Manganese (e.g., Manganate, Etc.) Patents (Class 423/599)
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Patent number: 5939043Abstract: A method of forming lithium manganese oxide spinel, comprising the steps of combining predetermined amounts of lithium carbonate powder and manganese dioxide powder, the powders having predetermined surface areas; mixing the lithium carbonate and manganese dioxide for about 0.5 hours to about 2.0 hours in a manner so as to thoroughly mix the powders, but not to significantly increase the surface area of the powders; increasing the temperature of the mixture from approximately room temperature to a calcining temperature between about 700.degree. C. to about 900.degree. C.; maintaining the calcining temperature of the mixture between about 700.degree. C. to about 900.degree. C. for about 7 hours to about 13 hours; reducing the temperature of the mixture from the calcining temperature to about 500.degree. C. at a cooling rate between about 10.degree. C./hour to about 120.degree. C./hour; and cooling the mixture from 500.degree. C. to room temperature.Type: GrantFiled: June 26, 1998Date of Patent: August 17, 1999Assignee: GA-TEK Inc.Inventor: Masataka Yahagi
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Patent number: 5932374Abstract: The cycling stability and capacity of Li-ion rechargeable batteries are improved, particularly in an elevated temperature range of about 55.degree. C., by the use of lithium magnesium manganese oxy-fluoride electrode components having the general formula, Li.sub.1+x Mg.sub.y Mn.sub.2-x-y O.sub.4-z F.sub.z, where x.ltoreq.0.2, 0.1.ltoreq.y.ltoreq.0.3, and 0.01.ltoreq.z.ltoreq.0.5.Type: GrantFiled: December 4, 1997Date of Patent: August 3, 1999Assignee: Telcordia Technologies, Inc.Inventor: Glenn G. Amatucci
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Patent number: 5928622Abstract: Technologies regarding camcorder, cellular phone and note book PC etc. have been developing rapidly according to the development of electronics, communication and computer industries. The secondary battery which can be used continuously by recharging has been required for the electric power of such instruments. Therefore, present invention relates to a high-capacity LiMn.sub.2 O.sub.4 compound used for non-aqueous electrolyte lithium ion battery, more particularly, to a method for preparing LiMn.sub.2 O.sub.4 intercalation compound doped with Li and Co ion, which comprises the following steps of : synthesis of spinel type LiMn.sub.2 O.sub.4 powder; dissolving and treating LiMn.sub.2 O.sub.4 powder in the solution to adsorb Li and Co ion; and thermal treatment of said LiMn.sub.2 O.sub.4 to obtain LiMn.sub.2 O.sub.4 doped with Li and Co ion.Type: GrantFiled: May 30, 1997Date of Patent: July 27, 1999Assignee: Korea Kumho Petrochemical Co., Ltd.Inventors: Kang Seon Hwang, Seung Eui Kim, Dong Hwan Kim
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Patent number: 5911920Abstract: It is an object of the present invention to provide a manufacturing method for Li composite oxides employed as electrode materials for Li ion batteries which is capable of obtaining Li composite oxides having a stable composition using heat treatment at comparatively low temperatures.An Li source compound and an M source compound (where M is one or more elements selected from a group containing Mn, Ni, Co, Fe, V, Ti, Sc, Y, and Al) having an element M in a composite with Li are mixed at predetermined proportions. A chemical reaction is caused by pulverizing and mixing this raw material mixture in an inert gas atmosphere. The pulverization, mixing, and reaction are continued until the raw material can no longer be detected. After pulverization and mixing, the raw material mixture is subjected to heat treatment by heating it to a temperature within a predetermined range.Type: GrantFiled: March 17, 1998Date of Patent: June 15, 1999Assignee: Mitsubishi Heavy Industries, Ltd.Inventors: Kazuhiro Hasezaki, Hikaru Motomura, Masatomo Kamada
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Patent number: 5904911Abstract: There are herein disclosed a raw material for a complex perovskite ceramic composition which is intended to uniformly disperse a trace amount of an addition component (manganese) therein, and a process for preparing the ceramic composition.A manganese-containing composite oxide is represented by the general formula (Mn.sub.a MeI.sub.1-a)MeII.sub.b O.sub.c wherein a is a value in the range of 0<a.ltoreq.0.3; MeI is at least one of Mg, Ni and Zn; MeII is one of Nb, Ta and W; when MeII is Nb or Ta, b is 2 and c is 6, or when MeII is W, b is 1 and c is 4. By the use of a raw material containing this manganese-containing complex oxide, there can be prepared an Mn-containing complex perovskite compound composition which contains Mn and at least one of complex perovskite compounds represented by the general formula Pb(BIBII)O.sub.3 wherein BI is one of Mg, Ni and Zn; and BII is one of Nb, Ta and W.Type: GrantFiled: February 27, 1998Date of Patent: May 18, 1999Assignee: NEC CorporationInventors: Toru Mori, Atsushi Ochi, Shinji Ito, Hiroshi Ishikawa, Tadahiko Horiguchi
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Patent number: 5891945Abstract: A production method of a magnesium hydroxide solid solution, Mg.sub.1-x M.sup.2+ .sub.x (OH).sub.2 or a resin and/or rubber material having as its effective elements containing said solid solution as its flame retardant, characterized by having M.sup.2+ distributed unevenly in a high concentration in the vicinity of the surface of each crystal, in the magnesium solid represented by the formula Mg.sub.1-x M.sup.2+ .sub.x (OH).sub.2 wherein M.sup.2+ is at least one divalent metal ion selected from the group consisting of Mn.sup.2+, Fe.sup.2+, Ni.sup.2+, Cu.sup.2+, Zn.sup.2+ and x indicates a range of 0.001.ltoreq.x<0.5.Type: GrantFiled: March 26, 1997Date of Patent: April 6, 1999Assignee: Tateho Chemical Industries, Co., Ltd.Inventors: Shigeo Miyata, Mitsuru Koresawa, Yasunori Kitano, Hirofumi Kurisu, Toshikazu Kotani, Kiminari Tottotsu
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Patent number: 5879654Abstract: The invention relates to a process for preparing lithium intercalation compounds by thermal solid state reaction of mixtures of lithium hydroxide or lithium oxide and oxides or oxide precursors of transition metals. A significant step of this process is the treatment of an aqueous suspension of the raw material components lithium hydroxide or lithium oxide and metal oxide or metal oxide precursors with hydrogen peroxide, resulting in the lithium compound going into solution. In the drying of the mixture, the lithium hydroxide is very uniformly absorbed onto the metal oxide. Calcination at temperatures between 450.degree. C. and 700.degree. C. results in complete reaction to form the lithium intercalation compound in less than 5 hours.Type: GrantFiled: March 27, 1996Date of Patent: March 9, 1999Assignee: Merck Patent Gesellschaft mit Beschrankter HaftungInventors: Max van Ghemen, Birgit Sauerbrey, Ludwig Pohl
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Patent number: 5874058Abstract: A continuous method of preparing a single phase lithiated manganese oxide intercalation compound of the formula Li.sub.1+x Mn.sub.2-x O.sub.4 comprising the steps of: mixing intimately a lithium hydroxide or a lithium salt and a manganese oxide or a manganese salt; feeding the intimately mixed salts to a reactor; continuously agitating the mixed salts in the reactor; heating the agitated mixed salts in the reactor at a temperature of from about 650 .degree. C. to about 800.degree. C. for a time not in excess of about 4 hours in an oxygen-containing atmosphere; and cooling the reacted product to less than about 200.degree. C. in an oxygen-containing atmosphere for a time not in excess of about 2 hours.Type: GrantFiled: March 12, 1997Date of Patent: February 23, 1999Assignee: Kerr-McGee Chemical LLCInventors: Stephen W. Sheargold, Terrell N. Andersen
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Patent number: 5866279Abstract: A nonaqueous electrolyte secondary cell, wherein a lithium-containing metal oxide capable of binding and releasing lithium is used as a positive electrode, and a nonaqueous electrolyte containing a lithium salt is used as an electrolyte, in which a spinel type lithium manganese oxide which satisfies the formula:Li?Mn.sub.2-x Li.sub.x !O.sub.4-.delta.wherein 0.ltoreq.x.ltoreq.0.05, and -0.025.ltoreq..delta..ltoreq.0.050, and wherein the average valency of Mn is within a range of from 3.501 to 3.535, is used as the lithium-containing metal oxide.Type: GrantFiled: March 18, 1997Date of Patent: February 2, 1999Assignee: Mitsubishi Chemical CorporationInventors: Hiroshi Wada, Kenji Shizuka
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Patent number: 5855862Abstract: A method for preparing an oxide (P), which includes the steps of (i) forming a solid phase compound (O) based on an oxide containing molecular entities (1) chosen from optionally substituted ammonium, diammonium, diazan-ium or diazandium, the entities being distributed within the solid matrix, and (ii) eliminating the entities (1) from the solid phase compound (O) by reacting the solid phase compound (O) with a gaseous stream containing a break-down reactant for the entities (1), and isolating the resulting solid material (P).Type: GrantFiled: January 8, 1997Date of Patent: January 5, 1999Assignee: Rhone-Poulenc ChimieInventors: Jean-Claude Grenier, Jean-Pierre Doumerc, Stephane Petit
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Patent number: 5840267Abstract: A method for producing a metal oxide powder which comprises heating a metal or metals in an atmosphere gas comprising a halogen gas, a hydrogen halide gas or a mixture of these gases in a concentration of from 0.5% by volume or more to 99.5% by volume or less; and oxygen, water vapor or a mixture of these gases in a concentration of from 0.5% by volume or more to 99.5% by volume or less.Type: GrantFiled: June 27, 1996Date of Patent: November 24, 1998Assignee: Sumitomo Chemical Co., Ltd.Inventor: Kunio Saegusa
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Patent number: 5824285Abstract: In a preferred method, a lithium compound is reacted with a manganese compound in the presence of gaseous ammonia produced by the decomposition of an ammonium compound. In the preferred method, the decomposition of the ammonium compound is initiated before the reaction occurs to form the lithium manganese oxide product spinel. It is also possible to have the decomposition initiated at about the same time as the reaction. It is possible to have the decomposition continue while the reaction to form the spinel occurs. The reaction to form the spinel occurs at an elevated temperature to provide a product of the desired nominal general formula, having a quantity of lithium corresponding to more than 1 atomic units of lithium for every 2 atomic units of manganese. This lithium-rich product, having greater than a 1:1 ratio of Mn.sup.+3 to Mn.sup.+4 is made possible by the presence of the ammonia decomposition gas.Type: GrantFiled: October 23, 1996Date of Patent: October 20, 1998Assignee: Valence Technology, Inc.Inventor: Rene Koksbang
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Patent number: 5820790Abstract: A positive active material for a non-aqueous cell comprising a lithium-manganese composite oxide having an oxygen-defect type spinel structure and its preparing process are disclosed. A cell comprising the positive active material for a non-aqueous cell has excellent properties with high discharge capacity, a monotonous variation of the potential without flection during both charging and discharging, and very limited loss of the electric capacity upon charging and discharging.Type: GrantFiled: November 8, 1995Date of Patent: October 13, 1998Assignee: Japan Storage Battery Co., Ltd.Inventors: Khalil Amine, Hideo Yasuda, Yuko Fujita
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Patent number: 5811068Abstract: Disclosed is a method for producing oxide powders and complex oxide powders having an oxygen amount smaller than the stoichiometric amount. The method comprises: spraying a combustible liquid that contains at least one raw material of metals capable of having a plural number of valences and compounds of such metals; and firing the raw material to give a powder of an oxide of at least one of said metals. The oxygen amount in the atmosphere in which the combustible liquid containing said raw material is sprayed and fired is smaller than the total of the oxygen amount necessary for the complete combustion of said combustible liquid and the oxygen amount necessary for the conversion of said raw material into an oxide that is the most stable in air at room temperature.Type: GrantFiled: January 24, 1997Date of Patent: September 22, 1998Assignee: Kabushiki Kaisha Toyota Chuo KenkyushoInventors: Kazumasa Takatori, Hideo Sobukawa, Naoyoshi Watanabe
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Patent number: 5807532Abstract: As a technique of stably producing a crystalline spinel type LiMn.sub.2 O.sub.4 having a large specific surface area by microscopically uniform mixing at atomic level of constitutional elements without causing crystal defects, there is proposed a method wherein water-soluble lithium salt and manganese nitrate (Mn(NO.sub.3).sub.2) are dissolved in water and then non-ion water-soluble high polymer containing no metal ion is added as a cation carried body to the resulting aqueous mixed solution and thereafter water is removed from the aqueous mixed solution under heating, preferably at a temperature of not lower than 100.degree. C. to synthesize crystalline spinel type LiMn.sub.2 O.sub.4.Type: GrantFiled: September 24, 1996Date of Patent: September 15, 1998Assignee: Japan Metals and Chemicals Co., Ltd.Inventors: Koh Takahashi, Takeshi Sotomura, Keiji Satoh
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Patent number: 5807646Abstract: A novel lithium-manganese oxide composition suitable for use in lithium secondary batteries as an active material for positive electrodes, said oxide having a spinel type crystal structure, an Li:Mn molar ratio of 0.9-1.10:2.00, a mean Mn oxidation number of 3.40-3.60 valencies, and a BET specific surface area of at least 1 m.sup.2 /g, substantially all the primary particles of said oxide being less than 1 .mu.m; a process for preparing such an oxide and a lithium secondary battery containing such an oxide are also disclosed.Type: GrantFiled: February 15, 1996Date of Patent: September 15, 1998Assignee: Tosoh CorporationInventors: Eiichi Iwata, Ken-ichi Takahashi, Setsuo Yoshida, Masaki Okada, Masanori Sawano
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Patent number: 5792442Abstract: 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 18, 1996Date of Patent: August 11, 1998Assignee: FMC CorporationInventors: Vesselin Manev, Titus Faulkner
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Patent number: 5789115Abstract: 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 2, 1997Date of Patent: August 4, 1998Assignee: FMC CorporationInventors: Vesselin Manev, Walter Ebner, William Thompson, Stephen Dow
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Patent number: 5783334Abstract: In a method for producing a lithium nickelate positive electrode, nickel hydroxide or nickel oxyhydroxide is held into an electrically conductive porous substrate to form an electrode plate, the electrode is treated with an alkaline solution containing lithium ion; and the electrode treated with the alkaline solution is heated at a temperature not higher than 450.degree. C.Type: GrantFiled: April 1, 1997Date of Patent: July 21, 1998Assignee: Japan Storage Battery Co., Ltd.Inventor: Hideo Yasuda
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Two powder synthesis of hydrotalcite and hydrotalcite-like compounds with monovalen inorganic anions
Patent number: 5776424Abstract: There is provided a method for making a monovalent inorganic anion-intercalated hydrotalcite-like material by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free, aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a monovalent inorganic anion, in its acid or soluble salt form, to make a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a bromide-, chloride-, nitrate- or vanadate-intercalated, hydrotalcite-like material.Type: GrantFiled: April 9, 1996Date of Patent: July 7, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr. -
Patent number: 5770018Abstract: The present invention provides a method of preparing an intercalation compound of the nominal general formula Li.sub.x Mn.sub.2 O.sub.4, where x is greater than 0 and less than 2, which comprises providing a manganese compound and a lithium compound and mixing such compounds in proportion which provides the desired amount of x demonstrated by the nominal general formula. The mixed compounds are then irradiated with electromagnetic radiation, desirably microwave frequency or infrared radiation whereby manganese, lithium, and oxygen combine to form the Li.sub.x Mn.sub.2 O.sub.4 having the desired quantity x of lithium. It is desired that the heating by radiation be conducted in air. Preferably, the radiation is microwave radiation and such radiation is at a frequency which causes atomic bonds to vibrate within at least a portion of the precursor compounds and/or the solvent contained in the mixture.Type: GrantFiled: April 10, 1996Date of Patent: June 23, 1998Assignee: Valence Technology, Inc.Inventor: M. Yazid Saidi
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Patent number: 5770173Abstract: In producing a cathode active material for a non-aqueous electrolyte secondary battery, an hydroxide or an oxyhydroxide of a 3d transition metal, e.g., MnOOH is exposed to an atmosphere of saturated water vapor containing alkali metal ions in a water mist preferably in a pressurized condition, so that the water mist substitutes the alkali metal ions for protons contained in the hydroxide or the oxyhydroxide.Type: GrantFiled: February 27, 1996Date of Patent: June 23, 1998Assignee: Matsushita Electric Industrial Co., Ltd.Inventors: Yoshiaki Nitta, Masatoshi Nagayama, Tomoaki Seo
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Patent number: 5766569Abstract: A method for manufacturing Li.sub.1+x Mn.sub.2 O.sub.4 comprising the steps of providing LiMn.sub.2 O.sub.4 or .beta.-MnO.sub.2 ; providing a source of lithium; dissolving lithium from the lithium source in a liquid medium in which lithium generates solvated electrons or the reduced form of an electron-transfer catalyst; and contacting the LiMn.sub.2 O.sub.4 or .beta.-MnO.sub.2 with the liquid medium containing the dissolved lithium and the solvated electrons or the reduced form of the electron-transfer catalyst.Type: GrantFiled: January 17, 1996Date of Patent: June 16, 1998Assignee: Kerr-McGee Chemical CorporationInventors: Paul C. Ellgen, Terrell N. Andersen
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Patent number: 5766800Abstract: A novel method of preparing a spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y 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+Y intercalation compound comprises providing a spinel Li.sub.1+X Mn.sub.2-X O.sub.4 intercalation compound having a lithium to manganese mole ratio of between about 1.02:2 and 1.1:2 and firing the spinel at different temperature ranges with corresponding gas flow rates to form the spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y intercalation compounds. The spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y intercalation compounds have a mean X value of between about 0.01 and 0.05, a mean Y value of between about -0.02 and 0.04 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 0.08.degree. and 0.13.degree.. The spinel Li.sub.Type: GrantFiled: June 2, 1997Date of Patent: June 16, 1998Assignee: FMC CorporationInventors: Vesselin Manev, Titus Faulkner
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Patent number: 5762900Abstract: Carbon-doped lithium manganese oxides in crystalline powder form can be used as electrode material. The carbon-doped lithium manganese oxide is prepared by a process including the steps of:preparing a first solution of a lithium compound and a manganese compound, said first solution having lithium ions and manganese ions at a mole ratio of 1:2;preparing a solution of polyethylene glycol and adding the polyethylene glycol solution to said first solution to form a second solution and then drying the second solution until a gel is obtained while stirring the second solution; andpre-treating said gel and then heating the pre-treated gel.Type: GrantFiled: June 20, 1996Date of Patent: June 9, 1998Assignee: Samsung Electronics Co., Ltd.Inventors: Ho-jin Kweon, Hyu-bum Park, Keon Kim
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Patent number: 5759510Abstract: The invention is directed to making a lithiated manganese dioxide using low and high temperature calcination steps.Type: GrantFiled: October 3, 1996Date of Patent: June 2, 1998Assignee: Carus Chemical CompanyInventor: G. Chithambarathanu Pillai
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Patent number: 5759509Abstract: By hydrating a metal oxide solid solution shown as the following formula (3), wherein an average primary crystal particle diameter is in the range of 1 to 10 .mu.m, in the presence of monocarboxylic acid and/or oxymonocarboxylic acid in aqueous medium,Mg.sub.1-z M.sup.2+.sub.z O (3)in which M.sup.2+ represents at least one divalent metal ion selected from the group consisting of Mn.sup.2+, Fe.sup.2+, Co.sup.2+, Ni.sup.2+, Cu.sup.2+ and Zn.sup.2+, and z is in the range of 0.01.ltoreq.z<0.5, a metal hydroxide solid solution having a high aspect ratio shown as the following formula (1) can be obtained;Mg.sub.1-x M.sup.2+.sub.x (OH).sub.2 (1)in which M.sup.2+ represents at least one divalent metal ion selected from the group consisting of Mn.sup.2+, Fe.sup.2+, Co.sup.2+, Ni.sup.2+, Cu.sup.2+ and Zn.sup.2+, and x is in the range of 0.01.ltoreq.x<0.5, characterized by that a crystal is a hexagonal plate in shape, 0.01 to 0.5 .mu.m in average thickness, 1 to 10 .mu.Type: GrantFiled: March 14, 1996Date of Patent: June 2, 1998Assignee: Tateho Chemical Industries Co., Ltd.Inventors: Shigeo Miyata, Ryuichi Ishibashi, Atsuya Kawase, Yasunori Kitano
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Patent number: 5759434Abstract: The present invention provides a compound magnetoresistive material having a perovskite related structure and being represented by M1.sub.m M2.sub.n+1 M3.sub.n Z.sub.y, where: M1 is a first metal comprising at least one element selected from the group consisting of Tl, Bi, Pb, and Hg; M2 is a second metal comprising at least one element selected from the group consisting of alkaline earth metals; M3 is a third metal comprising at least one element selected from the group consisting of Mn, Os, and Ru; Z is one selected from the group consisting of oxygen and anions in which some oxygen elements are replaced by Oh, F, B, Cl, Br, S, Se and Te; m is equal to 1 or 2; 1.ltoreq.n.ltoreq.4; y is variable and depends upon a kind of elements constituting the perovskite related structure, a ratio of composition thereof, and synthesis conditions thereof.Type: GrantFiled: July 22, 1996Date of Patent: June 2, 1998Assignee: NEC CorporationInventors: Yuichi Shimakawa, Yoshimi Kubo, Takashi Manako
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Patent number: 5753202Abstract: A method of making lithium manganese oxide of spinel structure is disclosed. The method involves the step of prelithiating a manganese oxide by reacting it with lithium hydroxide or lithium salt and then reacting the prelithiated manganese oxide in a second step at elevated temperature to form a lithium manganese oxide spinel. In a specific embodiment manganese dioxide powder is reacted with lithium hydroxide to prelithiate the manganese dioxide and the prelithiated manganese dioxide is separated from the reaction mixture and heated and reacted with lithium carbonate at elevated temperature to convert it to lithium manganese oxide spinel. The spinel product may be used advantageously in secondary (rechargeable) batteries.Type: GrantFiled: April 8, 1996Date of Patent: May 19, 1998Assignee: Duracell Inc.Inventors: Enoch I. Wang, William L. Bowden, Paul Gionet
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Patent number: 5747193Abstract: A novel process for making Li.sub.x Mn.sub.y O.sub.4 intercalation compounds, wherein 0<x.ltoreq.2 and 1.7.ltoreq.y.ltoreq.2, comprises the steps of: (1) synthesizing a lithiated manganese oxide precursor by reacting lithium hydroxide, manganese dioxide, and one or more polyhydric alcohols; and (2) heat-treating the lithiated manganese oxide precursor. The intercalation compounds are effectively employed as active components of positive electrodes in rechargeable lithiated intercalation battery cells.Type: GrantFiled: July 11, 1996Date of Patent: May 5, 1998Assignee: Bell Communications Research, Inc.Inventors: Bernard Gerand, Dominique Larcher, Jean-Marie Tarascon
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Patent number: 5742070Abstract: A method for preparing an active substance for use in a positive electrode in chemical cells comprising a negative electrode is described. The method comprises preparing a mixed aqueous solution of a water-soluble lithium compound, a water-soluble transition metal compound, and an organic acid selected from the group consisting of organic acids having, in the molecule, at least one carboxyl group and at least one hydroxyl group and organic acids having at least two carboxyl groups, preparing an organic acid complex comprising lithium and a transition metal, and thermally decomposing the complex at temperatures sufficient for the decomposition to obtain the active substance. The complex may be prepared by dehydrating the solution. Alternatively, the complex may be formed by spraying the solution under heating conditions.Type: GrantFiled: June 3, 1996Date of Patent: April 21, 1998Assignee: Nippondenso Co., Ltd.Inventors: Yasushi Hayashi, Norikazu Adachi, Hisanao Kojima
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Patent number: 5733685Abstract: A method of treating lithium manganese oxide of spinel structure is disclosed. The method involves heating the lithium manganese oxide spinel in an atmosphere of an inert gas which does not react with the spinel. Such gases may be selected advantageously from argon, helium, nitrogen, and carbon dioxide. Preferred nonreacting gases which may be employed for spinel treatment are nitrogen or carbon dioxide. The spinel is advantageously treated with such gases at elevated temperatures. Alternatively, the spinel may be first coated with a hydroxide, preferably lithium, sodium or potassium hydroxide and then heated in an atmosphere of carbon dioxide gas at elevated temperatures. Such treatment of lithium manganese oxide spinel has been determined to improve the performance of the spinel when employed as an electrode in rechargeable cells such as lithium-ion cells.Type: GrantFiled: July 12, 1996Date of Patent: March 31, 1998Assignee: Duracell Inc.Inventor: Enoch I. Wang
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Patent number: 5733681Abstract: Insertion compounds that are not stable in pure water can be prepared by an aqueous electrochemical method. The pH of the electrolyte and/or the concentration of ions of the inserted species must be sufficiently high to provide stability for the product compound. The method is useful for further lithiation of conventional lithium ion battery cathode materials.Type: GrantFiled: December 19, 1996Date of Patent: March 31, 1998Assignee: Moli Energy (1990) LimitedInventors: Wu Li, Jeffrey Raymond Dahn
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Patent number: 5730951Abstract: There is provided a method for making a polyvalent inorganic anion-intercalated hydrotalcite-like material by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free, aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a polyvalent inorganic anion, in its acid, acid salt or ammonium salt form, to make a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a borate- metatungstate- and paramolybdate-intercalated hydrotalcite-like material.Type: GrantFiled: May 14, 1996Date of Patent: March 24, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5728363Abstract: There is provided an improved method for making synthetic hydrotalcite by first reacting powdered magnesium oxide with a high surface area, transition alumina in a solution or suspension to form a meixnerite-like intermediate. This intermediate is then contacted with an anion source such as an acid, and most preferably carbon dioxide, to form the layered double hydroxide which is separated from the suspension by filtering, centrifugation, vacuum dehydration or other known means. On a preferred basis, the transition alumina combined with activated magnesia consists essentially of an rehydratable alumina powder having a surface area of 100 m.sup.2 /g or greater. To make related double hydroxide compounds, still other reactants such as bromides, chlorides, boric acids, or salts thereof, may be substituted for the carbon dioxide gas fed into this suspension.Type: GrantFiled: March 28, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, William E. Horn, Jr., Vito Cedro, III
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Patent number: 5728362Abstract: A mixed metal oxide powder of nominal composition M.sub.x M'.sub.x ' . . . , O.sub.z, wherein M, M', . . . are metal elements and each of x, x', . . . z is greater than zero, is produced by forming an aqueous solution comprising metal salts such that the solution contains at least some of the metal elements of the mixed metal oxide in a desired ratio and comprises at least one oxidizing agent such as a nitrate of one of the metals, and at least one reducing agent such as an organic acid. The oxidizing and the reducing agent as well as the ratio of the former to the latter are chosen such that the thus-formed tuned solution undergoes an exothermic reaction occurs at a desired rate and at a desired small temperature range. Aerosol-droplets of essentially equal dimensions are generated from the tuned solution and are sprayed into a heated gas jet.Type: GrantFiled: August 3, 1995Date of Patent: March 17, 1998Assignee: Asea Brown Boveri AGInventors: Felix Greuter, Daniel Werder
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Patent number: 5728367Abstract: A method for preparing a lithiated transition metal oxide electrochemical charge storage material for use in an electrochemical cell. The cell (10) includes a cathode (20), an anode (30) and an electrolyte (40) disposed therebetween. The method involves the preparation of the lithiated transition metal oxide material in an inert environment. The materials are characterized by improved electrochemical performance, and a multiphase composition in which at least one phase is substantially crystalline, while a second phase is substantially amorphous. By-products of the process may be re-used by converting them into one of the starting materials for the preparation process.Type: GrantFiled: March 18, 1997Date of Patent: March 17, 1998Assignee: Motorola, Inc.Inventor: Zhenhua Mao
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Patent number: 5728366Abstract: There is provided a method for making monovalent organic anion-intercalated hydrotalcite-like materials by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free, aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a monovalent organic anion to form a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a stearate-, acetate- or benzoate-intercalated hydrotalcite-like material.Type: GrantFiled: May 14, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5728364Abstract: There is provided an improved method for making synthetic hydrotalcite by first reacting a divalent metal compound with a trivalent metal oxide powder in a carboxylic acid-free, aqueous solution or suspension to form an intermediate. This intermediate is then contacted with an anion source such as carbon dioxide; a carbonate-containing compound; an acid or an ammonium salt to form a layered double hydroxide having the formula:A.sub.1-x B.sub.x (OH).sub.2 C.sub.z.mH.sub.2 O, where A represents a divalent metal cation, B represents a trivalent metal cation, C represents a mono- to polyvalent anion, and x, z and m satisfy the following conditions: 0.09<x<0.67; z=x/n, where n=the charge on the anion; and 2>m>0.5. Said layered double hydroxide is typically separated from the suspension by filtering, centrifugation, vacuum dehydration or other known means.Type: GrantFiled: April 9, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5728365Abstract: There is provided a method for making a divalent inorganic anion-intercalated hydrotalcite-like material by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a divalent inorganic anion, in its acid, acid salt or ammonium salt form, to make a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a sulfate- and metavanadate-intercalated hydrotalcite-like material.Type: GrantFiled: May 14, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5718877Abstract: A novel method of preparing a spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y 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+Y intercalation compound comprises providing a spinel Li.sub.1+X Mn.sub.2-X O.sub.4 intercalation compound having a lithium to manganese mole ratio of between about 1.02:2 and 1.1:2 and firing the spinel at different temperature ranges with corresponding gas flow rates to form the spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y intercalation compounds. The spinel Li.sub.1+X Mn.sub.2-X O.sub.4+Y intercalation compounds have a mean X value of between about 0.01 and 0.05, a mean Y value of between about -0.02 and 0.04 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 0.08.degree. and 0.13.degree.. The spinel Li.sub.Type: GrantFiled: June 18, 1996Date of Patent: February 17, 1998Assignee: FMC CorporationInventors: Vesselin Manev, Titus Faulkner
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Patent number: 5716737Abstract: A cathode active material for a nonaqueous electrolyte secondary battery is provided. The cathode active material is a composite oxide with a spinel-type structure represented by the general formula Li.sub.2-x ?Mn.sub.2-y Li.sub.y !O.sub.4, wherein -0.1.ltoreq.x<1.0 and 0.3.ltoreq.y.ltoreq.0.35 and wherein the ?Mn.sub.2-y Li.sub.y ! in the general formula is positioned at an octahedral site coordinated by cubic close-packed oxygen ions.Type: GrantFiled: March 14, 1996Date of Patent: February 10, 1998Assignee: Matsushita Electric Industrial Co.Inventors: Masaki Hasegawa, Yasuhiko Bito, Shuji Ito, Toshihide Murata, Yoshinori Toyoguchi
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Patent number: 5702674Abstract: Manganese oxide octahedral molecular sieves are provided in which a portion of the framework manganese is substituted by at least one other metal, e.g., a transition metal.Type: GrantFiled: June 24, 1996Date of Patent: December 30, 1997Assignee: Texaco Inc.Inventors: Chi Lin O'Young, Yan-Fei Shen, Roberto Nguyen Dequzman, Steven Lawrence Suib
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Patent number: 5702679Abstract: A continuous method of preparing a single phase lithiated manganese oxide intercalation compound of the formula Li.sub.1+x Mn.sub.2-x O.sub.4 comprising the steps of: mixing intimately a lithium hydroxide or a lithium salt and a manganese oxide or a manganese salt; feeding the intimately mixed salts to a reactor; continuously agitating the mixed salts in the reactor; heating the agitated mixed salts in the reactor at a temperature of from about 650.degree. C. to about 800.degree. C. for a time not in excess of about 4 hours in an oxygen-containing atmosphere; and cooling the reacted product to less than about 200.degree. C. in an oxygen-containing atmosphere for a time not in excess of about 2 hours.Type: GrantFiled: October 6, 1995Date of Patent: December 30, 1997Assignee: Kerr-McGee Chemical Corp.Inventors: Stephen W. Sheargold, Terrell N. Andersen
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Patent number: 5700442Abstract: The invention relates to the preparation of insertion compounds based on manganese oxide, usable as the positive electrode active material in a lithium battery.These compounds in the hatched area of FIG. 1 can be prepared by reacting in the solid state a manganese oxide powder MnO.sub.2 -.beta., having a specific surface below 7 m.sup.2 /g and an average grain size below 10 .mu.m, with a powder of a lithium compound such as Li.sub.2 CO.sub.3 or LiOH, at a temperature of 150.degree. to 500.degree. C. for an adequate time to convert the .beta.-MnO.sub.2 into manganese and lithium oxide having a lacunary or stoichiometric spinel structure.Type: GrantFiled: June 19, 1995Date of Patent: December 23, 1997Assignees: Commissariat a l'Energie Atomique, Electricite de France Service National, Bollore Technologies S.A., Sadacem, S.A.Inventors: Didier Bloch, Frederic Le Cras, Pierre Strobel
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Patent number: 5693307Abstract: Disclosed is a process for making a lithiated lithium manganese oxide spinel of the formula Li.sub.(1+x)Mn.sub.2 0.sub.4 comprising contacting a lithium manganese oxide spinel of the formula LiMn.sub.2 O.sub.4 with a lithium carboxylate compound, at a temperature and for a time sufficient to decompose the carboxylate compound and free the lithium to form said lithiated spinel.Type: GrantFiled: June 7, 1995Date of Patent: December 2, 1997Assignee: Duracell, Inc.Inventors: William L. Bowden, Andrew Kallmes, Enoch Wang
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Patent number: 5688480Abstract: A complex metal oxide powder having at least two metal elements, which contains polyhedral particles each having at least 6 planes, a number average particle size of from 0.1 to 500 .mu.m, and a D.sub.90 /D.sub.10 ratio of 10 or less in which D.sub.10 and D.sub.90 are particle sizes at 10% and 90% accumulation, respectively from the smallest particle size side in a cumulative particle size curve of the particles, and an yttrium-aluminum garnet powder containing polyhedral particles each having at least 6 planes, and a number average particle size of 20 to 500 .mu.m. These complex metal oxides contain less agglomerated particles, and have a narrow particle size distribution and a uniform particle shape.Type: GrantFiled: May 15, 1995Date of Patent: November 18, 1997Assignee: Sumitomo Chemical Company, LimitedInventors: Masahide Mohri, Hironobu Koike, Tetsu Umeda
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Patent number: 5683835Abstract: Lithium manganese ternary oxide Li Mn.sub.2 0.sub.4+x is produced, where 0.ltoreq..times..ltoreq.0.2, by adding carbon to a manganese-containing solution such as manganese acetate and reacting the solution in an inert atmosphere with a lithium-containing compound such as lithium hydroxide and ammonia. Carbon is added in a proportion up to 8 percent of the weight of the Li Mn.sub.2 0.sub.4+x produced, and preferably the proportion of carbon added is in the range 2 to 6 percent by weight of Li Mn.sub.2 0.sub.4+x. The carbon is preferably carbon powder such as carbon black. Preferably, the Li Mn.sub.2 0.sub.4+x produced as a gelatinous precipitate is dried and heat treated. Alternatively, lithium manganese ternary oxide Li Mn.sub.2 0.sub.4+x is produced by reacting a manganese-containing compound with lithium carbonate. The reaction takes place in water and a precipitate is formed which is dried. The dried precipitate may be heat treated. The manganese-containing compound comprises manganese acetate.Type: GrantFiled: September 15, 1995Date of Patent: November 4, 1997Assignee: Ultralife Batteries (UK) LimitedInventor: Peter George Bruce
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Patent number: 5677087Abstract: A positive electrode active material for lithium battery which is represented by general formula Li.sub.x Mn.sub.2-y M.sub.y O.sub.4 (M: a 2-valency metal selected from Ni, Co, Fe and Zn with 0.45.ltoreq.y.ltoreq.0.60, 1.ltoreq.x.ltoreq.2.1) having cubic spinel structure of lattice constant within 8.190 angstrom. Such an active material is manufactured by employing sol-gel process wherein one of inorganic salt, hydroxide and organic acid salt of lithium or a mixture of these for Li, one of inorganic salt and organic acid salt of manganese or a mixture of these for Mn, and one of inorganic salt and organic acid salt of the selected metal or a mixture of these for M are used as the starting materials for synthesis, ammonia water is added to the solutions of these starting materials in alcohol or water to obtain gelatinous material and the gelatinous material thus obtained is fired.Type: GrantFiled: October 9, 1996Date of Patent: October 14, 1997Assignee: Japan Storage Battery Co., Ltd.Inventors: Khalil Amine, Hideo Yasuda, Yuko Fujita
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Patent number: 5674645Abstract: The cycling stability and capacity of li-ion rechargeable batteries are improved by the use of lithium manganese oxy-fluoride electrode component intercalation materials having the general formula, Li.sub.1+x M.sub.y Mn.sub.2-x-y O.sub.4-z F.sub.z, where M is a transition metal, e.g., Co, Cr, or Fe, and x.ltoreq.0.4, y.ltoreq.0.3, and 0.05.ltoreq.z.ltoreq.1.0.Type: GrantFiled: September 6, 1996Date of Patent: October 7, 1997Assignee: Bell Communications Research, Inc.Inventors: Glenn G. Amatucci, Jean-Marie Tarascon