CN107983963A - A kind of low temperature preparation method of pure W-Cu nanocomposite powder - Google Patents
A kind of low temperature preparation method of pure W-Cu nanocomposite powder Download PDFInfo
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Abstract
A kind of low temperature preparation method of pure nanometer W Cu composite powders, belongs to refractory metal and powder metallurgical technology.Using micron order tungsten powder and nanoscale aluminium powder as raw material, high-energy ball milling is carried out by the way of mechanical alloying, Al is dissolved into W matrixes, prepares W Al composite powders；After NaOH solution corrosion Al, it can obtain nanoporous tungsten powder, it is separately added into the alcoholic solution of copper chloride and the alcoholic solution of oxalic acid, one layer of cupric oxalate is coated in gap and surface, reduced by heating, cupric oxalate resolves into copper and carbon dioxide, and carbon dioxide is removed with the argon gas of circulation, and the copper clad of generation is on the surface of tungsten hole.Since reduction temperature is low, particle growth is very limited, so as to obtain nanometer pure W-Cu composite powder of the particle size in below 50nm.
Description
Technical field
The present invention relates to a kind of preparation method for the W-Cu composite granules that nanoscale is quickly prepared under low temperature, belong to infusibility
Metal and powder metallurgical technology.
Background technology
The binary composite formed with refractory metal W and non-ferrous metal Cu, had both kept refractory metal high-melting-point, high rigidity
Etc. characteristic, but also with performances such as non-ferrous metal heat conduction, conduction, good plasticity；Simultaneously as the thing of refractory metal and non-ferrous metal
Rationality can differ greatly, and infusibility/non-ferrous alloy is produced new special performance.Therefore, infusibility/non-ferrous alloy tool
There are resistance to elevated temperatures, high heat-conductivity conducting rate, low thermal coefficient of expansion, high anti electric arc corrosion and the height that other class alloys hardly match
Temperature is from cooling characteristics etc..Tungsten-copper alloy is from the single electrical contact material as high-voltage appliance switch, to being progressively applied to electric resistance welding
With the electrode material of electric machining, then to fairly large it is used as Electronic Packaging and the heat sink material such as substrate, connector and radiating piece, closely
Development and application is in heat safe space flight, military project material etc. over year.The intrinsic performance advantage that infusibility/non-ferrous alloy has, makes
This kind of material possesses boundless application prospect in a variety of essential industry fields such as space flight, national defence, electronics, machinery.
Refractory metal and the significant physical difference of non-ferrous metal are that fusing point differs greatly, between two kinds of elements intersolubility difference or
It is immiscible, the methods of causing conventional melting and powder metallurgy, it is difficult to meet the preparation requirement of infusibility/non-ferrous alloy.Closely
Domestic scholars develop a variety of ultra-fine and preparation method of the infusibility of nanoscale, non-ferrous metal and its composite powder over year, e.g.,
Mechanical alloying, spray drying and sol-gel etc. prepare ultra-fine, W-Cu nanocomposite powder.Wherein, Mechanical Alloying
Middle long-time ball milling causes impurity content increase in powder, declines the electrical and thermal conductivity performance for finally preparing alloy, and because of ball milling
Powder particle internal flaw density is higher afterwards when causing then to sinter, and quick roughening easily occurs very much for grain structure；Sol-gel process
Can prepare the powder particle that grain size is reduced to tens nanometers, but this method prepare nano particle yield it is relatively low, and be difficult to
Addition other elements prepare multicomponent alloy；The methods of other are as being spray-dried, machinery-heat chemistry synthesis, controls nano particle ruler
Very little and distributing homogeneity difficulty is larger, and applicable material system is limited.
The preparation for the nanometer scale W-Cu composite powders that high-purity, size tunable, constituent element are evenly distributed, is always infusibility gold
One of technical barrier and significant challenge of category and field of powder metallurgy.
The content of the invention
The present invention is the technical barrier prepared for above-mentioned nanometer scale W-Cu composite powders, there is provided under a kind of low temperature
The method for preparing high-purity and uniform particle sizes W-Cu nanocomposite powders so that W-Cu composite powders purity height, size tunable, group
Member is evenly distributed.
The method provided by the invention for preparing W-Cu nanocomposite powder, it is characterised in that comprise the following steps：
(1) using micron order tungsten powder and nanoscale aluminium powder as raw material, according to aluminium：The molar ratio of tungsten is (3~5):1 is matched somebody with somebody
The mass ratio of material, abrading-ball and powder is (20~25):1, abrading-ball is put into ball grinder with powder in vacuum glove box and is carried out
Ball milling, 400~600r/min of rotating speed, Ball-milling Time 20-30h, scrape a wheat-middlings per 5h, avoid cold welding, it is compound to obtain tungsten aluminium
Powder.
(2) tungsten aluminium composite powder that step (1) obtains is added NaOH solution to be corroded, it is preferred to use concentration is
The NaOH solution of 1mol/L corrodes 15~25h, is filtered, during add ethanol and deionized water cleans powder,
1~2h is then dried at 50~70 DEG C in vacuum drying chamber, obtains pure nanoporous tungsten powder；
(3) the porous tungsten powder for obtaining step (2) adds the ethanol solution of copper chloride, and preferably copper chloride concentration is 0.2g/
ML, stirring, makes copper chloride ethanol solution enter in the hole of POROUS TUNGSTEN, after suction filtration in drying box dry 1 at 50~70 DEG C
~2h, then into powder add oxalic acid ethanol solution, preferably oxalic acid solution concentration be 0.3g/mL, stirring 5-10 minutes, make grass
Acid solution and copper chloride reaction generation cupric oxalate, filter, add ethanol cleaning, then the drying at 50~70 DEG C in drying box again
1~2h, obtains W-CuC2O4Composite powder；
(4) W-CuC for obtaining step (3)2O4Composite powder is reduced in the tube furnace of logical argon gas, with 3~6 DEG C/
The speed of min keeps the temperature 1~2h after being heated to 300~400 DEG C from room temperature, furnace cooling, it is 20~50nm's to obtain particle size
Pure W-Cu nanocomposite powder.
The technological process of this method and its principle are：Using micron order tungsten powder and nanoscale aluminium powder as raw material, closed using machinery
The mode of aurification carries out high-energy ball milling, and Al is dissolved into W matrixes, prepares W-Al composite powders, and the solid solubility of Al can be high
Up to 80%；After NaOH solution corrosion Al, the nanoporous tungsten powder that ligament size is 20~30nm is can obtain, is separately added into copper chloride
Ethanol solution and oxalic acid ethanol solution, coat one layer of cupric oxalate on gap and surface, reduced by heating, cupric oxalate decomposes
Into copper and carbon dioxide, carbon dioxide is removed with the argon gas of circulation, and the copper clad of generation is in pore surface.Due to reduction temperature
Low, copper particle growth is very limited, so as to can obtain nanometer tungsten aluminium composite powder of the whole particle size in below 50nm.
The characteristic and technical advantage of this technology are as follows：
Compared with the preparation of traditional tungsten copper powder, the present invention using chemical method can more accurately ensure high-purity and
Nanoscale, and low temperature is quick, method is simple, favorable repeatability.Other methods that tungsten powder is prepared by chemical method at present,
Mainly pass through H2、CH4Or the gas such as Co carries out high temperature reduction, therefore, the tungsten powder obtained by these methods to oxide powder
Particle is thick, and there are considerable risk using above-mentioned reducibility gas.The present invention is compared with these preparation methods, advantage
It is to prepare composite material using the characteristic of nano-porous materials, synthesis temperature substantially reduces, and effectively suppresses particle growth, gives birth to
Into W-Cu composite powder average grain diameter up to less than 50 nanometers, and powder diameter is evenly distributed；When cupric oxalate reaches decomposition
Copper is generated during temperature and carbon dioxide, product are safe, controllable；Tungsten is nano-porous structure, and hole mesoxalic acid copper is formed after decomposing
Copper clad on the surface of tungsten particle, copper is more evenly distributed in tungsten basal body, to subsequently preparing tungsten-copper alloy block material
Material has high compactness and nanostructured, has particularly important guaranteeing role.
Brief description of the drawings
Fig. 1 is the thing phasor of the POROUS TUNGSTEN obtained in example 1；
Fig. 2 is the thing phasor of the W-Cu composite powder obtained in example 1；
Fig. 3 is the microstructure figure of the POROUS TUNGSTEN obtained in example 2；
Fig. 4 is the microstructure figure of the W-Cu composite powder obtained in example 2；
Fig. 5 is the transmission electron microscope picture of the porous tungsten powder obtained in example 3；
Fig. 6 is the transmission electron microscope picture of the W-Cu composite powder obtained in example 3.
Embodiment
Following embodiments further illustrate the present invention, but the present invention is not limited to following embodiments.
Embodiment 1
Using micron order tungsten powder and nanoscale aluminium powder as raw material, according to aluminium：The molar ratio of tungsten is 3:1 carry out dispensing, abrading-ball with
The mass ratio of powder is 22:1, abrading-ball and powder are put into ball grinder in vacuum glove box and carry out ball milling, rotating speed 400r/
Min, Ball-milling Time 25h, scrape a wheat-middlings per 5h, avoid cold welding, obtain tungsten aluminium composite powder.The tungsten aluminium composite powder that will be obtained
End adds the NaOH solution that concentration is 1mol/L and corrodes 15h, is filtered, during add ethanol and deionized water to powder into
Capable cleaning, 1h is then dried in vacuum drying chamber, obtains pure nanoporous tungsten powder, its thing is mutually as shown in Figure 1 at 60 DEG C.
Obtained porous tungsten powder is added to the ethanol solution for the copper chloride that concentration is 0.2g/mL, stirring, enters copper chloride solution porous
In the hole of tungsten, 1h is dried after suction filtration at 60 DEG C in drying box, then the second for the oxalic acid that concentration is 0.3g/mL is added into powder
Alcoholic solution stirs 8 minutes, oxalic acid solution is reacted generation cupric oxalate with copper chloride, filters again, adds ethanol cleaning, then dry
Dry 1h at 60 DEG C, obtains W-CuC in dry case2O4Composite powder.The W-CuC that will be obtained2O4Tubular type of the composite powder in logical argon gas
Reduced in stove, be heated to from room temperature keep the temperature 1h after 350 DEG C with the speed of 5 DEG C/min, furnace cooling, obtain average grain ruler
It is very little be 39 pure W-Cu nanocomposite powder, its thing is mutually as shown in Figure 2.
Embodiment 2
Using micron order tungsten powder and nanoscale aluminium powder as raw material, according to aluminium：The molar ratio of tungsten is 4:1 carry out dispensing, abrading-ball with
The mass ratio of powder is 20:1, abrading-ball and powder are put into ball grinder in vacuum glove box and carry out ball milling, rotating speed 500r/
Min, Ball-milling Time 20h, scrape a wheat-middlings per 5h, avoid cold welding, obtain tungsten aluminium composite powder.The tungsten aluminium composite powder that will be obtained
End adds the NaOH solution that concentration is 1mol/L and corrodes 20h, is filtered, during add ethanol and deionized water to powder into
Capable cleaning, 1h is then dried in vacuum drying chamber, obtains pure nanoporous tungsten powder, its microstructure is such as at 70 DEG C
Shown in Fig. 3.Obtained porous tungsten powder is added to the ethanol solution for the copper chloride that concentration is 0.2g/mL, stirring, makes copper chloride solution
Into in the hole of POROUS TUNGSTEN, 1h is dried after suction filtration at 70 DEG C in drying box, then it is 0.3g/mL's to add concentration into powder
The ethanol solution of oxalic acid stirs 5 minutes, oxalic acid solution is reacted generation cupric oxalate with copper chloride, filters again, it is clear to add ethanol
Wash, then dry 1h at 70 DEG C in drying box, obtain W-CuC2O4Composite powder.The W-CuC that will be obtained2O4Composite powder is logical
Reduced in the tube furnace of argon gas, be heated to from room temperature keep the temperature 2h after 300 DEG C with the speed of 3 DEG C/min, furnace cooling, obtained
Average particle size particle size is the pure W-Cu nanocomposite powder of 43nm, its microstructure is as shown in Figure 4.
Embodiment 3
Using micron order tungsten powder and nanoscale aluminium powder as raw material, according to aluminium：The molar ratio of tungsten is 5:1 carry out dispensing, abrading-ball with
The mass ratio of powder is 25:1, abrading-ball and powder are put into ball grinder in vacuum glove box and carry out ball milling, rotating speed 600r/
Min, Ball-milling Time 30h, scrape a wheat-middlings per 5h, avoid cold welding, obtain tungsten aluminium composite powder.The tungsten aluminium composite powder that will be obtained
End adds the NaOH solution that concentration is 1mol/L and corrodes 25h, is filtered, during add ethanol and deionized water to powder into
Capable cleaning, 2h is then dried in vacuum drying chamber, obtains pure nanoporous tungsten powder, its transmission electron microscope pattern is such as at 50 DEG C
Shown in Fig. 5.Obtained porous tungsten powder is added to the ethanol solution for the copper chloride that concentration is 0.2g/mL, stirring, makes copper chloride solution
Into in the hole of POROUS TUNGSTEN, 2h is dried after suction filtration at 50 DEG C in drying box, then it is 0.3g/mL's to add concentration into powder
The ethanol solution of oxalic acid stirs 10 minutes, oxalic acid solution is reacted generation cupric oxalate with copper chloride, filters again, it is clear to add ethanol
Wash, then dry 2h at 50 DEG C in drying box, obtain W-CuC2O4Composite powder.The W-CuC that will be obtained2O4Composite powder is logical
Reduced in the tube furnace of argon gas, be heated to from room temperature keep the temperature 1h after 400 DEG C with the speed of 6 DEG C/min, furnace cooling, obtained
Average particle size particle size is the pure W-Cu nanocomposite powder of 45nm, its transmission electron microscope pattern is as shown in Figure 6.
Claims (6)
1. a kind of low temperature preparation method of pure W-Cu nanocomposite powder, it is characterised in that comprise the following steps：
(1) using micron order tungsten powder and nanoscale aluminium powder as raw material, according to aluminium：The molar ratio of tungsten is (3~5):1 carries out dispensing, mill
The mass ratio of ball and powder is (20~25):1, abrading-ball and powder are put into ball grinder in vacuum glove box and carry out ball milling,
400~600r/min of rotating speed, Ball-milling Time 20-30h, scrape a wheat-middlings per 5h, avoid cold welding, obtain tungsten aluminium composite powder；
(2) tungsten aluminium composite powder that step (1) obtains is added NaOH solution to be corroded, then filtered, during add second
Alcohol and deionized water clean powder, then dry 1~2h at 50~70 DEG C in vacuum drying chamber, obtain pure receive
Meter Duo Kong tungsten powders；
(3) the porous tungsten powder for obtaining step (2) adds the ethanol solution stirring of copper chloride, enters copper chloride ethanol solution
In the hole of POROUS TUNGSTEN, 1~2h is dried after suction filtration at 50~70 DEG C in drying box, then the ethanol of addition oxalic acid is molten into powder
Liquid, is stirred 5-10 minutes, oxalic acid solution is reacted generation cupric oxalate with copper chloride, is filtered again, adds ethanol cleaning, then dry
Dry 1~2h at 50~70 DEG C, obtains W-CuC in dry case2O4Composite powder；
(4) W-CuC for obtaining step (3)2O4Composite powder is reduced in the tube furnace of logical argon gas, with 3~6 DEG C/min
Speed from room temperature be heated to 300~400 DEG C after keep the temperature 1~2h, furnace cooling, obtains pure W-Cu nanocomposite powder.
A kind of 2. low temperature preparation method of pure W-Cu nanocomposite powder described in accordance with the claim 1, it is characterised in that step
Suddenly (2) use concentration to corrode 15~25h for the NaOH solution of 1mol/L.
A kind of 3. low temperature preparation method of W-Cu nanocomposite powder described in accordance with the claim 1, it is characterised in that copper chloride
Concentration is 0.2g/mL.
A kind of 4. low temperature preparation method of pure W-Cu nanocomposite powder described in accordance with the claim 1, it is characterised in that grass
Acid solutions are 0.3g/mL.
A kind of 5. low temperature preparation method of pure W-Cu nanocomposite powder described in accordance with the claim 1, it is characterised in that W-
The grain size of Cu composite powders is 20~50nm.
A kind of 6. low temperature preparation method of pure W-Cu nanocomposite powder described in accordance with the claim 1, it is characterised in that tungsten
For nano-porous structure, copper clad is on the surface of tungsten particle in hole.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108655392A (en) * | 2018-05-18 | 2018-10-16 | 有研粉末新材料（北京）有限公司 | A kind of preparation method of copper clad chromium composite powder |
| CN113894281A (en) * | 2021-10-12 | 2022-01-07 | 中国科学院福建物质结构研究所 | Titanium-aluminum alloy microsphere with uniform nano-porous structure on surface and preparation method and application thereof |
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| CN113894281A (en) * | 2021-10-12 | 2022-01-07 | 中国科学院福建物质结构研究所 | Titanium-aluminum alloy microsphere with uniform nano-porous structure on surface and preparation method and application thereof |
| CN113894281B (en) * | 2021-10-12 | 2022-10-11 | 中国科学院福建物质结构研究所 | Titanium-aluminum alloy microsphere with uniform nano-porous structure on surface and preparation method and application thereof |
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