CN107354333A - A kind of preparation method of tungsten-copper composite material - Google Patents
A kind of preparation method of tungsten-copper composite material Download PDFInfo
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- CN107354333A CN107354333A CN201710510327.7A CN201710510327A CN107354333A CN 107354333 A CN107354333 A CN 107354333A CN 201710510327 A CN201710510327 A CN 201710510327A CN 107354333 A CN107354333 A CN 107354333A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- 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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of preparation method of tungsten-copper composite material, belong to powder metallurgical technology.The present invention is first using ammonium tungstate as raw material, with being dried after rice husk and absolute ethyl alcohol mixing and ball milling, dry ball abrasive material is made, isothermal reaction in the gaseous mixture atmosphere formed then at argon gas and hydrogen, through alkali cleaning, wash and dry, porous tungsten powder is made, then by porous tungsten powder and yttrium nitrate solution, copper nitrate solution etc. is stirred, and add precipitating reagent urea, after reaction terminates, concentration, dry and anaerobic is calcined, obtain presoma, gained presoma is reduced in hydrogen atmosphere again, obtain reducing material, reducing material is pressed into green compact in a mold again, and by green compact in hydrogen atmosphere centrifugal burning, chilling while hot again, produce tungsten-copper composite material.The tungsten-copper composite material product consistency that the present invention is prepared is high, conductive and excellent thermal conductivity, better mechanical property.
Description
Technical field
The invention discloses a kind of preparation method of tungsten-copper composite material, belong to powder metallurgical technology.
Background technology
Tungsten has high fusing point, high density, the low coefficient of expansion and high intensity, and copper has good heat conduction, conduction
Property, the advantages of tungsten-copper composite material being made up of tungsten and copper has tungsten and copper concurrently, and can be controlled by changing its proportion of composing
With adjust its each corresponding machinery and physical property, it also has both combinations and caused new capability in addition, as it is in height
It is caused from cooling effect due to the evaporation endothermic of contained copper under the conditions of temperature.Therefore, it be widely used in space flight,
The field of the industrial departments such as electronics, machinery, electrical equipment, particularly some high-tech.
The fusing point of tungsten and copper differs greatly, and the fusing point of tungsten is 3410 DEG C, far above the boiling point of copper, and tungsten and with immiscible,
Therefore tungsten-copper composite material can only use powder metallurgy process to prepare, and the preparation technology of traditional tungsten-copper composite material mainly has infiltration
Method, high-temperature liquid-phase sintering process and activation lqiuid phase sintering method.
At present, infiltration method is that tradition prepares a kind of method being most widely used in tungsten-copper composite material, infiltration method be by
Tungsten powder is pressed into base, and pre-burning at a certain temperature is prepared into the POROUS TUNGSTEN matrix skeleton with certain density and intensity, then will
The relatively low copper fusing of fusing point is penetrated into W skeleton, so as to obtain finer and close tungsten-copper composite material.Its mechanism is mainly in metal
When liquid phase soaks porous matrix, under capillary force action, molten metal flows filling stephanoporate framework hole along particulate interspaces, so as to
Obtain finer and close material.As U.S. R.M.German et al. prepares W skeleton using injection molding technology, through 900 DEG C of pre-burnings,
It is excellent in 1500 DEG C of 90~120min of infiltration, the alloy property being prepared.But use this method very big deficiency to be present, specifically
Show：Due to W skeleton it is difficult to accomplish hole all connections and in the same size, and the product copper distributed mutually after infiltration is uniform
Property it is poor, in addition, material after infiltration needs to be machined out to remove copper-rich epidermis, add follow-up machining expense, drop
Low yield rate, is unfavorable for the processing of the extremely complex parts of shape.
High-temperature liquid-phase sintering process be tungsten powder and copper powder are mixed by a certain percentage, suppressed, liquid-phase sintering and be made tungsten copper answer
The process of condensation material.Traditional method is typically to make its fine and close higher than more than 300 DEG C progress high-temperature liquid-phase sintering of copper fusing point
Change, feature is that production process is simple, but has that sintering temperature is high, sintering time is long, copper largely volatilizees, sintered density is low（Only
90% or so of solid density）The shortcomings of, requirement can not be met.
Activation lqiuid phase sintering method develops on the basis of high-temperature liquid-phase sintering process, by adding in preparation process
Enter micro active element to improve sintering effect.J.L.Johnsom and R.M.German et al. have studied filtering element of Fe,
Ni, Co, Pb compared with high-temperature liquid-phase sintering process, reduce sintering temperature, shorten burning to the activation effect of tungsten-copper composite material
The time is tied, improves sintered density, but the addition of activator reduces the electrical and thermal conductivity performance of material, and this is to electric-conductivity heat-conductivity high
Microelectronic material for be unfavorable.
Therefore, a kind of preparation technology of new tungsten-copper composite material is developed, current traditional handicraft is existing to burn to improve
The problem of junction temperature is high, and sintered density is low, and conductive and heat conductivility is undesirable, make it have higher consistency and excellent comprehensive
Performance is closed, application of the tungsten-copper composite material in fields such as microelectronics information is widened, there is Great significance.
The content of the invention
The present invention solves the technical problem of：After being sintered for the tungsten-copper composite material prepared using traditional handicraft,
Sintered density is low, causes the problem of product is conductive and heat conductivility is undesirable, there is provided a kind of preparation side of tungsten-copper composite material
Method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Count in parts by weight, take 80~100 parts of ammonium tungstates, 10~20 parts of powdered rice hulls, 30~50 parts of absolute ethyl alcohols, ball successively
After 4~6h of mill mixing, dried in baking oven to constant weight, obtain dry ball abrasive material；
（2）Above-mentioned gained dry ball abrasive material is moved into tube furnace, 3~5h of isothermal reaction, treats natural cooling under gaseous mixture atmosphere
To room temperature, successively through alkali liquid washing, washing and vacuum drying, porous tungsten powder is obtained；
（3）Count in parts by weight, it is 3~5% yttrium nitrate solutions to take 10~20 parts of mass fractions successively, 80~100 parts of mass fractions
For 10% copper nitrate solution, 8~10 parts of mass concentrations are 2g/L dopamines, 30~40 parts of porous tungsten powders, add in reactor, stir
Mix after being well mixed, add precipitating reagent, then concentrated, dry and anaerobic calcining, obtain presoma；
（4）Gained presoma is reduced in hydrogen atmosphere, obtains reducing material, then reducing material is pressed into green compact in a mold, and
By green compact in hydrogen atmosphere centrifugal burning, then chilling while hot, produce tungsten-copper composite material.
Step（1）Described powdered rice hulls are that particle diameter is 325~500 mesh powdered rice hulls.
Step（2）The described isothermal reaction condition under gaseous mixture atmosphere is：With 30~60mL/min speed to tube furnace
In be passed through gaseous mixture, in temperature be 600~800 DEG C under the conditions of 3~5h of isothermal reaction；Described gaseous mixture is that argon gas and hydrogen are pressed
Volume ratio is 8：1~10：1 mixes.
Step（2）Described alkali liquid washing is that use quality fraction is that 10~20% sodium hydroxide solutions wash 3~5 times.
Step（3）Described precipitating reagent is that mass fraction is 10% urea liquid；The precipitating reagent dosage is copper nitrate solution
2~3 times of volume.
Step（4）The described reducing condition in hydrogen atmosphere is：In reduction furnace, with 10~30mL/min speed to stove
Hydrogen is inside passed through, reductase 12~4h under the conditions of being 800~850 DEG C in temperature.
Step（4）The described centrifugal burning condition in hydrogen atmosphere is：The mould for filling green compact is placed in hydrogen atmosphere
In, with being 2500~2800N after centrifugal force, sintering temperature sinters 2~3h under the conditions of being 1100~1300 DEG C.
Step（4）The rate of temperature fall control of described chilling while hot is in 80~100 DEG C/s, until being cooled to room temperature.
The beneficial effects of the invention are as follows：
（1）The present invention, with rice husk and absolute ethyl alcohol mixing and ball milling, is covered first using ammonium tungstate as raw material using powdered rice hulls outer surface
Smooth keratinization silica coating, certain lubrication can be played in mechanical milling process, in addition, rice husk in argon gas and
Heated under the conditions of hydrogen atmosphere, generation reducing substances can be decomposed, caused reducibility gas is thermally decomposed with ammonium tungstate oneself
And hydrogen coordinates, and tungsten in system is reduced into simple substance tungsten, while make ammonium tungstate fragmentation and form porous tungsten powder, recycle alkali lye to wash
Removal residual silica is washed, avoids impacting properties of product, it is carrier to recycle porous tungsten powder, and it is improved with dopamine
Absorption property, using urea liquid as precipitating reagent, hydroxide ion caused by hydrolysis of urea and copper ion ruthenium ion in system are slow
With reference to formation Kocide SD and yttrium hydroxide precipitation, the sediment of formation are filled in porous tungsten powder pore structure, reach uniform
Mixing and the purpose of fine and close filling；
（2）The present invention is sintered using centrifugal burning mode to green compact, under the action of the centrifugal force, is advantageous to system sintering
During gas discharge, reduce product porosity, make product consistency improve, in addition, by quenching after sintering, due to cold
But speed block, degree of supercooling is big, improves after processing the second phase content in matrix, and makes the further disperse of precipitated phase, refinement, acquisition
Crystal grain is tiny, the nanocrystalline structure of reduced in segregation, so that product keeps good conduction and heat conductivility, and makes the high temperature of product
Intensity is improved；
（3）The present invention can obviously improve product microscopic structure by adding a small amount of rare-earth substance, a small amount of addition, improves product and burns
Density is tied, suppresses the coalescence between tungsten particle during sintering, while product arc characteristic can be improved, improves product conduct
The performance of microelectronics information material.
Embodiment
To count in parts by weight, take 80~100 parts of ammonium tungstates successively, 10~20 parts of particle diameters are 325~500 mesh powdered rice hulls, 30
~50 parts of absolute ethyl alcohols, are poured into ball grinder, are 10 by ball material mass ratio：1~20：1 adds ball milling pearl, 4~6h of ball milling mixing
Afterwards, discharge, obtain ball milling material, and gained ball milling material is transferred in baking oven, dried under the conditions of being 105~110 DEG C in temperature to constant weight,
Obtain dry ball abrasive material；Gained dry ball abrasive material is moved into tube furnace again, gaseous mixture is passed through into stove with 30~60mL/min speed,
Under gaseous mixture atmosphere, 3~5h of isothermal reaction under the conditions of being 600~800 DEG C in temperature, after naturally cool to room temperature, discharging, obtain
Material is decomposed, then gained is washed for 10~20% sodium hydroxide solutions with mass fraction successively and decomposes material 3~5 times, use deionized water
Washing 3~5 times, then decomposition material after deionized water is washed move into vacuum drying chamber, true under the conditions of being 60~80 DEG C in temperature
Sky dries 6~8h, obtains porous tungsten powder；Count in parts by weight, it is 3~5% yttrium nitrate solutions to take 10~20 parts of mass fractions successively,
80~100 parts of mass fractions are 10% copper nitrate solution, and 8~10 parts of mass concentrations are 2g/L dopamines, 30~40 parts of POROUS TUNGSTENs
Powder, add in reactor, 20~30min is stirred with 300~500r/min rotating speeds, under stirring, to reactor
The middle mass fraction for adding 2~3 times of copper nitrate solution volume is 10% urea liquid, treats that urea liquid adds and finishes, continues to stir
4~6h is reacted, then material in reactor is concentrated in vacuo 30~45min under the conditions of vacuum is 80~90kPa, must be concentrated
Material, then gained concentrate feed is dried in vacuo, composite granule is obtained, and gained composite granule is moved into tube furnace, in argon gas atmosphere,
600~680 DEG C are warming up to, anaerobic calcines 60~90min, after naturally cool to room temperature, obtains presoma；Then by gained presoma
Be transferred to reduction furnace, hydrogen be passed through into stove with 10~30mL/min speed, in temperature be 800~850 DEG C under the conditions of reductase 12~
4h, room temperature is cooled in hydrogen atmosphere, obtains reducing material, and gained reducing material is poured into punching block, with 50~60MPa pressure
Be pressed into green compact, and the punching block for filling green compact be placed in hydrogen atmosphere, in centrifugal force be 2500~2800N, temperature 1100
Under the conditions of~1300 DEG C, 2~3h of centrifugal burning, end to be sintered, while hot to punching block carry out chilling, control rate of temperature fall be 80~
100 DEG C/s, until being cooled to room temperature, it is stripped, produces tungsten-copper composite material.Described gaseous mixture be argon gas and hydrogen by volume
For 8：1~10：1 mixes.
Example 1
Count in parts by weight, take 80 parts of ammonium tungstates successively, 10 parts of particle diameters are 325 mesh powdered rice hulls, 30 parts of absolute ethyl alcohols, pour into ball milling
It is 10 by ball material mass ratio in tank：1 adds ball milling pearl, after ball milling mixing 4h, discharging, obtains ball milling material, and gained ball milling material is turned
Enter in baking oven, dried under the conditions of being 105 DEG C in temperature to constant weight, obtain dry ball abrasive material；Gained dry ball abrasive material is moved into again and managed
Formula stove, gaseous mixture is passed through into stove with 30mL/min speed, under gaseous mixture atmosphere, constant temperature is anti-under the conditions of being 600 DEG C in temperature
3h is answered, after naturally cool to room temperature, discharging, material must be decomposed, then wash institute with mass fraction for 10% sodium hydroxide solution successively
Material must be decomposed 3 times, be washed with deionized 3 times, then the decomposition material after deionized water is washed moves into vacuum drying chamber, in temperature
To be dried in vacuo 8h under the conditions of 60 DEG C, porous tungsten powder is obtained；Count in parts by weight, take 10 parts of mass fractions molten for 3% yttrium nitrate successively
Liquid, 80 parts of mass fractions are 10% copper nitrate solution, and 8 parts of mass concentrations are 2g/L dopamines, 30 parts of porous tungsten powders, add reaction
In kettle, 20min is stirred with 300r/min rotating speeds, under stirring, copper nitrate solution volume 2 is added into reactor
Times mass fraction be 10% urea liquid, treat that urea liquid adds and finish, continuation stirring reaction 4h, then by material in reactor
30min is concentrated in vacuo under the conditions of vacuum is 80kPa, obtains concentrate feed, then gained concentrate feed is dried in vacuo, obtains composite powder
Body, and gained composite granule is moved into tube furnace, in argon gas atmosphere, 600 DEG C are warming up to, anaerobic calcining 60min, treats that nature is cold
But to room temperature, presoma is obtained；Gained presoma is then transferred to reduction furnace, hydrogen is passed through into stove with 10mL/min speed, in
Temperature is reductase 12 h under the conditions of 800 DEG C, and room temperature is cooled in hydrogen atmosphere, obtains reducing material, and gained reducing material is poured into
In punching block, green compact are pressed into 50MPa pressure, and the punching block for filling green compact is placed in hydrogen atmosphere, are in centrifugal force
2500N, under the conditions of temperature is 1100 DEG C, centrifugal burning 2h, end to be sintered, chilling, control cooling speed are carried out to punching block while hot
Rate is 80 DEG C/s, until being cooled to room temperature, is stripped, produces tungsten-copper composite material.Described gaseous mixture is that argon gas and hydrogen press body
Product is than being 8：1 mixes.
Example 2
Count in parts by weight, take 100 parts of ammonium tungstates successively, 20 parts of particle diameters are 500 mesh powdered rice hulls, 50 parts of absolute ethyl alcohols, pour into ball
It is 20 by ball material mass ratio in grinding jar：1 adds ball milling pearl, and after ball milling mixing 6h, discharging obtains ball milling material, and by gained ball milling material
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain dry ball abrasive material；Gained dry ball abrasive material is moved into again
Tube furnace, gaseous mixture is passed through into stove with 60mL/min speed, under gaseous mixture atmosphere, constant temperature under the conditions of being 800 DEG C in temperature
5h is reacted, after naturally cool to room temperature, discharging, material must be decomposed, is then washed successively with mass fraction for 20% sodium hydroxide solution
Gained decomposes material 5 times, is washed with deionized 5 times, then the decomposition material after deionized water is washed moves into vacuum drying chamber, Yu Wen
Spend to be dried in vacuo 8h under the conditions of 80 DEG C, obtain porous tungsten powder；Count in parts by weight, it is 5% yttrium nitrate to take 20 parts of mass fractions successively
Solution, 100 parts of mass fractions are 10% copper nitrate solution, and 10 parts of mass concentrations are 2g/L dopamines, 40 parts of porous tungsten powders, are added
In reactor, 30min is stirred with 500r/min rotating speeds, under stirring, copper nitrate solution is added into reactor
The mass fraction that 3 times of volume is 10% urea liquid, treats that urea liquid adds and finishes, continues stirring reaction 6h, then by reactor
Material is concentrated in vacuo 45min under the conditions of vacuum is 90kPa, obtains concentrate feed, then gained concentrate feed is dried in vacuo, and obtains compound
Powder, and gained composite granule is moved into tube furnace, in argon gas atmosphere, 680 DEG C are warming up to, anaerobic calcining 90min, treats nature
Room temperature is cooled to, obtains presoma；Gained presoma is then transferred to reduction furnace, hydrogen is passed through into stove with 30mL/min speed,
4h is reduced under the conditions of being 850 DEG C in temperature, room temperature is cooled in hydrogen atmosphere, obtains reducing material, and gained reducing material is fallen
Enter in punching block, green compact are pressed into 60MPa pressure, and the punching block for filling green compact is placed in hydrogen atmosphere, be in centrifugal force
2800N, under the conditions of temperature is 1300 DEG C, centrifugal burning 3h, end to be sintered, chilling, control cooling speed are carried out to punching block while hot
Rate is 100 DEG C/s, until being cooled to room temperature, is stripped, produces tungsten-copper composite material.Described gaseous mixture is that argon gas and hydrogen press body
Product is than being 10：1 mixes.
Example 3
Count in parts by weight, take 90 parts of ammonium tungstates successively, 15 parts of particle diameters are 400 mesh powdered rice hulls, 40 parts of absolute ethyl alcohols, pour into ball milling
It is 15 by ball material mass ratio in tank：1 adds ball milling pearl, after ball milling mixing 5h, discharging, obtains ball milling material, and gained ball milling material is turned
Enter in baking oven, dried under the conditions of being 108 DEG C in temperature to constant weight, obtain dry ball abrasive material；Gained dry ball abrasive material is moved into again and managed
Formula stove, gaseous mixture is passed through into stove with 50mL/min speed, under gaseous mixture atmosphere, constant temperature is anti-under the conditions of being 700 DEG C in temperature
4h is answered, after naturally cool to room temperature, discharging, material must be decomposed, then wash institute with mass fraction for 15% sodium hydroxide solution successively
Material must be decomposed 4 times, be washed with deionized 4 times, then the decomposition material after deionized water is washed moves into vacuum drying chamber, in temperature
To be dried in vacuo 7h under the conditions of 70 DEG C, porous tungsten powder is obtained；Count in parts by weight, take 15 parts of mass fractions molten for 4% yttrium nitrate successively
Liquid, 90 parts of mass fractions are 10% copper nitrate solution, and 9 parts of mass concentrations are 2g/L dopamines, 35 parts of porous tungsten powders, add reaction
In kettle, 25min is stirred with 400r/min rotating speeds, under stirring, copper nitrate solution volume is added into reactor
2.5 times of mass fraction is 10% urea liquid, treats that urea liquid adds and finishes, continues stirring reaction 5h, then by thing in reactor
Expect to be concentrated in vacuo 40min under the conditions of vacuum is 85kPa, obtain concentrate feed, then gained concentrate feed is dried in vacuo, obtain composite powder
Body, and gained composite granule is moved into tube furnace, in argon gas atmosphere, 660 DEG C are warming up to, anaerobic calcining 80min, treats that nature is cold
But to room temperature, presoma is obtained；Gained presoma is then transferred to reduction furnace, hydrogen is passed through into stove with 20mL/min speed, in
Temperature reduces 3h under the conditions of being 820 DEG C, and room temperature is cooled in hydrogen atmosphere, obtains reducing material, and gained reducing material is poured into
In punching block, green compact are pressed into 55MPa pressure, and the punching block for filling green compact is placed in hydrogen atmosphere, are in centrifugal force
2600N, under the conditions of temperature is 1200 DEG C, centrifugal burning 3h, end to be sintered, chilling, control cooling speed are carried out to punching block while hot
Rate is 90 DEG C/s, until being cooled to room temperature, is stripped, produces tungsten-copper composite material.Described gaseous mixture is that argon gas and hydrogen press body
Product is than being 9：1 mixes.
Example 4（Comparative example）
W skeleton is prepared using injection molding technology, through 900 DEG C of pre-burnings, under the conditions of 1500 DEG C, using copper liquid infiltration 120min,
Copper-rich epidermis is removed with machining again, produces tungsten-copper composite material.
The products obtained therefrom of example 1 to 4 is subjected to performance detection, specific detection method is as described below：
Product density is determined using Archimedes principle, and calculates its relative density；
Product conductance is determined using direct current four-terminal method；
Product thermal conductivity is measured using LTC-1000 types laser conductometer；
Product bending strength and Vickers hardness are determined using omnipotent sample machine and micro-vickers hardness tester respectively.
Specific testing result is as shown in table 1：
Table 1
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Relative density（%） | 99.78 | 99.79 | 99.72 | 95.5 |
| Conductance（%IACS） | 45 | 46 | 41 | 35 |
| Thermal conductivity（W/（m·K）） | 196 | 198 | 192 | 178 |
| Bending strength（MPa） | 1042 | 1048 | 1040 | 1008 |
| Vickers hardness（HV） | 322 | 324 | 320 | 296 |
Data are detected from table 1, the tungsten-copper composite material product consistency that the present invention is prepared is high, conductive and heat conductivility
It is excellent, better mechanical property.
Claims (8)
1. a kind of preparation method of tungsten-copper composite material, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, take 80~100 parts of ammonium tungstates, 10~20 parts of powdered rice hulls, 30~50 parts of absolute ethyl alcohols, ball successively
After 4~6h of mill mixing, dried in baking oven to constant weight, obtain dry ball abrasive material；
（2）Above-mentioned gained dry ball abrasive material is moved into tube furnace, 3~5h of isothermal reaction, treats natural cooling under gaseous mixture atmosphere
To room temperature, successively through alkali liquid washing, washing and vacuum drying, porous tungsten powder is obtained；
（3）Count in parts by weight, it is 3~5% yttrium nitrate solutions to take 10~20 parts of mass fractions successively, 80~100 parts of mass fractions
For 10% copper nitrate solution, 8~10 parts of mass concentrations are 2g/L dopamines, 30~40 parts of porous tungsten powders, add in reactor, stir
Mix after being well mixed, add precipitating reagent, then concentrated, dry and anaerobic calcining, obtain presoma；
（4）Gained presoma is reduced in hydrogen atmosphere, obtains reducing material, then reducing material is pressed into green compact in a mold, and
By green compact in hydrogen atmosphere centrifugal burning, then chilling while hot, produce tungsten-copper composite material.
A kind of 2. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（1）Described
Powdered rice hulls are that particle diameter is 325~500 mesh powdered rice hulls.
A kind of 3. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（2）Described
Isothermal reaction condition is under gaseous mixture atmosphere：Gaseous mixture is passed through into tube furnace with 30~60mL/min speed, is in temperature
3~5h of isothermal reaction under the conditions of 600~800 DEG C；Described gaseous mixture is that argon gas and hydrogen are 8 by volume：1~10：1 mixing
Form.
A kind of 4. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（2）Described
Alkali liquid washing is that use quality fraction is that 10~20% sodium hydroxide solutions wash 3~5 times.
A kind of 5. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（3）Described
Precipitating reagent is that mass fraction is 10% urea liquid；The precipitating reagent dosage is 2~3 times of copper nitrate solution volume.
A kind of 6. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（4）Described
Reducing condition is in hydrogen atmosphere：In reduction furnace, hydrogen is passed through into stove with 10~30mL/min speed, is in temperature
Reductase 12~4h under the conditions of 800~850 DEG C.
A kind of 7. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（4）Described
Centrifugal burning condition is in hydrogen atmosphere：The mould for filling green compact is placed in hydrogen atmosphere, is 2500 with after centrifugal force
~2800N, sintering temperature sinter 2~3h under the conditions of being 1100~1300 DEG C.
A kind of 8. preparation method of tungsten-copper composite material according to claim 1, it is characterised in that：Step（4）Described
The rate of temperature fall control of chilling is in 80~100 DEG C/s while hot, until being cooled to room temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110014163A (en) * | 2019-04-19 | 2019-07-16 | 广东省材料与加工研究所 | Tungsten alloy powder and its preparation method and application |
| CN113414399A (en) * | 2021-06-02 | 2021-09-21 | 河南科技大学 | Tungsten-copper powder with high copper content and preparation method thereof |
| CN115229189A (en) * | 2022-06-27 | 2022-10-25 | 北京科技大学 | Preparation method of uniform porous tungsten product |
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