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US4065544A Expired / Lapsed US ⏱️ 0.0 years remaining

Finely divided metal oxides and sintered objects therefrom

Assignee: Kemet Electronics Corp
•
Filing: 1974-06-20
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Granted: 1977-12-27
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Expires: 1994-06-20
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Abstract

Abstract Finely-divided metal oxides are prepared by the steps of (a) contacting a compound of a metal with a carbohydrate material to obtain an intimate mixture thereof, (b) igniting this mixture to oxidize the same and to insure conversion of substantially all of said metal compound to a fragile agglomerate of its metal oxide, and (c) pulverizing the product of step (b) to form a finely-divided metal oxide powder having a mean particle size below about 1.0 micron. Certain of the finely-divided metal oxide powders produced by this process have the useful property of sinterability at temperatures significantly lower than metal oxide powders heretofore readily available. The powders are useful in the preparation of high strength compacted shapes for use in high temperature and/or corrosive environment, in the preparation of refractory cements, catalysts, catalysts supports and the like.

Inventors

  • 👤 Bernard H. Hamling
  • 👤 Alfred W. Naumann

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-27 19:35
CPC Classifications
H; H01; H01F; H01F1/00; H01F1/01; H01F1/03; H01F1/032; H01F1/10; H01F1/11; B; B01; B01J; B01J37/00; B01J37/0009; B01J37/0018; B82; B82Y; B82Y30/00; C; C01; C01B; C01B13/00; C01B13/14; C01B13/32; C01B13/322; C01F; C01F17/00; C01F17/20; C01F17/206; C01F17/224; C01F17/229; C01G; C01G23/00; C01G23/003; C01G23/006; C01G23/04; C01G23/047; C01G25/00; C01G25/02; C01G37/00; C04; C04B; C04B35/00; C04B35/01; C04B35/26; C04B35/2683; C04B35/46; C04B35/462; C04B35/465; C04B35/468; C04B35/4682; C04B35/48; C04B35/486; C04B35/50; C04B35/51; C04B35/622; C04B35/626; G; G11; G11B; G11B5/00; G11B5/62; G11B5/68; G11B5/70; G11B5/706; G11B5/70626; G11B5/70642; G11B5/70678; C01P; C01P2002/00; C01P2002/60; C01P2002/70; C01P2004/00; C01P2004/01; C01P2004/03; C01P2004/50; C01P2004/60; C01P2004/62; C01P2004/64; C01P2006/00; C01P2006/10; C01P2006/12; C01P2006/13; C01P2006/32; C01P2006/33

Claims Analysis

Total Claims: 43
Claim 1
Independent Claim 116 words
Process for producing finely divided metal oxygen-containing compounds which comprises: a. contacting a carbohydrate material with at least one compound of a metal to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said metal compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of submicron size metal oxygen-containing particles; d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided metal oxygen-containing compounds having a mean particle size below one micron.
Claim 2
Dependent Claim 116 words
Process for producing finely divided metal oxygen-containing compounds which comprises: a. contacting a carbohydrate material with at least one compound of a metal to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said metal compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of submicron size metal oxygen-containing particles; d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided metal oxygen-containing compounds having a mean particle size below one micron.
Claim 3
Dependent Claim 11 words
The process of claim 1 wherein said carbohydrate material is cellulosic.
Claim 4
Dependent Claim 12 words
The process of claim 1 wherein said carbohydrate material is wood pulp.
Claim 5
Dependent Claim 11 words
The process of claim 1 wherein said carbohydrate material is cotton.
Claim 6
Dependent Claim 12 words
The process of claim 1 wherein said carbohydrate material is a sugar.
Claim 7
Dependent Claim 10 words
The process of claim 5 wherein said sugar is sucrose.
Claim 8
Dependent Claim 11 words
The process of claim 5 wherein said sugar is invert syrup.
Claim 9
Dependent Claim 14 words
The process of claim 1 wherein said metal oxygen-containing compound is a metal oxide.
Claim 10
Dependent Claim 13 words
The process of claim 1 wherein said metal oxygen-containing compound is a ferrite.
Claim 11
Dependent Claim 57 words
The process of claim 1 wherein said oxygen-containing compounds are comprised of at least one metal which is selected from the group consisting of beryllium, magnesium, calcium, the Group III B metals, the Group IV B metals, niobium, tantalum, the Group VI B metals, manganese, iron, cobalt, nickel, copper, zinc, cadmium, aluminum; gallium, tin, lead and bismuth.
Claim 12
Dependent Claim 83 words
The process of claim 1 wherein said oxygen-containing compounds are comprised of at least one metal which is selected from the group consisting of beryllium, magnesium, calcium, the Group IIIB metals, the Group IVB metals, niobium, tantalum, the Group VIB metals, manganese, iron, cobalt, nickel, copper, zinc, cadmium, aluminum, gallium, tin, lead and bismuth, and at least one additional metal selected from the group consisting of lithium, sodium, potassium, rubidium, cesium, strontium, barium, germanium, vanadium, ruthenium, osmium, rhodium, indium, iridium, thallium and antimony.
Claim 13
Dependent Claim 19 words
Process of claim 1 wherein in step (a), said metal compound comprises an aqueous solution of a zirconium compound.
Claim 14
Dependent Claim 28 words
Process of claim 12 wherein said aqueous solution of a zirconium compound also contains dissolved therein a compound of a metal that forms an oxide that stabilizes zirconia.
Claim 15
Dependent Claim 16 words
Process of claim 13 wherein said metal that forms an oxide that stabilizes zirconia is yttrium.
Claim 16
Dependent Claim 13 words
Process of claim 12 wherein the zirconia is comminuted by wet ball milling.
Claim 17
Dependent Claim 30 words
Process of claim 12 wherein said aqueous solution of a zirconium compound also contains dissolved therein at least one copper and at least one chromium compound that forms an oxide.
Claim 18
Dependent Claim 28 words
Process of claim 1 wherein in step (a), said metal compounds comprise at least one barium and one titanium compound, said mixture being essentially free of chloride ions.
Claim 19
Dependent Claim 140 words
A process for the preparation of submicron barium titanate powders which process comprises the steps of: a. contacting a water soluble carbohydrate with an aqueous acidic solution of a tetraalkyl titanate and an aqueous solution of barium alkanoate, to form an intimate mixture thereof, said mixture being essentially free of chloride ions, b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said barium titanate compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of sub-micron size barium titanate particles, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided barium titanate powder having a mean particle size below one micron.
Claim 20
Dependent Claim 140 words
A process for the preparation of submicron barium titanate powders which process comprises the steps of: a. contacting a water soluble carbohydrate with an aqueous acidic solution of a tetraalkyl titanate and an aqueous solution of barium alkanoate, to form an intimate mixture thereof, said mixture being essentially free of chloride ions, b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said barium titanate compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of sub-micron size barium titanate particles, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided barium titanate powder having a mean particle size below one micron.
Claim 21
Dependent Claim 14 words
The process of claim 17 wherein said barium and titanium compounds are organic compounds.
Claim 22
Dependent Claim 12 words
The process of claim 17 wherein said barium compound is barium acetate.
Claim 23
Dependent Claim 12 words
The process of claim 17 wherein said titanium compound is triethanolamine titanate.
Claim 24
Dependent Claim 12 words
The process of claim 17 wherein said titanium compound is tetraisopropyl titanate.
Claim 25
Dependent Claim 14 words
The process of claim 17 wherein said barium titanate also contains other metal oxides.
Claim 26
Dependent Claim 179 words
A process for producing a sintered article comprised of a metal oxide which is sinterable to essentially its theoretical density at low temperatures, sid article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of a metal to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said metal compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of metal oxide particles of sub-micron size, d. disrupting sid agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided metal oxide powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article at a temperature and for a period of time sufficient to form said article.
Claim 27
Dependent Claim 179 words
A process for producing a sintered article comprised of a metal oxide which is sinterable to essentially its theoretical density at low temperatures, sid article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of a metal to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said metal compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of metal oxide particles of sub-micron size, d. disrupting sid agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided metal oxide powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article at a temperature and for a period of time sufficient to form said article.
Claim 28
Dependent Claim 168 words
A process for producing a sintered article comprised of zirconia essentially at its theoretical density, said article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of zirconium to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said zirconium compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of zirconia particles of sub-micron size, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised the agglomerates to produce finely divided zirconia powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 29
Dependent Claim 168 words
A process for producing a sintered article comprised of zirconia essentially at its theoretical density, said article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of zirconium to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said zirconium compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of zirconia particles of sub-micron size, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised the agglomerates to produce finely divided zirconia powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 30
Dependent Claim 168 words
A process for producing a sintered article comprised of thoria essentially at its theoretical density, said article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of thorium to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but sufficient to substantially sinter said thorium compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of thoria particles of sub-micron size, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised the agglomerates to produce finely divided thoria powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 31
Dependent Claim 168 words
A process for producing a sintered article comprised of thoria essentially at its theoretical density, said article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of thorium to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but sufficient to substantially sinter said thorium compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of thoria particles of sub-micron size, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised the agglomerates to produce finely divided thoria powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 32
Dependent Claim 13 words
The sintered article comprised of thoria prepared by the process of claim 26.
Claim 33
Dependent Claim 168 words
A process for producing a sintered article comprised of erbia essentially at its theoretical density, said article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of erbium to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said erbium compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material to produce easily disrupted agglomerates of erbia particles of sub-micron size, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised the agglomerates to produce finely divided erbia powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 34
Dependent Claim 168 words
A process for producing a sintered article comprised of erbia essentially at its theoretical density, said article having a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with a compound of erbium to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said erbium compound; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material to produce easily disrupted agglomerates of erbia particles of sub-micron size, d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised the agglomerates to produce finely divided erbia powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 35
Dependent Claim 13 words
A sintered article comprised of erbia prepared by the process of claim 28.
Claim 36
Dependent Claim 195 words
A process for producing a sintered article comprised of two or more metal oxides, said article having a surface area which is at least 10 square meters per gram, and a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with two or more compounds of a metal to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said metal compounds; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of metal oxide particles of sub-micron size, at least some of which metal oxide particles are sinterable; d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided metal oxide powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 37
Dependent Claim 195 words
A process for producing a sintered article comprised of two or more metal oxides, said article having a surface area which is at least 10 square meters per gram, and a compressive strength of at least 5,000 pounds per square inch, which process comprises: a. contacting a carbohydrate material with two or more compounds of a metal to form an intimate mixture thereof; b. introducing said mixture into a heating zone having a temperature sufficient to ignite said mixture but insufficient to substantially sinter said metal compounds; c. igniting said mixture in said heating zone for a time period sufficient to decompose and remove said carbohydrate material and produce easily disrupted agglomerates of metal oxide particles of sub-micron size, at least some of which metal oxide particles are sinterable; d. disrupting said agglomerates without substantially reducing the size of the individual particles which comprised said agglomerates to produce finely divided metal oxide powder having a mean particle size of less than 0.1 micron, e. shaping and compacting said powder into the form of said article, and f. sintering said shaped article, at a temperature and for a period of time sufficient to form said article.
Claim 38
Dependent Claim 18 words
The process of claim 30 wherein said sintered article is comprised of the oxides of zirconium and aluminum.
Claim 39
Dependent Claim 24 words
The process of claim 31 wherein said oxide of aluminum is present in an amount of from about 5 to about 70 weight percent.
Claim 40
Dependent Claim 18 words
The process of claim 30 wherein said sintered article is comprised of the oxides of copper and aluminum.
Claim 41
Dependent Claim 24 words
The process of claim 33 wherein said oxide of aluminum is present in an amount of from about 5 to about 70 weight percent.
Claim 42
Dependent Claim 21 words
A sintered article comprised of the oxides of copper and aluminum, said article being prepared by the process of claim 30.
Claim 43
Dependent Claim 25 words
The sintered article of claim 35 wherein aid oxide of aluminum is present in an amount of from about 5 to about 70 weight percent.

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-12-26 1981-06-27 1981-12-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-12-26 1985-06-27 1985-12-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-12-26 1989-06-27 1989-12-27 $7700.00 Window Closed / Lapsed

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