EP0667200B1 - Herstellung von Reinstmetallpulver aus Metallalkoxiden - Google Patents
Herstellung von Reinstmetallpulver aus Metallalkoxiden Download PDFInfo
- Publication number
- EP0667200B1 EP0667200B1 EP95101419A EP95101419A EP0667200B1 EP 0667200 B1 EP0667200 B1 EP 0667200B1 EP 95101419 A EP95101419 A EP 95101419A EP 95101419 A EP95101419 A EP 95101419A EP 0667200 B1 EP0667200 B1 EP 0667200B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- tungsten
- alkoxide
- metal
- tantalum
- methoxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
- B22F2201/013—Hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2203/00—Controlling
- B22F2203/11—Controlling temperature, temperature profile
Definitions
- the present invention relates to a method for producing high-purity Metal powder.
- the microfabrication of highly integrated electronic components always poses higher requirements for the purity of the interconnect metals, e.g. Titanium, Niobium, tantalum, molybdenum or tungsten.
- the radioactive elements Thorium and uranium, as ⁇ -emitters can have serious consequences in highly integrated applications Cause memory chips.
- Ion exchange resins are used, as in Metallurgy of the Rarer Metals, Volume 6, Tantalum and Niobium, page 129-133.
- Tungsten hexafluoride Distillative separation via the metal halides, e.g. Tungsten hexafluoride in principle also possible.
- This method is the subject of JP-A 02 30,706.
- Tungsten hexafluoride is converted to tungsten powder with hydrogen at 650-1400 ° C reduced, which is suitable for the production of sputtering targets.
- Disadvantage of this The process is that in the reduction with hydrogen, a large amount of hydrogen fluoride attack.
- the object of this invention was therefore to provide a process for the production of to provide high purity metal powder which is simple and can be carried out inexpensively. This problem is solved by Implementation of volatile, i.e. sublimable or distillable, Metal alkoxides with a reaction gas.
- This method is the subject of this invention.
- the metal alkoxide compounds which are used according to the invention have the general formula M (OR) x , where M is a metal from Group 3-14 (according to IUPAC 1985), R is an alkyl, aryl, cycloalkyl or aralkyl radical and M (OR ) x is a sublimable or distillable compound.
- M is a metal from Group 3-14 (according to IUPAC 1985)
- R is an alkyl, aryl, cycloalkyl or aralkyl radical
- M (OR ) x is a sublimable or distillable compound.
- some alkoxide compounds that are suitable according to the invention are listed as examples.
- Metal alkoxide boiling point Aluminum isopropylate 128 ° C / 5 mbar Chromium (IV) tert-butoxide 66 ° C / 3.6 mbar Gallium ethylate 185 ° C / 0.7 mbar Niobium methylate 153 ° C / 0.13 mbar Niobium ethylate 156 ° C / 0.07 mbar Tantalum methylate 130 ° C / 0.3 mbar Tantalum ethylate 146 ° C / 0.2 mbar Titanium ethylate 104 ° C / 1.3 mbar Tungsten methylate 90 ° C / 0.5 mbar
- the reaction gas in the reaction according to the invention is preferably hydrogen.
- the reaction gas can also be mixed with an inert carrier gas, in particular argon be diluted.
- the method according to the invention is preferably at a temperature between 400 ° C and 1400 ° C carried out.
- the most preferred reaction temperature lies between 600 ° C and 1200 ° C.
- WF 6 is converted into W (OCH 3 ) 6 in an equilibrium reaction with volatile Si (OCH 3 ) 4 as ligand transfer agent.
- OCH 3 volatile Si
- Complete methoxylation is only possible by treating the partially fluorinated product with a methanolic NaOCH 3 solution.
- Suitable reactors for carrying out the process according to the invention can Furnaces with an adjustable atmosphere or gas phase reactors. Since the metal alkoxide compounds according to the invention all in a simple manner in the gas phase to be brought is also a gas phase reactor according to DE-A 4 214 720 suitable. The choice of reactor is determined by the particular requirements regarding fine particle size and particle size distribution of the metal powder.
- a 0.5 molar solution of LiCl in methanol was electrolysed under argon protective gas in a flat ground reaction vessel which was provided with a steel cathode, an anode made of tungsten and a reflux condenser. It was electrolyzed with direct current and a current density of 200 mA / cm 2 . The electrolyte solution turned yellow-orange and began to boil shortly after the start of electrolysis.
- a solution of 50 g of NH 4 Cl in 2000 ml of methanol was electrolysed under argon protective gas in a flat-ended reaction vessel which was provided with a steel cathode, an anode made of tantalum and a reflux condenser. It was electrolyzed with direct current and a current density of 200 mA / cm 2 .
- the electrolytic solution turned yellowish and began to boil shortly after the start of the electrolysis.
- Electrochemically produced tungsten ethoxide is purified by sublimation in a glass apparatus and then reacted with hydrogen in a tube furnace at 1000 ° C., equation (2).
- the tungsten metal powder was analyzed for impurities using GDMS (glow-discharge mass spectroscopy). Analysis of the tungsten metal powder, values in ppm.
- Al 1 B ⁇ 0.05 Ba 0.09 Bi ⁇ 0.02 Approx 0.34 CD ⁇ 0.05 Co 0.08 Cr 0.26 Cu 0.06 Fe 0.31 K ⁇ 0.05 Mg 5 Mn 0.015 Mon 6 N / A 0.2 Ni 0.12 P 0.19 Pb 0.03 Sb ⁇ 0.05 Si 9 Sn ⁇ 0.05 Sr. ⁇ 0.02 Th ⁇ 0.0005 Ti 0.48 U ⁇ 0.0005 V ⁇ 0.02 Zn ⁇ 0.02 Zr ⁇ 0.05
- Electrochemically produced tantalum methoxide is purified by distillation at 130 ° C. in a vacuum (0.3 mbar) in a glass apparatus and then reacted with hydrogen in a tube furnace at 1000 ° C., equation (3).
- Ta (OCH 3 ) 5 + 21 ⁇ 2 H 2 ⁇ Ta + 5 CH 3 OH The tantalum metal powder was analyzed for impurities using GDMS (glow-discharge mass spectroscopy). Analysis of the tantalum metal powder, values in ppm.
- Electrochemically produced titanium ethoxide is purified by distillation at 104 ° C. in a vacuum (0.3 mbar) in a glass apparatus and then reacted with hydrogen in a tube furnace at 1000 ° C., equation (4).
- the titanium metal powder was analyzed for impurities using GDMS (glow-discharge mass sprectroscopy). Analysis of the titanium metal powder, values in ppm.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Carbon And Carbon Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Metallalkoxid | Siedepunkt |
Aluminiumisopropylat | 128°C/5 mbar |
Chrom(IV)-tert.-butylat | 66°C/3,6 mbar |
Galliumethylat | 185°C/0,7 mbar |
Niobmethylat | 153°C/0,13 mbar |
Niobethylat | 156°C/0,07 mbar |
Tantalmethylat | 130°C/0,3 mbar |
Tantalethylat | 146°C/0,2 mbar |
Titanethylat | 104°C/1,3 mbar |
Wolframmethylat | 90°C/0,5 mbar |
Analyse des Wolframmetallpulvers, Werte in ppm. | |||||||||
Al | 1 | B | <0,05 | Ba | 0,09 | Bi | <0,02 | Ca | 0,34 |
Cd | <0,05 | Co | 0,08 | Cr | 0,26 | Cu | 0,06 | Fe | 0,31 |
K | <0,05 | Mg | 5 | Mn | 0,015 | Mo | 6 | Na | 0,2 |
Ni | 0,12 | P | 0,19 | Pb | 0,03 | Sb | <0,05 | Si | 9 |
Sn | <0,05 | Sr | <0,02 | Th | <0,0005 | Ti | 0,48 | U | <0,0005 |
V | <0,02 | Zn | <0,02 | Zr | <0,05 |
Analyse des Tantalmetallpulvers, Werte in ppm. | |||||||||
Al | 0,5 | B | <0,05 | Ba | 0,09 | Bi | <0,02 | Ca | 0,4 |
Cd | <0,05 | Co | 0,05 | Cr | 0,04 | Cu | 0,06 | Fe | 0,2 |
K | <0,05 | Mg | 3 | Mn | 0,015 | Mo | 0,9 | Na | 0,4 |
Nb | 8 | Ni | 0,15 | P | 0,1 | Pb | 0,03 | Sb | <0,05 |
Si | 7 | Sn | <0,05 | Sr | <0,02 | Th | <0,0005 | Ti | 0,6 |
U | <0,0005 | V | <0,02 | Zn | <0,02 | Zr | <0,05 |
Analyse des Titanmetallpulvers, Werte in ppm. | |||||||||
Al | 2 | B | <0,05 | Ba | 0,5 | Bi | <0,02 | Ca | 0,2 |
Cd | <0,05 | Co | 0,25 | Cr | 0,15 | Cu | 0,06 | Fe | 0,4 |
K | <0,05 | Mg | 3 | Mn | 0,01 | Mo | 0,4 | Na | 0,3 |
Nb | 0,25 | Ni | 0,15 | P | 0,2 | Pb | 0,02 | Sb | <0,05 |
Si | 6,5 | Sn | <0,05 | Sr | <0,02 | Th | <0,000 5 | U | <0,0005 |
V | <0,02 | Zn | <0,02 | Zr | 6 |
Claims (8)
- Verfahren zur Herstellung von hochreinem Metallpulver, dadurch gekennzeichnet, daß die Herstellung durch Reaktion einer oder von mehreren flüchtigen Metallalkoxidverbindungen mit einem Reduktionsgas erfolgt.
- Verfahren gemäß Anspruch 1, dadurch gekennzeichnet, daß als Reduktionsgas Wasserstoff eingesetzt wird.
- Verfahren gemäß einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß das Reduktionsgas mit einem inerten Trägergas aus der Gruppe der Edelgase verdünnt ist.
- Verfahren gemäß Anspruch 3, dadurch gekennzeichnet, daß das Trägergas Argon ist.
- Verfahren gemäß einem oder mehreren der Ansrüche 1 bis 4, dadurch gekennzeichnet, daß das Metallalkoxid ein Alkoxid eines Elementes der Gruppe 3 bis 14 des Periodensystems der Elemente ist.
- Verfahren gemäß einem oder mehreren der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Alkoxidverbindungen bevorzugt Methoxide sind.
- Verfahren gemäß einem oder mehreren der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß die Alkoxidverbindung Wolframmethoxid und/oder Tantalmethoxid sind.
- Verfahren gemäß einem oder mehreren der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß die Reaktion bei einer Temperatur zwischen 400°C und 1400°C, besonders bevorzugt zwischen 600°C und 1200°C, durchgeführt werden.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4404747A DE4404747C2 (de) | 1994-02-15 | 1994-02-15 | Herstellung von Reinstmetallpulver aus Metallalkoxiden |
DE4404747 | 1994-02-15 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0667200A1 EP0667200A1 (de) | 1995-08-16 |
EP0667200B1 true EP0667200B1 (de) | 1998-08-26 |
Family
ID=6510268
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP95101419A Expired - Lifetime EP0667200B1 (de) | 1994-02-15 | 1995-02-02 | Herstellung von Reinstmetallpulver aus Metallalkoxiden |
Country Status (11)
Country | Link |
---|---|
US (1) | US5711783A (de) |
EP (1) | EP0667200B1 (de) |
JP (1) | JPH07252511A (de) |
KR (1) | KR950031331A (de) |
CN (1) | CN1112467A (de) |
AT (1) | ATE170116T1 (de) |
CA (1) | CA2142254A1 (de) |
DE (2) | DE4404747C2 (de) |
IL (1) | IL112620A (de) |
RU (1) | RU2126735C1 (de) |
TW (1) | TW257706B (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10231777A1 (de) * | 2002-07-13 | 2004-02-05 | Diehl Munitionssysteme Gmbh & Co. Kg | Verfahren zur Herstellung eines Wolfram-Basismaterials und Verwendung desselben |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6100415A (en) * | 1998-03-16 | 2000-08-08 | Japan Pionics Co., Ltd. | Purified alkoxide and process for purifying crude alkoxide |
WO2000067936A1 (en) * | 1998-05-06 | 2000-11-16 | H.C. Starck, Inc. | Metal powders produced by the reduction of the oxides with gaseous magnesium |
US5997612A (en) * | 1998-07-24 | 1999-12-07 | The Boc Group, Inc. | Pressure swing adsorption process and apparatus |
US6375704B1 (en) * | 1999-05-12 | 2002-04-23 | Cabot Corporation | High capacitance niobium powders and electrolytic capacitor anodes |
US7187396B2 (en) * | 2003-11-07 | 2007-03-06 | Engelhard Corporation | Low visibility laser marking additive |
AU2005286168B2 (en) | 2004-09-23 | 2012-01-19 | Element Six (Pty) Ltd | Polycrystalline abrasive materials and method of manufacture |
US7399335B2 (en) * | 2005-03-22 | 2008-07-15 | H.C. Starck Inc. | Method of preparing primary refractory metal |
US7758668B1 (en) | 2006-04-18 | 2010-07-20 | Chemnano, Inc. | Process of manufacturing metallic nano-scale powders |
US9856569B2 (en) * | 2012-07-03 | 2018-01-02 | Field Upgrading Limited | Apparatus and method of producing metal in a nasicon electrolytic cell |
CN109396456B (zh) * | 2018-12-28 | 2024-02-13 | 西安赛隆金属材料有限责任公司 | 一种球形钨粉末的制备装置及方法 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3117833A (en) * | 1958-09-25 | 1964-01-14 | Fansteel Metallurgical Corp | Process of purifying and separating columbium and tantalum values from each other |
US3640093A (en) * | 1969-03-10 | 1972-02-08 | Owens Illinois Inc | Process of converting metalorganic compounds and high purity products obtained therefrom |
GB1307581A (en) * | 1970-05-05 | 1973-02-21 | Monsanto Chemicals | Production of alkoxides |
DE3662916D1 (en) * | 1985-03-04 | 1989-05-24 | Toshiba Kk | Methods for preparing high-purity molybdenum or tungsten powder and high-purity oxides powder of the same |
US4582696A (en) * | 1985-04-15 | 1986-04-15 | Ford Motor Company | Method of making a special purity silicon nitride powder |
US4615736A (en) * | 1985-05-01 | 1986-10-07 | Allied Corporation | Preparation of metal powders |
US4755369A (en) * | 1985-05-22 | 1988-07-05 | Research Development Corporation Of Japan | Production of ultrafine particles |
JPS61275108A (ja) * | 1985-05-30 | 1986-12-05 | Mitsubishi Mining & Cement Co Ltd | 誘電体粉末の製造方法 |
JPS63184306A (ja) * | 1986-09-22 | 1988-07-29 | Mitsui Toatsu Chem Inc | 強磁性金属粉末の安定化方法 |
JPH0230706A (ja) * | 1988-07-19 | 1990-02-01 | Central Glass Co Ltd | β−タングステン粉末の製造法 |
-
1994
- 1994-02-15 DE DE4404747A patent/DE4404747C2/de not_active Expired - Fee Related
-
1995
- 1995-01-16 TW TW084100320A patent/TW257706B/zh active
- 1995-02-02 EP EP95101419A patent/EP0667200B1/de not_active Expired - Lifetime
- 1995-02-02 DE DE59503295T patent/DE59503295D1/de not_active Expired - Fee Related
- 1995-02-02 AT AT95101419T patent/ATE170116T1/de not_active IP Right Cessation
- 1995-02-10 JP JP7045098A patent/JPH07252511A/ja active Pending
- 1995-02-10 CA CA002142254A patent/CA2142254A1/en not_active Abandoned
- 1995-02-13 IL IL112620A patent/IL112620A/xx not_active IP Right Cessation
- 1995-02-14 KR KR1019950002665A patent/KR950031331A/ko not_active Application Discontinuation
- 1995-02-15 CN CN95101889A patent/CN1112467A/zh active Pending
- 1995-02-15 RU RU95101844A patent/RU2126735C1/ru active
-
1996
- 1996-07-11 US US08/678,095 patent/US5711783A/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10231777A1 (de) * | 2002-07-13 | 2004-02-05 | Diehl Munitionssysteme Gmbh & Co. Kg | Verfahren zur Herstellung eines Wolfram-Basismaterials und Verwendung desselben |
Also Published As
Publication number | Publication date |
---|---|
IL112620A (en) | 1997-09-30 |
RU2126735C1 (ru) | 1999-02-27 |
EP0667200A1 (de) | 1995-08-16 |
IL112620A0 (en) | 1995-05-26 |
US5711783A (en) | 1998-01-27 |
CA2142254A1 (en) | 1995-08-16 |
RU95101844A (ru) | 1997-03-10 |
KR950031331A (ko) | 1995-12-18 |
TW257706B (de) | 1995-09-21 |
DE4404747A1 (de) | 1995-08-17 |
ATE170116T1 (de) | 1998-09-15 |
CN1112467A (zh) | 1995-11-29 |
JPH07252511A (ja) | 1995-10-03 |
DE4404747C2 (de) | 1995-12-14 |
DE59503295D1 (de) | 1998-10-01 |
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