CN103194629A - Method for preparing tungsten molybdenum copper composite material - Google Patents
Method for preparing tungsten molybdenum copper composite material Download PDFInfo
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- CN103194629A CN103194629A CN201310098234XA CN201310098234A CN103194629A CN 103194629 A CN103194629 A CN 103194629A CN 201310098234X A CN201310098234X A CN 201310098234XA CN 201310098234 A CN201310098234 A CN 201310098234A CN 103194629 A CN103194629 A CN 103194629A
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Abstract
The invention discloses a method for preparing a tungsten molybdenum copper composite material. The method comprises the steps of 1, ball grinding to obtain tungsten molybdenum mixed powder after screening tungsten powder and molybdenum powder; 2, pressing the tungsten molybdenum mixed powder into a tungsten molybdenum billet; 3, putting the tungsten molybdenum billet on a heating furnace to prepare a tungsten molybdenum skeleton; 4, putting a silicon nitride crucible with an oxygen-free copper plate into the heating furnace, and putting the tungsten molybdenum skeleton above the silicon nitride crucible by a silicon nitride hanging scaffold, heating under a vacuum condition, and then feeding to copper solution to infiltrate; and 5, closing vacuum, and charging argon to the heating furnace, lifting the silicon nitride hanging scaffold to separate from the copper solution, cooling and discharging after cooling to obtain the tungsten molybdenum copper composite material. By adopting the method disclosed by the invention, the machining procedure is saved; the material is saved; the technology is simplified; the method is easy to implement; the tungsten molybdenum copper composite material prepared by the method is low in content of impurity elements such as C, O, Fe and Ni, and high in compactness; and the relative density can be up to over 99.2%.
Description
Technical field
The invention belongs to the Composite Preparation technical field, be specifically related to a kind of preparation method of tungsten carbon/carbon-copper composite material.
Background technology
Tungsten copper " alloy ", molybdenum copper " alloy " are because tungsten, molybdenum and copper are difficult to form alloying truly and are referred to as " pseudoalloy " usually, and its essence is the matrix material that two-phase or a few phase metal are formed.Usually tungsten, molybdenum with its fusing point height, hot strength height, ablation resistance is good and thermal expansivity is low and as the base material of matrix material, copper is then good and as the compound phase of matrix material with its heat conduction, conductivity excellence and plasticity.
At present, the preparation method of tungsten copper, composite material of molybdenum and copper mainly contains infiltration method, powder metallurgic method.Infiltration method utilizes tungsten powder, molybdenum powder compacting sintering to prepare the W skeleton of certain porosity, molybdenum skeleton, utilize electrolytic copper powder to be pressed into copper coin then or directly utilize the fine copper plate to carry out liquid-phase infiltrating (Xue Xiang, Li Song, .W-Cu composite study such as Qiu Ruliang progress. the material Leader, 2008,22(X): 294～298; Han Shengli, Song Yueqing, Cui Shun waits the R and D of .Mo-Cu alloy to make progress. powder metallurgy industry, 2007,17(5): 40～45).The shortcoming of infiltration method is still must carry out mechanical process behind tungsten copper, the molybdenum infiltration of copper to remove unnecessary copper, and it is restricted that the densification difference of its product also makes it be extensive use of, and also do not appear in the newspapers simultaneously and utilize infiltration method to prepare the documents and materials of tungsten carbon/carbon-copper composite material.
Powder metallurgic method is namely prepared tungsten copper, molybdenum copper or tungsten copper composite powder, compression moulding then, liquid phase sintering are fine and close and carry out follow-up densification or processing treatment (V.I.Nizhenko, V.Ya.Petrishchev, and V.V.Shorokhod.Effect of Liquid Phase on the Densification of Tungsten-Copper and Molybdenum-Copper Pseudoalloys in Singtering.Powder Metallurgy and Metal Ceramics, 2008, Vol.47, NOS.3-4).There is the investigator to make precursor solution with ammonium metawolframate and cupric nitrate, drying makes precursor powder, calcine then, hydrogen reduction makes W-Cu composite powder (Su Weifeng, Xiong Ning, Zhou Wuping etc. a kind of novel process for preparing the W-Cu matrix material. Materials Science and Engineering of Powder Metallurgy, 2007,12 (6): 369～373).There is research directly to utilize oxide powder coreduction under hydrogen atmosphere of tungsten, molybdenum and copper to prepare tungsten copper, molybdenum cuprum composite powder (Li Zaiyuan, Zhai Yuchun, Tian Yanwen, etc. the hydrogen reduction of tungsten copper compound prepares class composite W-Cu powder research. the material Leader, 2004,18(1): 95～99).Also have the research and utilization sol-gel method prepare tungsten copper, molybdenum cuprum composite powder (Zhao Ming, Wang Jinshu, the sol-gel preparation of .WCu composite granules such as Liu Wei and reduction act research thereof. Rare Metals Materials and engineering, 2011,2:362-366; The high English that accounts for, Chen Wenge, fourth is held political power. and sol-gel method prepares nanometer MoCu composite granule. Rare Metals Materials and engineering, 2005,34 (6): 990～993).High-energy ball milling machinery alloying (MA) legal system is equipped with tungsten copper in addition, the molybdenum copper powder also once was widely studied (Li Yunping, Qu Xuanhui, Zheng Zhoushun etc. thermomechanometry prepares ultra-fine disperse distribution W-Cu composite powder. powder metallurgy technology, 2004,22(5): 266～269; Zhou Xianliang is full of the sea, Hua Xiaozhen etc. and mechanical alloying is to the influence of Mo-Cu alloy property. powder metallurgy technology, 2007,25(1): 21～23).In above-mentioned preparation tungsten copper, the molybdenum cuprum composite powder material method, utilize the method for presoma calcining reduction to introduce chemical method, its advantage is can be with mixed powder disperse refinement, might improve the homogeneity of tungsten copper, molybdenum copper sintered compact, but prolonged the composite material preparation process flow process, increase uncontrollable factor, also do not seen the report of extensive application as yet.Oxide compound hydrogen co-reducing process since during the oxide compound reduction of tungsten, molybdenum, copper reduction temperature differ factors such as big, thermodynamics factor complexity, atmosphere be wayward and cause reducing process complicated, the composite granule character instability of this method preparation simultaneously causes defectives such as the microtexture of tungsten copper, molybdenum copper of following liquid-phase sintering is inhomogeneous more as powder size skewness, plasticity difference etc.Sol-gel method still is in the R and D of laboratory stage, and industrial applications is still waiting further investigation.The expectation of high-energy ball milling machinery alloying (MA) method utilizes collision energy in the high-energy ball milling process with tungsten powder, molybdenum powder and copper powder carry out cold welding, or glutinous company such as friction welding forms the mechanical alloying powder, or with tungsten powder, molybdenum powder, copper powder is milled to ultra-fine or Nano grade, but because the ball milling tank body in the high-energy ball milling process, abrading-ball or agitator arm are used stainless steel usually, materials such as zirconium white or other alloy, inevitably with Fe, Ni, Zr, impurity such as Si are brought in the mixed powder, significantly worsen the heat conduction of the finished product, performances such as conduction, simultaneously for the ultra-fine size of pursuing mixed powder for a long time ball milling powder O content is sharply increased, and can make that mixed powder is glutinous to be connected on the wall of ball milling chamber, or glutinous be connected on the abrading-ball and easily collecting not.The tungsten copper of powder metallurgic method preparation, molybdenum copper powder are after overmolding in general, and the density that liquid phase sintering can acquire a certain degree, its advantage are only to need less processing or need not carry out machining, thereby have improved the utilization ratio of material.But because the wetting angle of tungsten, molybdenum and copper is little, tungsten copper, molybdenum copper and tungsten copper sintered compact internal void are difficult to discharge fully, and sintered compact is difficult to complete densification.The preparation method of above-mentioned these tungsten coppers, molybdenum copper, tungsten carbon/carbon-copper composite material is in the laboratory development mostly at present, all a large amount of production and application of prematurity.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of tungsten carbon/carbon-copper composite material at above-mentioned the deficiencies in the prior art.This method has been saved the machining program, has saved material, has been simplified technology and easy to implement, the ratio that employing handle to obtain tungsten powder and the Fisher particle size of molybdenum powder through screening is that 1: 2 powder is raw material, tungsten powder, molybdenum powder have been eliminated because difference of specific gravity causes the problem of batch mixing inequality, compare with common batch mixing, can reduce C in the powder, O content thereby significantly reduce mixing time; Pre-burning skeleton step adopts the sintering method of first vacuum, back hydrogen atmosphere, thereby the hole that is conducive to molybdenum skeleton formation perforation is beneficial to follow-up infiltration processing; Adopt vacuum atmosphere in the vacuum infiltration stage, the pre-burning skeleton is immersed in the liquid phase copper, be conducive to liquid phase copper and fully spread in the molybdenum hole, prepared tungsten carbon/carbon-copper composite material has higher compactness, and density is up to more than 99.2%.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of tungsten carbon/carbon-copper composite material is characterized in that this method may further comprise the steps:
Step 2, the mixed powder of tungsten described in the step 1 is pressed into the tungsten biscuit;
Step 3, the biscuit of tungsten described in the step 2 is placed on the smooth silicon nitride hanging scaffold, together place in the process furnace then, be incubated 60min～240min after under vacuum condition, being warming up to 800 ℃～1600 ℃ with the temperature rise rate of 10 ℃/min～30 ℃/min, then close vacuum, in process furnace, charge into hydrogen, continue insulation 60min～240min, last furnace cooling obtains the tungsten skeleton;
Step 4, the silicon nitride crucible that will be placed with no-oxygen copper plate place in the process furnace, and adopt the silicon nitride hanging scaffold that the skeleton of tungsten described in the step 3 is placed directly over the silicon nitride crucible, under vacuum condition with the temperature rise rate of 10 ℃/min～30 ℃/min with stove in temperature rise to 1100 ℃～1400 ℃, to be arranged in tungsten skeleton on the silicon nitride hanging scaffold then and send into copper liquid with the fall off rate of 1mm/min～2mm/min and infiltrate, the infiltration time is 20min～120min;
Step 5, treat described in the step 4 that infiltration is finished after, close vacuum, in process furnace, charge into argon gas, promoting the silicon nitride hanging scaffold makes it separate with copper liquid, then process furnace is down to below 1000 ℃ with the rate of temperature fall of 15 ℃/min～30 ℃/min, naturally cool to discharging after the room temperature at last, obtain the tungsten carbon/carbon-copper composite material.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the material of ball grinder described in the step 1 are molybdenum.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, ball milling described in the step 1 mixes employing molybdenum abrading-ball, and ratio of grinding media to material is 1: 1.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the height of spacing pressing mode restriction tungsten biscuit is adopted in compacting described in the step 2.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the pressure of suppressing described in the step 2 is 150MPa～200MPa, the press time is 5s～8s.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the porosity of the biscuit of tungsten described in the step 2 is 35%～45%.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the flow of hydrogen described in the step 3 is 0.2m
3/ h～0.4m
3/ h, the amount of charging into of hydrogen is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the flow 0.2m of argon gas described in the step 5
3/ h～0.4m
3/ h, the amount of charging into of argon gas is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
The preparation method of above-mentioned a kind of tungsten carbon/carbon-copper composite material, the quality percentage composition of tungsten is 10%～60% in the carbon/carbon-copper composite material of tungsten described in the step 5, and the quality percentage composition of molybdenum is 20%～50%, and the quality percentage composition of copper is 20%～40%.
The present invention compared with prior art has the following advantages:
1, tungsten copper content of the present invention can be adjusted within the specific limits, and wherein W content is 10%～60%, and molybdenum content is 20%～50%, and copper content is 20%～40%.
2, the present invention handles through screening and obtains the tungsten powder Fisher particle size: the molybdenum powder Fisher particle size is 1: 2 powder, tungsten powder, molybdenum powder have been eliminated because difference of specific gravity causes the uneven problem of batch mixing, compare with common batch mixing, can reduce C in the powder, O content thereby significantly reduce mixing time; In mixed powder process, adopt molybdenum batch can processed and abrading-ball, with the common stainless steel batch can of using, the method of material such as zirconium white, wolfram varbide abrading-ball is compared, can not increase and mix in the powder process because the impurity such as Fe, Ni that tank body and abrading-ball abrasive action are brought, C, O in the tungsten carbon/carbon-copper composite material of preparation, impurity contents such as Fe, Ni are low.
3, pre-burning skeleton step of the present invention adopts the sintering method of first vacuum, back hydrogen atmosphere, thereby the hole that is conducive to molybdenum skeleton formation perforation is beneficial to follow-up infiltration processing.
4, the present invention adopts vacuum atmosphere in the vacuum infiltration stage, the pre-burning skeleton is immersed in the liquid phase copper, being conducive to liquid phase copper fully spreads in the molybdenum hole, prepared tungsten carbon/carbon-copper composite material has higher compactness, relative density is up to more than 99.2%, utilize silicon nitride crucible to substitute traditional plumbago crucible simultaneously, can eliminate molybdenum at the carbonization phenomenon in infiltration stage, guaranteed that the thing of tungsten carbon/carbon-copper composite material is stable mutually.
5, the present invention separates the tungsten carbon/carbon-copper composite material after infiltration is finished with liquid phase copper, utilize argon gas atmosphere to cool off fast, suppressed the volatilization of copper phase in the tungsten carbon/carbon-copper composite material of infiltration back, also need machining to go the method for copper to compare with traditional tungsten copper, molybdenum infiltration of copper are follow-up, saved the machining program, saved material, simplified technology and easy to implement.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the SEM photo of the W60Mo20Cu20 matrix material nature fracture of the embodiment of the invention 1 preparation.
Fig. 2 is the SEM photo of the W30Mo40Cu30 matrix material nature fracture of the embodiment of the invention 2 preparations.
Fig. 3 is the SEM photo of the W10Mo50Cu40 matrix material nature fracture of the embodiment of the invention 3 preparations.
Embodiment
The preparation of W60Mo20Cu20 matrix material
Step 2, take by weighing tungsten mixed powder described in the 1100g step 1, the length and width of packing into is respectively in the die cavity of 50mm, 100mm, adopts oil press to carry out spacing compacting, and maximum height limit is 20mm, obtains porosity and be 20 * 50 * 100mm tungsten biscuit of 35%; The pressure of described compacting is 200MPa, and the press time is 5s;
Step 3, the biscuit of tungsten described in the step 2 is placed on the smooth silicon nitride hanging scaffold, together place in the process furnace then, be evacuated to 0.02Pa, be incubated 60min after being warming up to 1600 ℃ with the temperature rise rate of 30 ℃/min, then close the vacuum unit, in process furnace, charge into hydrogen, continue insulation 60min, last furnace cooling obtains the tungsten skeleton; The flow of described hydrogen is 0.2m
3/ h, the amount of charging into of hydrogen is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa;
Step 4, the silicon nitride crucible that will be placed with no-oxygen copper plate place in the process furnace, and adopt the silicon nitride hanging scaffold that the skeleton of tungsten described in the step 3 is placed directly over the silicon nitride crucible, be evacuated to that the temperature rise rate with 30 ℃/min rises to 1200 ℃ with temperature in the stove behind the 0.02Pa, to be arranged in tungsten skeleton on the silicon nitride hanging scaffold then and send into copper liquid with the fall off rate of 1mm/min and infiltrate, the infiltration time is 20min;
Step 5, treat described in the step 4 that infiltration is finished after, close the vacuum unit, in process furnace, charge into argon gas, promoting the silicon nitride hanging scaffold makes it separate with copper liquid, then furnace temperature of heating furnace is down to below 1000 ℃ with the rate of temperature fall of 30 ℃/min, naturally cool to discharging after the room temperature at last, obtain the tungsten carbon/carbon-copper composite material; The flow 0.2m of described argon gas
3/ h, the amount of charging into of argon gas is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
After testing, in the present embodiment in the prepared tungsten carbon/carbon-copper composite material W content be 59wt%, molybdenum content is 20wt%, copper content is 21wt%, relative density is 99.3%.Fig. 1 is the SEM photo of the W60Mo20Cu20 matrix material nature fracture of present embodiment preparation.As can be seen from Figure 1, W, Mo evenly distribute mutually in the W60Mo20Cu20 matrix material, and with W, Mo particle parcel, residual porosity is few with latticed for Cu.
Embodiment 2
The preparation of W30Mo40Cu30 matrix material
Step 2, take by weighing tungsten mixed powder described in the 1250g step 1, the length and width of packing into is respectively in the die cavity of 50mm, 100mm, adopts oil press to carry out spacing compacting, and maximum height limit is 30mm, obtains porosity and be 30 * 50 * 100mm tungsten biscuit of 41%; The pressure of described compacting is 180MPa, and the press time is 6s;
Step 3, the biscuit of tungsten described in the step 2 is placed on the smooth silicon nitride hanging scaffold, together place in the process furnace then, be evacuated to 0.02Pa, be incubated 120min after being warming up to 1200 ℃ with the temperature rise rate of 15 ℃/min, then close the vacuum unit, in process furnace, charge into hydrogen, continue insulation 120min, last furnace cooling obtains the tungsten skeleton; The flow of described hydrogen is 0.3m
3/ h, the amount of charging into of hydrogen is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa;
Step 4, the silicon nitride crucible that will be placed with no-oxygen copper plate place in the process furnace, and adopt the silicon nitride hanging scaffold that the skeleton of tungsten described in the step 3 is placed directly over the silicon nitride crucible, be evacuated to that the temperature rise rate with 15 ℃/min rises to 1100 ℃ with temperature in the stove behind the 0.02Pa, to be arranged in tungsten skeleton on the silicon nitride hanging scaffold then and send into copper liquid with the fall off rate of 1.5mm/min and infiltrate, the infiltration time is 60min;
Step 5, treat described in the step 4 that infiltration is finished after, close the vacuum unit, in process furnace, charge into argon gas, promoting the silicon nitride hanging scaffold makes it separate with copper liquid, then furnace temperature of heating furnace is down to below 1000 ℃ with the rate of temperature fall of 15 ℃/min, naturally cool to discharging after the room temperature at last, obtain the tungsten carbon/carbon-copper composite material; The flow 0.3m of described argon gas
3/ h, the amount of charging into of argon gas is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
After testing, in the present embodiment in the prepared tungsten carbon/carbon-copper composite material W content be 30.5wt%, molybdenum content is 41wt%, copper content is 28.5wt%, relative density is 99.2%.Fig. 2 is the SEM photo of the W30Mo40Cu30 matrix material nature fracture of present embodiment preparation.As can be seen from Figure 2, W, Mo evenly distribute mutually in the W30Mo40Cu30 matrix material, and with W, Mo particle parcel, residual porosity is few with latticed for Cu.
Embodiment 3
The preparation of W10Mo50Cu40 matrix material
Step 2, take by weighing tungsten mixed powder described in the 1250g step 1, the length and width of packing into is respectively in the die cavity of 50mm, 100mm, adopts oil press to carry out spacing compacting, and maximum height limit is 40mm, obtains porosity and be 40 * 50 * 100mm tungsten biscuit of 45%; The pressure of described compacting is 150MPa, and the press time is 8s;
Step 3, the biscuit of tungsten described in the step 2 is placed on the smooth silicon nitride hanging scaffold, together place in the process furnace then, be evacuated to 0.02Pa, be incubated 240min after being warming up to 800 ℃ with the temperature rise rate of 10 ℃/min, then close the vacuum unit, in process furnace, charge into hydrogen, continue insulation 240min, last furnace cooling obtains the tungsten skeleton; The flow of described hydrogen is 0.4m
3/ h, the amount of charging into of hydrogen is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa;
Step 4, the silicon nitride crucible that will be placed with no-oxygen copper plate place in the process furnace, and adopt the silicon nitride hanging scaffold that the skeleton of tungsten described in the step 3 is placed directly over the silicon nitride crucible, be evacuated to that the temperature rise rate with 10 ℃/min rises to 1400 ℃ with temperature in the stove behind the 0.02Pa, to be arranged in tungsten skeleton on the silicon nitride hanging scaffold then and send into copper liquid with the fall off rate of 2mm/min and infiltrate, the infiltration time is 120min;
Step 5, treat described in the step 4 that infiltration is finished after, close the vacuum unit, in process furnace, charge into argon gas, promoting the silicon nitride hanging scaffold makes it separate with copper liquid, then furnace temperature of heating furnace is down to below 1000 ℃ with the rate of temperature fall of 20 ℃/min, naturally cool to discharging after the room temperature at last, obtain the tungsten carbon/carbon-copper composite material; The flow 0.4m of described argon gas
3/ h, the amount of charging into of argon gas is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
After testing, in the present embodiment in the prepared tungsten carbon/carbon-copper composite material W content be 10wt%, molybdenum content is 50.3wt%, copper content is 39.7wt%, relative density is 99.5%.Fig. 3 is the SEM photo of the W10Mo50Cu40 matrix material nature fracture of present embodiment preparation.As can be seen from Figure 3, W, Mo evenly distribute mutually in the W10Mo50Cu40 matrix material, and with W, Mo particle parcel, residual porosity is few with latticed for Cu.
The above; it only is preferred embodiment of the present invention; be not that the present invention is done any restriction, every any simple modification, change and equivalent structure of above embodiment being done according to the invention technical spirit changes, and all still belongs in the protection domain of technical solution of the present invention.
Claims (9)
1. the preparation method of a tungsten carbon/carbon-copper composite material is characterized in that, this method may further comprise the steps:
Step 1, tungsten powder and molybdenum powder are sieved processing respectively, will sieve then obtain after handling tungsten powder and molybdenum powder add in the ball grinder, obtain the tungsten mixed powder behind ball milling mixing 60min～240min; The ratio of the tungsten powder that screening obtains after handling and the Fisher particle size of molybdenum powder is 1: 2;
Step 2, the mixed powder of tungsten described in the step 1 is pressed into the tungsten biscuit;
Step 3, the biscuit of tungsten described in the step 2 is placed on the smooth silicon nitride hanging scaffold, together place in the process furnace then, be incubated 60min～240min after under vacuum condition, being warming up to 800 ℃～1600 ℃ with the temperature rise rate of 10 ℃/min～30 ℃/min, then close vacuum, in process furnace, charge into hydrogen, continue insulation 60min～240min, last furnace cooling obtains the tungsten skeleton;
Step 4, the silicon nitride crucible that will be placed with no-oxygen copper plate place in the process furnace, and adopt the silicon nitride hanging scaffold that the skeleton of tungsten described in the step 3 is placed directly over the silicon nitride crucible, under vacuum condition with the temperature rise rate of 10 ℃/min～30 ℃/min with stove in temperature rise to 1100 ℃～1400 ℃, to be arranged in tungsten skeleton on the silicon nitride hanging scaffold then and send into copper liquid with the fall off rate of 1mm/min～2mm/min and infiltrate, the infiltration time is 20min～120min;
Step 5, treat described in the step 4 that infiltration is finished after, close vacuum, in process furnace, charge into argon gas, promoting the silicon nitride hanging scaffold makes it separate with copper liquid, then process furnace is down to below 1000 ℃ with the rate of temperature fall of 15 ℃/min～30 ℃/min, naturally cool to discharging after the room temperature at last, obtain the tungsten carbon/carbon-copper composite material.
2. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, the material of ball grinder described in the step 1 is molybdenum.
3. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, ball milling described in the step 1 mixes employing molybdenum abrading-ball, and ratio of grinding media to material is 1: 1.
4. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, the height of spacing pressing mode restriction tungsten biscuit is adopted in compacting described in the step 2.
5. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, the pressure of suppressing described in the step 2 is 150MPa～200MPa, and the press time is 5s～8s.
6. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, the porosity of the biscuit of tungsten described in the step 2 is 35%～45%.
7. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, the flow of hydrogen described in the step 3 is 0.2m
3/ h～0.4m
3/ h, the amount of charging into of hydrogen is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
8. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1 is characterized in that, the flow 0.2m of argon gas described in the step 5
3/ h～0.4m
3/ h, the amount of charging into of argon gas is not more than 0.5 * 10 for making the process furnace internal pressure
3Pa.
9. the preparation method of a kind of tungsten carbon/carbon-copper composite material according to claim 1, it is characterized in that, the quality percentage composition of tungsten is 10%～60% in the carbon/carbon-copper composite material of tungsten described in the step 5, and the quality percentage composition of molybdenum is 20%～50%, and the quality percentage composition of copper is 20%～40%.
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| CN104259787A (en) * | 2014-09-28 | 2015-01-07 | 哈尔滨工业大学（威海） | Preparation method of powdery deformable tungsten-copper composite material thin tube |
| CN107326241A (en) * | 2017-07-10 | 2017-11-07 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN107326241B (en) * | 2017-07-10 | 2019-01-15 | 四川大学 | A method of tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN107937748B (en) * | 2017-10-20 | 2019-06-14 | 四川大学 | A method of tungsten molybdenum copper composite material is prepared with high current electrical resistance sintering |
| CN107937748A (en) * | 2017-10-20 | 2018-04-20 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with high current electrical resistance sintering |
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| CN109852861B (en) * | 2019-02-28 | 2020-07-03 | 北京工业大学 | Low-temperature rapid preparation method of high-density nanocrystalline tungsten-copper-based bulk composite material |
| CN110983085A (en) * | 2019-12-28 | 2020-04-10 | 泰州市华诚钨钼制品有限公司 | Manufacturing process of tungsten-molybdenum composite material |
| CN113493878A (en) * | 2020-04-08 | 2021-10-12 | 安泰科技股份有限公司 | Efficient and uniform metal copper infiltration composite material and preparation method thereof |
| CN113493878B (en) * | 2020-04-08 | 2022-05-27 | 安泰科技股份有限公司 | Efficient and uniform metal copper infiltration composite material and preparation method thereof |
| CN114657481A (en) * | 2022-03-08 | 2022-06-24 | 厦门欧斯拓科技有限公司 | Preparation method of rare earth composite material |
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