RU2010109437A - NANOSTRUCTURES CONSISTING OF VENTAL METALS AND VENTIL METAL SUXOXIDES AND THE METHOD FOR PRODUCING THEM - Google Patents

NANOSTRUCTURES CONSISTING OF VENTAL METALS AND VENTIL METAL SUXOXIDES AND THE METHOD FOR PRODUCING THEM Download PDF

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RU2010109437A
RU2010109437A RU2010109437/02A RU2010109437A RU2010109437A RU 2010109437 A RU2010109437 A RU 2010109437A RU 2010109437/02 A RU2010109437/02 A RU 2010109437/02A RU 2010109437 A RU2010109437 A RU 2010109437A RU 2010109437 A RU2010109437 A RU 2010109437A
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valve metal
structures
suboxide
metal
reducing
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RU2010109437/02A
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RU2493939C2 (en
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Герхард ГИЛЛЕ (DE)
Герхард ГИЛЛЕ
Кристоф ШНИТТЕР (DE)
Кристоф ШНИТТЕР
Хольгер БРУММ (DE)
Хольгер БРУММ
Хельмут ХААС (DE)
Хельмут ХААС
Роберт МЮЛЛЕР (DE)
Роберт МЮЛЛЕР
Манфред БОБЕТ (DE)
Манфред БОБЕТ
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Х. К. Штарк Гмбх (De)
Х. К. Штарк Гмбх
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Priority claimed from DE102007057761A external-priority patent/DE102007057761A1/en
Application filed by Х. К. Штарк Гмбх (De), Х. К. Штарк Гмбх filed Critical Х. К. Штарк Гмбх (De)
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/24Obtaining niobium or tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/04Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004Details
    • H01G9/04Electrodes or formation of dielectric layers thereon
    • H01G9/048Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/052Sintered electrodes
    • H01G9/0525Powder therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1263Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1268Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004Details
    • H01G9/04Electrodes or formation of dielectric layers thereon
    • H01G9/048Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/052Sintered electrodes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/12All metal or with adjacent metals
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/12All metal or with adjacent metals
    • Y10T428/12431Foil or filament smaller than 6 mils
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/12All metal or with adjacent metals
    • Y10T428/12431Foil or filament smaller than 6 mils
    • Y10T428/12438Composite

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Nanotechnology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Powder Metallurgy (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)

Abstract

1. Подобные полосам или листам структуры вентильного металла и субоксида вентильного металла, имеющие поперечный размер от 5 до 100 нм. ! 2. Структуры вентильного металла и субоксида вентильного металла по п.1, имеющие первичную структуру, подобную листу или слою, в форме порошков. ! 3. Структуры вентильного металла и субоксида вентильного металла по п.1 в форме структур поверхностных полос. ! 4. Структуры вентильного металла по п.3 в форме фольги или проводов, имеющих полосы, имеющие ширину от 5 до 100 нм и расстояние между полосами величиной от одного до 2 раз больше ширины полосы. ! 5. Структуры вентильного металла и субоксида вентильного металла по п.1, где полосы или ламеллы расположены параллельно в группах. ! 6. Структуры вентильного металла и субоксида вентильного металла п.1, где поперечный размер или ширина полосы составляет от 8 до 50 нм. ! 7. Структуры вентильного металла п.1, содержащие в качестве вентильного металла Ti, Zr, V, Nb, Та, Мо, W, Hf или Аl, в особенности, Nb или Та, или их сплавы. ! 8. Структуры субоксида вентильного металла п.1, имеющие формулу NbOx, где 0,7<х<1,3. ! 9. Структуры вентильного металла и субоксида вентильного металла по любому из пп.1-8, отличающиеся содержанием, по меньшей мере, одного восстанавливающего металла в количестве от 10 до 500 млн. долей. ! 10. Способ восстановления оксидов вентильных металлов посредством паров восстанавливающих металлов при температуре, достаточной для восстановления, с формированием слоистых наноструктур, отличающийся тем, что оксид восстановленного вентильного металла замораживают до термического разложения слоистой структуры и превращения в огрубленные структуры. ! 11. Способ по п.10, 1. Strip-like or sheet-like structures of valve metal and valve metal suboxide having a transverse dimension of 5 to 100 nm. ! 2. The valve metal and valve metal suboxide structures of claim 1 having a primary structure like a sheet or layer in the form of powders. ! 3. Valve metal structures and valve metal suboxide according to claim 1 in the form of surface strip structures. ! 4. The valve metal structures of claim 3 in the form of foils or wires having strips having a width of 5 to 100 nm and a distance between the strips of one to 2 times the width of the strip. ! 5. The valve metal and valve metal suboxide structures of claim 1, wherein the stripes or lamellae are arranged in parallel in groups. ! 6. Valve metal and valve metal suboxide structures of claim 1, wherein the transverse dimension or bandwidth is 8 to 50 nm. ! 7. Valve metal structures of claim 1, containing as valve metal Ti, Zr, V, Nb, Ta, Mo, W, Hf or Al, in particular Nb or Ta, or their alloys. ! 8. Structures of valve metal suboxide of claim 1, having the formula NbOx, where 0.7 <x <1.3. ! 9. Valve metal and valve metal suboxide structures according to any one of claims 1 to 8, characterized by the content of at least one reducing metal in an amount from 10 to 500 ppm. ! 10. A method of reducing valve metal oxides by means of reducing metal vapors at a temperature sufficient for reduction, with the formation of layered nanostructures, characterized in that the reduced valve metal oxide is frozen to thermal decomposition of the layered structure and transformation into coarse structures. ! 11. The method according to claim 10,

Claims (14)

1. Подобные полосам или листам структуры вентильного металла и субоксида вентильного металла, имеющие поперечный размер от 5 до 100 нм.1. Strip-like or sheet-like structures of a valve metal and valve metal suboxide having a transverse size of 5 to 100 nm. 2. Структуры вентильного металла и субоксида вентильного металла по п.1, имеющие первичную структуру, подобную листу или слою, в форме порошков.2. Valve metal and valve metal suboxide structures according to claim 1, having a primary structure similar to a sheet or layer in the form of powders. 3. Структуры вентильного металла и субоксида вентильного металла по п.1 в форме структур поверхностных полос.3. Valve metal structures and valve metal suboxide according to claim 1 in the form of surface strip structures. 4. Структуры вентильного металла по п.3 в форме фольги или проводов, имеющих полосы, имеющие ширину от 5 до 100 нм и расстояние между полосами величиной от одного до 2 раз больше ширины полосы.4. The valve metal structure according to claim 3 in the form of foil or wires having strips having a width of 5 to 100 nm and a distance between strips of one to 2 times the width of the strip. 5. Структуры вентильного металла и субоксида вентильного металла по п.1, где полосы или ламеллы расположены параллельно в группах.5. The valve metal and valve metal suboxide structures of claim 1, wherein the strip or lamella is arranged in parallel in groups. 6. Структуры вентильного металла и субоксида вентильного металла п.1, где поперечный размер или ширина полосы составляет от 8 до 50 нм.6. The valve metal and valve metal suboxide structures of claim 1, wherein the transverse size or bandwidth is from 8 to 50 nm. 7. Структуры вентильного металла п.1, содержащие в качестве вентильного металла Ti, Zr, V, Nb, Та, Мо, W, Hf или Аl, в особенности, Nb или Та, или их сплавы.7. The valve metal structures of claim 1, containing Ti, Zr, V, Nb, Ta, Mo, W, Hf or Al, especially Nb or Ta, or their alloys as the valve metal. 8. Структуры субоксида вентильного металла п.1, имеющие формулу NbOx, где 0,7<х<1,3.8. Valve metal suboxide structures of claim 1, having the formula NbO x , where 0.7 <x <1.3. 9. Структуры вентильного металла и субоксида вентильного металла по любому из пп.1-8, отличающиеся содержанием, по меньшей мере, одного восстанавливающего металла в количестве от 10 до 500 млн. долей.9. Valve metal and valve metal suboxide structures according to any one of claims 1 to 8, characterized in at least one reducing metal in an amount of from 10 to 500 million shares. 10. Способ восстановления оксидов вентильных металлов посредством паров восстанавливающих металлов при температуре, достаточной для восстановления, с формированием слоистых наноструктур, отличающийся тем, что оксид восстановленного вентильного металла замораживают до термического разложения слоистой структуры и превращения в огрубленные структуры.10. A method of reducing valve metal oxides by means of reducing metal vapors at a temperature sufficient to reduce, with the formation of layered nanostructures, characterized in that the oxide of the reduced valve metal is frozen until the thermal decomposition of the layered structure and transformation into coarsened structures. 11. Способ по п.10, отличающийся тем, что восстановление проводят при давлении инертного газа менее 0,2 бара и давлении паров восстанавливающего металла от 10-2 до 0,4 бара.11. The method according to claim 10, characterized in that the reduction is carried out at an inert gas pressure of less than 0.2 bar and a vapor pressure of the reducing metal from 10 -2 to 0.4 bar. 12. Способ по п.10, отличающийся тем, что продукт восстановления охлаждают до температуры ниже 100°С в течение нескольких минут немедленно после того, как восстановление завершено.12. The method according to claim 10, characterized in that the reduction product is cooled to a temperature below 100 ° C for several minutes immediately after the recovery is completed. 13. Способ по п.10, отличающийся тем, что Li, Al, Mg и/или Са, в особенности Mg, используют в качестве восстанавливающего металла.13. The method according to claim 10, characterized in that Li, Al, Mg and / or Ca, in particular Mg, is used as a reducing metal. 14. Способ по любому из пп.10-13, отличающийся тем, что оксиды Al, Hf, Ti, Zr, V, Nb, Та, Мо и/или W и их смешанные оксиды, в особенности Nb или Та, используют в качестве оксидов, подлежащих восстановлению. 14. The method according to any one of claims 10 to 13, characterized in that the oxides of Al, Hf, Ti, Zr, V, Nb, Ta, Mo and / or W and their mixed oxides, in particular Nb or Ta, are used as oxides to be reduced.
RU2010109437/02A 2007-08-16 2008-07-23 Nanostructures consisting of gate metals and gate metal sub oxides and methods of their production RU2493939C2 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE102007038581A DE102007038581A1 (en) 2007-08-16 2007-08-16 Valve metal structure and valve metal sub-oxide structure, have lateral dimension of 5 to 10 nanometers and are expanded in streaky or flat manner and valve metal structures are in form of foils or wires
DE102007038581.3 2007-08-16
DE102007057761.5 2007-11-30
DE102007057761A DE102007057761A1 (en) 2007-11-30 2007-11-30 Strip-like or sheet-like valve metal and valve metal suboxide structures in the form of surface strip structures, foils, or wires, useful e.g. as catalysts and support materials for catalysts, have specified transverse dimension
PCT/EP2008/059659 WO2009021820A1 (en) 2007-08-16 2008-07-23 Nanosize structures composed of valve metals and valve metal suboxides and process for producing them

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EP (1) EP2188081A1 (en)
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EP2188081A1 (en) 2010-05-26
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KR101530727B1 (en) 2015-06-22
KR20100065280A (en) 2010-06-16
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US20110123822A1 (en) 2011-05-26
CN104889381A (en) 2015-09-09
WO2009021820A1 (en) 2009-02-19
JP5542672B2 (en) 2014-07-09
MX2010001586A (en) 2010-03-15
RU2493939C2 (en) 2013-09-27

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