Yasuda
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Patent number: 5985237Abstract: A process for producing a lithium manganese oxide which has a formula of Li.sub.x MnO.sub.2 in which x is between 0.1 and 1 and which is suitable for use as a 3 volt cathode material, which comprises mixing at least one lithium compound with at least one manganese compound at a Li/Mn atomic ratio of 0.1-1 in a solvent selected from an aliphatic lower alcohol having from 1 to 3 carbon atoms, water and a mixture of the alcohol and water, allowing the resultant mixture to form a gel-like mixture, drying the gel-like mixture as required, and calcining the resulting product in an oxidative atmosphere at a temperature of 200-350.degree. C.Type: GrantFiled: October 28, 1997Date of Patent: November 16, 1999Assignee: Honjo Chemical CorporationInventors: Qi Lu, Gohei Yoshida, Kazuhiko Hirao, Yukinori Honjo
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Patent number: 5981106Abstract: An inexpensive positive electrode active material for lithium batteries which comprises lithium manganate having a hexagonal layered structure with space group of R3m and exhibits continuous discharge voltage characteristics between 4.5 V and 2 V for metallic lithium.Type: GrantFiled: June 13, 1997Date of Patent: November 9, 1999Assignee: Japan Storage Battery Co., Ltd.Inventors: Khalil Amine, Hideo Yasuda, Yuko Fujita
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Patent number: 5976489Abstract: A method of making a lithium manganese oxide intercalation compound in powder form comprises forming a solution of a manganese compound and a lithium compound in a solvent; and spray-drying the solution by atomizing the solution to form droplets thereof and contacting the droplets with a stream of non-oxidizing hot gas at a first elevated temperature to evaporate at least a major portion by weight of the solvent present in the solution thereby providing a precursor powder. The precursor powder is heated at a second elevated temperature which is below the melting point of the lithium manganese oxide compound. The second temperature is sufficient to cause reaction among constituents in the precursor powder thereby providing the lithium manganese oxide compound having a spinel unit structure.Type: GrantFiled: February 27, 1997Date of Patent: November 2, 1999Assignee: Valence Technology, Inc.Inventors: M. Yazid Saidi, Eileen Saidi, Arnold Stux
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Patent number: 5976488Abstract: Apparatus and a process are provided for converting and/or removing harmful constituents from solid hazardous or other undesirable waste material by heating the waste in a reactor in the presence of a continuous flow of oxygen and waste metals, wherein the waste material becomes a molten metal oxide bath which when solidified, has a spinel structure to chemically bond harmful constituents within the spinel structure by crystal chemical substitution. The resulting metal oxides are environmentally acceptable. A substantially gaseous effluent which may contain particulate material is also generated. The effluent is conducted through a high temperature zone to destroy organic and other harmful constituents influenced by temperature and dwell time. The effluent is further processed through an emissions treatment system to achieve acceptable environmental quality.Type: GrantFiled: August 14, 1996Date of Patent: November 2, 1999Assignee: Phoenix Environmental, Ltd.Inventors: Jason Workman, Peter DellaValle
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Patent number: 5961950Abstract: Lithiated manganese oxides are synthesized using a novel two stage process. Using appropriate starting materials, lithiation is accomplished via low temperature ion exchange in aqueous warm salt solution. A drying stage follows which completes the synthesis. Materials suitable for use as cathodes in lithium ion rechargeable batteries have been prepared in this way. Other solid solution transition metal materials might also be prepared using a similar low temperature ion exchange process.Type: GrantFiled: December 29, 1997Date of Patent: October 5, 1999Assignee: NEC Moli Energy (Canada) LimitedInventors: Jeffery Raymond Dahn, Erik Rossen, Jan N. Reimers, Eric Wayne Fuller
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Patent number: 5961949Abstract: A novel method of preparing a highly homogenous spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y intercalation compound having a predetermined mean particle size and particle size distribution for 4 V secondary lithium and lithium ion cells is provided. The method comprises mixing at least one manganese compound having a predetermined particle size distribution with at least one lithium compound wherein the manganese compound has a mean particle size of between about 1 and 15 microns and the mean particle size of the lithium compound is less than that of the manganese compound. The mixture is then fired in one or more firing steps within specific temperature ranges to form the Li.sub.1+X Mn.sub.2-X O.sub.4+Y intercalation compound. Preferably, at least one firing step is at a temperature of between about 700.degree. C. and 900.degree. C. The Li.sub.1+X Mn.sub.2-X O.sub.Type: GrantFiled: June 6, 1997Date of Patent: October 5, 1999Assignee: FMC CorporationInventors: Vesselin Manev, Walter Ebner, William Thompson, Stephen Dow
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Patent number: 5962166Abstract: A series of electroactive insertion compounds, LiM.sub.y.sup.II M.sub.z.sup.III Mn.sub.l.sup.III Mn.sub.q.sup.IV O.sub.4 (0<y+z.ltoreq.0.5, y+z+l+q=2), where M=any transition metal or combination of metals, for application in non-aqueous batteries, capacitors, and superconducting materials, are disclosed. These newly synthesized compounds are unique in that they contain at least two mixed valence elements, thereby allowing the reversible intercalation of lithium cations at potentials near 4.7-5.1 V vs. lithium. Also disclosed are novel copper insertion compounds of the formula LiM.sub.y Cu.sub.0.5-y Mn.sub.1.5 O.sub.4 (0.ltoreq.y.ltoreq.0.49), where M=one or more metals or transition metals. Such materials have also been found to be remarkably stable at this voltage upon repeated cycling.Type: GrantFiled: May 8, 1998Date of Patent: October 5, 1999Assignee: Covalent Associates, Inc.Inventors: Yair Ein-Eli, Wilmont F. Howard, Jr.
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Patent number: 5958362Abstract: The present method is to produce an active material powder formed of a spinel oxide containing lithium or a layer-structured oxide containing lithium for a lithium secondary battery which is uniform in composition, fine in particle size and free of oxygen defects, and which is unlikely to cause capacity deterioration resulted from repetitive charge/discharge cycles at a high current density.A suspension 1 prepared by suspending an ingredient of the active material powder in a combustible liquid or an emulsion prepared by emulsifying a solution of the ingredient in the combustible liquid is sprayed in a droplet state 15 together with an oxygenic gas 2. The combustible liquid contained in the droplet 15 is burned to have the ingredient therein reacted and to evaporate the solvent. As a result, active material powder 4 formed of the spinel oxide containing lithium is obtained.Type: GrantFiled: March 27, 1997Date of Patent: September 28, 1999Assignee: Kabushiki Kaisha Toyota Chuo KenkyushoInventors: Kazumasa Takatori, Naoyoshi Watanabe, Toshihiko Tani, Tsuyoshi Sasaki, Akio Takahashi, Masahiko Kato, Akihiko Murakami
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Patent number: 5955052Abstract: The invention is a process which provides a high purity lithiated manganese oxide (Li.sub.1+x Mn.sub.2-y O.sub.4) from chemically made MnO.sub.2. The lithiated manganese oxide has an especially effective utility for use as a cathodic material in rechargeable batteries. The process of the invention includes blending a lithium compound with a chemically made manganese dioxide to form a manganese dioxide/lithium compound blend. The lithium compound in the blend is at least about one mole of lithium for every mole of manganese dioxide. The manganese dioxide and lithium compound in the blend are reacted to provide an ion replaced product where lithium ions have replaced sodium and potassium ions in the MnO.sub.2 to form an ion replaced product. Thereafter, the ion replaced product is heated or calcined to provide the lithiated manganese oxide.Type: GrantFiled: May 21, 1998Date of Patent: September 21, 1999Assignee: Carus CorporationInventors: Akshaya Kumar Padhi, G. Chithambarathanu Pillai
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Patent number: 5951919Abstract: Provided is a method of preparing a cathode material for lithium ion cell, which is designed to have the cycle characteristic enhanced and high initial discharge capacity, by synthesizing LiMn.sub.2 O.sub.4 powder having a stable spinel structure, vigorously agitating the powder in an aqueous solution of Li and Ni ions, dispersing the solution through a supersonic wave treatment, filtering it so as for the powder to adsorb the ions, and performing a heat treatment for doping the ions.Type: GrantFiled: April 8, 1998Date of Patent: September 14, 1999Assignee: Korea Kumho Petro Chemical Co., Ltd.Inventors: Kang-Seon Hwang, Dong-Hwan Kim, Sung-Ruyl Kwon