CN1371774A - Method for preparing nano metal composite particle - Google Patents
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- CN1371774A CN1371774A CN 01106255 CN01106255A CN1371774A CN 1371774 A CN1371774 A CN 1371774A CN 01106255 CN01106255 CN 01106255 CN 01106255 A CN01106255 A CN 01106255A CN 1371774 A CN1371774 A CN 1371774A
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Abstract
The preparation method of nano metal composite particle includes the following steps: dissolving soluble metal salt and inorganic salt in water, uniformly mixing them to obtain precursor aqueous solution, drying the above-mentioned precursor aqueous solution to obtain precursor or its powder; heating precursor or its powder under the atmosphere of air, oxygen gas, nitrogen gas or their gas mixture; adopting self-spreading pyrogenic decomposition method to remove soluble salt and other ion to obtain intermediate compound powder and making said intermediate compound undergo the process of reduction treatment by means of thermal chemical process in fixed bed or moving bed.
Description
The present invention relates to nano material, specifically a kind of method for preparing nano metal composite particle.
In the prior art, the chemical manufacturing method of nano material has many, as: coprecipitation, hydro-thermal method, Hydrolyze method, micropore liquid method, sol-gel processing, spray-on process, the oxide particle that wherein adopts spray-on process to generate is generally spherical, good fluidity and be easy to handle, thereby obtained using widely at aspects such as inorganic matter preparation, catalyst and ceramic material are synthetic.In spray drying process, metal salt solution sprays in the hot blast, thereby solvent evaporates the nano particle of precipitating metal salt rapidly, and pyrolysis then (both desalination reactions) obtains oxide.At patent US, 5,882,376 hot mechanochemical reaction and US, 5,352,269 spraying transformation approach prepare in the tungsten carbide nanometer powder, at first prepare metal salt solution, the spray-drying salting liquid is to prepare uniform precursor powder, pyrolysis desalination at a certain temperature gets oxidation of precursor thing powder, carries out hydrogen reduction, with carbon or CO/CO
2Three processes of mist carbonization.Patent US, 5,842,108 mechanochemistries prepare in the W/Cu nano powder, adopt the spray-drying salting liquid to prepare uniform precursor powder, back desalination, mechanical mixture and hydrogen reduction.Above desalination temperature is 750 ℃, and 2 hours, in patent JP 4316236 solution legal system W/Cu, desalination temperature was 750～850 ℃, 1 hour.Yet low reaction temperature, the short resolving time can be made the high activity product, helps subsequent processes.So in order to reduce the pyrolysis temperature of salt, people generally select the organic salt system, have increased cost like this; Select for use nitrate can be easy to decompose, but can produce harmful nitrogen oxide.
At present, spray heating decomposition then is that solution is sprayed in the high-temperature atmosphere, and the thermal decomposition of solvent evaporation and slaine is carried out simultaneously, thereby makes the method for oxide nano particles with a procedure.For example with analyzing pure Co (CH
3COO)
24H
2O, Mn (CH
3OO)
24H
2O and Ni (CH
3OO)
24H
2O makes precursor material, after being mixed with solution by a certain percentage, it being sprayed in the quartz ampoule of high temperature heating, is 0.138MPa at atomizer pressure, under the process conditions that pyrolysis temperature is 750 ℃, can obtain average grain diameter is the CoMnNiO multicomponent composite oxide particle of 29nm.But high pyrolysis temperature is had relatively high expectations to equipment, and milling efficiency is imitated low.Also need consider simultaneously the gas problem that is harmful to.
The purpose of this invention is to provide a kind of have low cost, low reaction temperatures, combination property height, the method for preparing nano metal composite particle that no pernicious gas produces.
To achieve these goals, technical scheme of the present invention is to operate as follows:
(1) preparation precursor water solution: soluble metallic salt and the inorganic salts selected are soluble in water, metallic element is evenly mixed on molecular level, make precursor water solution;
(2) drying: with above-mentioned precursor water solution, adopt evaporation or atom atomization drying method to carry out drying and handle, make presoma or precursor powder;
(3) desalination: heating presoma or precursor powder under air, oxygen, nitrogen or described gas mixture atmosphere, adopt from spreading other ion that pyrolysismethod is removed soluble-salt in the described reactant, make intermediate powder; In 250～450 ℃ of temperature ranges, keep 5min～1hr;
(4) reduction: in fixed bed or thermopnore, under flowing gas hydrogen shield atmosphere, intermediate powder is reduced processing, make composite nano-powder or high density nano bulk material by heat chemistry;
Transition metal is tungsten-copper, tungsten-cobalt, tungsten-cobalt-vanadium, tungsten-cobalt-titanium, tungsten-cobalt-tantalum, tungsten-cobalt-chromium, tungsten-nickel, tungsten-copper-nickel in soluble metallic salt of the present invention and the inorganic salts, one of copper aluminium, neodymium iron boron or its combination;
Described dry run will add the organic-fuel of described solution 5～30% in the above-mentioned precursor water solution, adopt evaporation or atom atomization drying method to carry out drying and handle, and makes presoma or precursor powder; Described organic-fuel is amion acetic acid, a urea in citric acid, the amine compound in organic carbonyl;
Described reduction process; in fixed bed or thermopnore, under flowing gas hydrogen shield atmosphere, add the carbon of intermediate powder weight 1～30%; by heat chemistry intermediate powder is reduced processing, make composite nano-powder or high density nano bulk material.
The evaporation that dry run of the present invention adopts is solution to be heated evaporate to dryness take place simultaneously from spreading pyrolytic reaction; The atom atomization drying that adopts is that solution atomization is become superfine drop, the solvent evaporation is made the method for particle then under hot-air, takes place simultaneously from spreading pyrolytic reaction; The present invention will spread pyrolysismethod certainly and prepare the intermediate powder of metal oxide in conjunction with atom atomization drying technology or thermal evaporation, and when atom atomization drying temperature surpassed 300 ℃, then self-propagating reaction took place, and reduces reaction temperature with this.Further, the present invention has more hole and specific area, and this intermediate powder can obtain active very big nano metal powder such as WCu, Cu/Al through hydrogen reduction or carbon thermal reduction
2O
3, WC/Co has good moulding and sintering characteristic.In addition, CO
2And N
2Be nitrate anion in the desalination reaction and organic matter product.
The present invention has following advantage:
1. has low reaction temperatures, the high product combination property.The present invention with they precursor solutions of making soluble in water, makes metallic element evenly mix in the atom magnitude by selecting suitable soluble metallic salt and organic salt then; Solution is made precursor powder or heating evaporation becomes the presoma lotion through the evaporation drying technology.This presoma is being lighted more than 300 ℃, and through spreading the pyrolysis heat release certainly, salt decomposes in the reactant, forms the intermediate powder of metal oxide; Because the present invention compares with the powder of pyrolysismethod formation in the prior art from the intermediate powder that spreads pyrolytic reaction formation, pyrolysis reaction temperature is low, time shortens, the present invention will spread pyrolysismethod prepares metal oxide in conjunction with atom atomization drying technology or thermal evaporation intermediate powder certainly, when atom atomization drying temperature surpasses 300 ℃, then self-propagating reaction takes place, this process and spray heating decomposition are similar, (general temperature is between 250-450 ℃ but temperature is hanged down several Baidu, reaction 5min～1hr, and the prior art temperature is between 750～850 ℃, 1～2 hour); Further, product of the present invention also has more hole and high specific surface area, and this intermediate powder can obtain active very big nano metal powder such as WCu, Cu/Al through hydrogen reduction or carbon thermal reduction
2O
3, WC/Co, and have good moulding and sintering characteristic, the product combination property improves 30%; Only behind the low temperature solid-phase sintering, higher density, the uniform composite of composition can be obtained, 1200 ℃ of sintering 1 hour, density 99.9% above nano block Tungsten-copper Composites can be obtained as the intermediate powder of tungsten copper; And because no activator, heat conduction of the present invention, electric conductivity are all unaffected.
2. the present invention prepares the compound powder process on molecular level of nano metal composite particle method through hydrogen or carbon thermal reduction, can once produce required product, cumbersome procedure such as follow-up mixing have been removed from, technology is simple, composition is even and adjustable, with low cost, use the comparable existing technology of the present invention to reduce by 40% processing charges; In addition, the prepared particle of the present invention can prepare the product of different shape complexity through injection moulding, and the present invention adds micro-grain growth inhibitor such as V, Cr, Ta etc., can make product grains size and other performances controlled.
3. energy-conservation.The present invention forms the combustion reaction system by metal nitrate and organic-fuel, utilizes the effect of exothermic heat of reaction and generation gas to prepare nano-particle material, and is less demanding to equipment, has characteristics of energy saving.
4. environmental.Because nitrate anion and organic matter product are CO in the desalination reaction of the present invention
2And N
2,, have the environmental protection characteristics so the no pernicious gas of reaction produces.
5. applied range.The present invention is with producing the preparation that is applicable to any oxide, make raw material as nano level WCu powder, can produce the electrical contact of good integrated circuit with heat conducting inserts and microelectronic packaging material and anti-galvanic corrosion, and war products, utilize the present invention also can produce the product of high thermal conductance, low thermal coefficient of expansion.
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
(1) preparation precursor water solution: get ammonium metatungstate 70 grams in the metal tungstates, inorganic salts cobalt nitrate 30 grams are dissolved in the 100 gram water, and metallic element is evenly mixed on molecular level, are mixed with the precursor solution that can form WC-10Co;
(2) drying: add 5% in the urea of solution weight in above-mentioned precursor water solution, adopt thermal evaporation that this solution heating is reached 100 ℃, evaporation forms lotion;
(3) desalination: heating presoma lotion under air, oxygen mix atmosphere, insert 300 ℃ of muffle furnaces, 5 minutes, adopt from spreading pyrolysismethod generation combustion reaction, gas is emitted simultaneously, removes other ion of soluble-salt in the reactant, gets W-Co-O composite oxides intermediate powder;
(4) reduction: in fixed bed, under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency is made nano-complex particle product W-Co;
(5) carbonization: in rotary furnace, under the flowing hydrogen gas atmosphere, add 2% carbon of intermediate powder weight, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect C
2Reduction efficiency is made nano-complex particle product WC-Co.
Embodiment 2
(1) preparation precursor water solution: get ammonium metatungstate 70 grams in the metal tungstates, inorganic salts cobalt nitrate and nitric acid vanadium 30 grams are dissolved in the 100 gram water, and metallic element is evenly mixed on molecular level, are mixed with the precursor solution that can form WC-10Co-V;
(2) drying: add 10% in the urea of solution weight in above-mentioned precursor water solution, adopt thermal evaporation that this solution heating is reached 100 ℃, evaporation forms lotion;
(3) desalination: heating presoma lotion under air, oxygen mix atmosphere, insert 320 ℃ of muffle furnaces, 5 minutes, adopt from spreading pyrolysismethod generation combustion reaction, gas is emitted simultaneously, removes other ion of soluble-salt in the reactant, gets W-Co-V-O composite oxides intermediate powder;
(4) reduction: in fixed bed, under the flowing hydrogen gas atmosphere, add the carbon of intermediate powder weight 5%, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect the H2 reduction efficiency, makes nano-complex particle product W-Co-V;
(5) carbonization: in rotary furnace, under the flowing hydrogen gas atmosphere, add 15% carbon of intermediate powder weight, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect C
2Reduction efficiency is made nano-complex particle product WC-Co-V.
Embodiment 3
(1) preparation precursor water solution: get ammonium metatungstate 70 grams in the metal tungstates, inorganic salts cobalt nitrate and nitric acid vanadium 30 grams are dissolved in the 100 gram water, and metallic element is evenly mixed on molecular level, are mixed with the precursor solution that can form WC-10Co-V;
(2) drying: add 30% in the urea of solution weight in above-mentioned precursor water solution, adopt thermal evaporation that this solution heating is reached 100 ℃, evaporation forms lotion;
(3) desalination: heating presoma lotion under air, oxygen mix atmosphere, insert 340 ℃ of muffle furnaces, 5 minutes, adopt from spreading pyrolysismethod generation combustion reaction, gas is emitted simultaneously, removes other ion of soluble-salt in the reactant, gets W-Co-V-O composite oxides intermediate powder;
(4) reduction: in fixed bed, under the flowing hydrogen gas atmosphere, add the carbon of intermediate powder weight 30%, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency is made nano-complex particle product W-Co-V;
(5) carbonization: in rotary furnace, under the flowing hydrogen gas atmosphere, add 30% carbon of intermediate powder weight, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect C
2Reduction efficiency is made nano-complex particle product WC-Co-V.
Embodiment 4
(1) preparation precursor water solution: get ammonium metatungstate 70 grams in the metal tungstates, cobalt nitrate and chloric acid titanium 30 restrain in the inorganic salts, are dissolved in the 100 gram water being mixed with the precursor solution that can form WC-10Co-Ti;
(2) drying: with above solution under flow 20 ml/min, 11000 rev/mins of rotating speeds, 250 ℃ of inlet temperatures, 117 ℃ of situations of outlet temperature, adopt atom atomisation method with solution atomization poling small droplet, under hot-air, solvent is evaporated then, get precursor powder;
(3) desalination: heat precursor powder under air and inert gas argon gas mixed atmosphere, adopt from spreading pyrolysismethod and place 250 ℃ of muffle furnaces, gas is emitted in burning in 15 minutes simultaneously, obtains W-Co-Ti-O composite oxides intermediate powder;
(4) reduction: in thermopnore and under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency is made nano-complex particle product W-Co-Ti.
Embodiment 5
(1) preparation precursor water solution: get ammonium metatungstate 70 grams in the metal tungstates, cobalt nitrate and nitric acid tantalum 30 restrain in the inorganic salts, are dissolved in the 100 gram water being mixed with the precursor solution that can form WC-10Co-Ta;
(2) drying: with above solution under flow 20 ml/min, 11000 rev/mins of rotating speeds, 290 ℃ of inlet temperatures, 117 ℃ of situations of outlet temperature, adopt atom atomisation method with solution atomization poling small droplet, under hot-air, solvent is evaporated then, get precursor powder;
(3) desalination: under air and inert gas argon gas mixed atmosphere, heat precursor powder, adopt from spreading pyrolysismethod and place 750 ℃ of muffle furnaces, 2 hours combustion and pyrolysis (present embodiment is not adding under the urea situation) are emitted gas simultaneously and are obtained W-Co-Ta-O composite oxides intermediate powder;
(4) reduction: in fixed bed and under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency is made nano-complex particle product W-Co-Ta.
Embodiment 6
(1) preparation precursor water solution: get heavy ammonium tungstate 70 grams in the metal tungstates, copper nitrate 30 grams are dissolved in the 100 gram water and are mixed with the precursor solution that can form W-20Cu in the inorganic salts;
(2) drying: in above-mentioned precursor water solution, add 20% in the citric acid of solution weight, adopt thermal evaporation that this solution evaporation, heating are reached 100 ℃, form lotion;
(3) desalination: under oxygen atmosphere, heat the presoma lotion, adopt from spreading pyrolysismethod and insert 400 ℃ of muffle furnaces, 35 minutes, combustion reaction takes place, gas is emitted simultaneously, gets W-Cu-O composite oxides intermediate powder;
(4) reduction: in thermopnore and under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect the H2 reduction efficiency, makes nano-complex particle product W-Cu.
Embodiment 7
(1) preparation precursor water solution: get heavy ammonium tungstate 70 grams in the metal tungstates, copper nitrate and nickel nitrate 30 restrain in the inorganic salts, are dissolved in the 100 gram water being mixed with the precursor solution that can form W-20Cu-Ni;
(2) drying: in precursor solution, add 15% in the amion acetic acid of solution weight, adopt atom atomisation method, under hot-air, the solvent evaporation is formed lotion then with solution atomization poling small droplet;
(3) desalination: under air atmosphere, heat the presoma lotion, adopt from spreading pyrolysismethod and insert 450 ℃ of muffle furnaces, 45 minutes, combustion reaction takes place, gas is emitted simultaneously, gets W-Cu-Ni-O composite oxides intermediate powder;
(4) reduction: under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction in fixed bed, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency generates product W-Cu-Ni.
Embodiment 8
(1) preparation precursor water solution: get metal aluminum nitrate 70 grams, copper nitrate 30 restrains in the inorganic salts, is dissolved in the 100 gram water being mixed with the precursor solution that can form Cu-Al;
(2) drying: in precursor solution, add 20% in the amion acetic acid of solution weight, adopt atom atomisation method, under hot-air, the solvent evaporation is formed lotion then with solution atomization poling small droplet;
(3) desalination: under air atmosphere, heat the presoma lotion, adopt from spreading pyrolysismethod and insert 450 ℃ of muffle furnaces, 45 minutes, combustion reaction takes place, gas is emitted simultaneously, gets Al-Cu-O composite oxides intermediate powder;
(4) reduction: under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction in fixed bed, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency generates products C u-Al
2O
3
Embodiment 9
(1) preparation precursor water solution: get metal metaphosphate ammonium borate and neodymium nitrate 70 grams, ferric nitrate 30 restrains in the inorganic salts, is dissolved in the 100 gram water being mixed with the precursor solution that can form Nd-Fe-B;
(2) drying: in precursor solution, add 25% in the amion acetic acid of solution weight, adopt atom atomisation method, under hot-air, the solvent evaporation is formed lotion then with solution atomization poling small droplet;
(3) desalination: under air atmosphere, heat the presoma lotion, adopt from spreading pyrolysismethod and insert 410 ℃ of muffle furnaces, 45 minutes, combustion reaction takes place, gas is emitted simultaneously, gets Nd-Fe-B composite oxides intermediate powder;
(4) reduction: under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction in fixed bed, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency generates product Nd-Fe-B.
Embodiment 10
(1) preparation precursor water solution: get in the slaine in the copper nitrate 70 gram inorganic salts chromic nitrate 30 grams and be dissolved in the 100 gram water and be mixed with the precursor solution that can form Cu-Cr;
(2) drying: in above-mentioned precursor water solution, add 25% in the citric acid of solution weight, adopt thermal evaporation that this solution evaporation, heating are reached 100 ℃, form lotion;
(3) desalination: under oxygen atmosphere, heat the presoma lotion, adopt from spreading pyrolysismethod and insert 430 ℃ of muffle furnaces, 35 minutes, combustion reaction takes place, gas is emitted simultaneously, gets Cu-Cr-O composite oxides intermediate powder;
(4) reduction: in thermopnore and under the flowing hydrogen gas atmosphere, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency is made nano-complex particle products C u-Cr.
Embodiment 11
(1) preparation precursor water solution: get heavy ammonium tungstate 70 grams in the metal tungstates, nickel nitrate 30 grams are dissolved in the 100 gram water and are mixed with the precursor solution that can form W-20Ni in the inorganic salts;
(2) drying: in above-mentioned precursor water solution, add 6% in the citric acid of solution weight, adopt thermal evaporation that this solution evaporation, heating are reached 100 ℃, form lotion;
(3) desalination: under oxygen atmosphere, heat the presoma lotion, adopt from spreading pyrolysismethod and insert 350 ℃ of muffle furnaces, 35 minutes, combustion reaction takes place, gas is emitted simultaneously, gets W-Ni-O composite oxides intermediate powder;
(4) reduction: in fixed bed and under the flowing hydrogen gas atmosphere, add the carbon of intermediate powder weight 10%, by heat chemistry intermediate powder is carried out reduction reaction, wherein temperature is controlled at 750 ℃, H
2Flow is 200 ml/min, and X-ray relative intensity value is used to detect H
2Reduction efficiency is made nano-complex particle product W-Ni.
Claims (5)
1. method for preparing nano metal composite particle is characterized in that operating as follows:
(1) preparation precursor water solution: soluble metallic salt and the inorganic salts selected are soluble in water, metallic element is evenly mixed on molecular level, make precursor water solution;
(2) drying: with above-mentioned precursor water solution, adopt evaporation or atom atomization drying method to carry out drying and handle, make presoma or precursor powder;
(3) desalination: heating presoma or precursor powder under air, oxygen, nitrogen or described gas mixture atmosphere, adopt from spreading other ion that pyrolysismethod is removed soluble-salt in the described reactant, make intermediate powder; In 250～450 ℃ of temperature ranges, keep 5min～1hr;
(4) reduction: in fixed bed or thermopnore, under flowing gas hydrogen shield atmosphere, intermediate powder is reduced processing, make composite nano-powder or high density nano bulk material by heat chemistry.
2. according to the described method for preparing nano metal composite particle of claim 1, it is characterized in that: transition metal is tungsten-copper, tungsten-cobalt, tungsten-cobalt-vanadium, tungsten-cobalt-titanium, tungsten-cobalt-tantalum, tungsten-cobalt-chromium, tungsten-nickel, tungsten-copper-nickel in described soluble metallic salt and the inorganic salts, one of copper aluminium, neodymium iron boron or its combination.
3. according to the described method for preparing nano metal composite particle of claim 1, it is characterized in that: described dry run, the organic-fuel of described solution weight 5～30% will be added in the above-mentioned precursor water solution, adopt evaporation or atom atomization drying method to carry out drying and handle, make presoma or precursor powder.
4. according to the described method for preparing nano metal composite particle of claim 3, it is characterized in that: described organic-fuel is amion acetic acid, a urea in citric acid, the amine compound in organic carbonyl.
5. according to the described method for preparing nano metal composite particle of claim 1; it is characterized in that: described reduction process; in fixed bed or thermopnore; under flowing gas hydrogen shield atmosphere; the carbon that adds intermediate powder weight 1～30%; by heat chemistry intermediate powder is reduced processing, make composite nano-powder or high density nano bulk material.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031401A (en) * | 2011-01-04 | 2011-04-27 | 合肥工业大学 | Preparation method of nano-alumina reinforcing copper-based composite |
| CN102229496A (en) * | 2011-06-08 | 2011-11-02 | 浙江大学 | SiC/magnetic metal nanometer light composite material prepared from agricultural wastes and method for preparing SiC/magnetic metal nanometer light composite material |
| CN102601378A (en) * | 2011-07-18 | 2012-07-25 | 厦门虹鹭钨钼工业有限公司 | Method for preparing ultrafine tungsten copper composite powder by low-temperature combustion method |
| CN103981381A (en) * | 2014-05-15 | 2014-08-13 | 厦门理工学院 | Method for preparing nano aluminum oxide dispersion enhanced copper-base composite material according to sol-gel method |
| CN104801705A (en) * | 2015-04-24 | 2015-07-29 | 第一拖拉机股份有限公司 | Ultra-fine aluminum oxide and tungsten mixed powder and preparation method thereof |
| CN104874807A (en) * | 2015-06-17 | 2015-09-02 | 北京科技大学 | Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure |
| CN104889415A (en) * | 2015-06-17 | 2015-09-09 | 北京科技大学 | Preparation method of nano nickel powder |
| CN105268983A (en) * | 2015-10-21 | 2016-01-27 | 陕西理工学院 | Preparation method of W-Ni-Cu prealloyed powder |
| CN106670505A (en) * | 2017-01-13 | 2017-05-17 | 昆明理工大学 | Method for preparing tungsten-cobalt-carbon composite powder through spray pyrolysis method |
| CN114941096A (en) * | 2022-05-17 | 2022-08-26 | 西北有色金属研究院 | Tungsten-based alloy suitable for additive manufacturing and preparation method thereof |
-
2001
- 2001-02-28 CN CN 01106255 patent/CN1371774A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031401A (en) * | 2011-01-04 | 2011-04-27 | 合肥工业大学 | Preparation method of nano-alumina reinforcing copper-based composite |
| CN102229496A (en) * | 2011-06-08 | 2011-11-02 | 浙江大学 | SiC/magnetic metal nanometer light composite material prepared from agricultural wastes and method for preparing SiC/magnetic metal nanometer light composite material |
| CN102601378A (en) * | 2011-07-18 | 2012-07-25 | 厦门虹鹭钨钼工业有限公司 | Method for preparing ultrafine tungsten copper composite powder by low-temperature combustion method |
| CN103981381A (en) * | 2014-05-15 | 2014-08-13 | 厦门理工学院 | Method for preparing nano aluminum oxide dispersion enhanced copper-base composite material according to sol-gel method |
| CN104801705A (en) * | 2015-04-24 | 2015-07-29 | 第一拖拉机股份有限公司 | Ultra-fine aluminum oxide and tungsten mixed powder and preparation method thereof |
| CN104874807A (en) * | 2015-06-17 | 2015-09-02 | 北京科技大学 | Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure |
| CN104889415A (en) * | 2015-06-17 | 2015-09-09 | 北京科技大学 | Preparation method of nano nickel powder |
| CN105268983A (en) * | 2015-10-21 | 2016-01-27 | 陕西理工学院 | Preparation method of W-Ni-Cu prealloyed powder |
| CN105268983B (en) * | 2015-10-21 | 2017-09-22 | 陕西理工学院 | The preparation method of W Ni Cu pre-alloyed powders |
| CN106670505A (en) * | 2017-01-13 | 2017-05-17 | 昆明理工大学 | Method for preparing tungsten-cobalt-carbon composite powder through spray pyrolysis method |
| CN114941096A (en) * | 2022-05-17 | 2022-08-26 | 西北有色金属研究院 | Tungsten-based alloy suitable for additive manufacturing and preparation method thereof |
| CN114941096B (en) * | 2022-05-17 | 2022-12-09 | 西北有色金属研究院 | Tungsten-based alloy suitable for additive manufacturing and preparation method thereof |
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