CN103194629B - Method for preparing tungsten molybdenum copper composite material - Google Patents
Method for preparing tungsten molybdenum copper composite material Download PDFInfo
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- CN103194629B CN103194629B CN201310098234.XA CN201310098234A CN103194629B CN 103194629 B CN103194629 B CN 103194629B CN 201310098234 A CN201310098234 A CN 201310098234A CN 103194629 B CN103194629 B CN 103194629B
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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 technical field of composite preparation, be specifically related to a kind of preparation method of tungsten molybdenum copper composite material.
Background technology
Tungsten copper " alloy ", molybdenum copper " alloy " are referred to as " pseudoalloy " usually because tungsten, molybdenum and copper are difficult to the alloying that formed truly, and its essence is the matrix material of two-phase or a few phase metal composition.Usual tungsten, molybdenum are high using its fusing point, hot strength is high, ablation resistance is excellent and thermal expansivity is low and as the base material of matrix material, copper then using its heat conduction, conductivity is excellent and plasticity is good and as the compound phase of matrix material.
At present, the preparation method of tungsten copper, composite material of molybdenum and copper mainly contains infiltration method, powder metallurgic method.The W skeleton that infiltration method utilizes tungsten powder, molybdenum powder compacting sintering prepares certain porosity, molybdenum skeleton, then utilize electrolytic copper powder to be pressed into copper coin or directly utilize fine copper plate to carry out liquid-phase infiltrating (Xue Xiang, Li Song, the progress of the .W-Cu matrix materials such as Qiu Ruliang. material Leader, 2008,22(X): 294 ~ 298; Han Shengli, Song Yueqing, Cui Shun, wait the R and D of .Mo-Cu alloy to be in progress. powder metallurgy industry, 2007,17(5): 40 ~ 45).The shortcoming of infiltration method is tungsten copper, still must carry out mechanical process to remove unnecessary copper after molybdenum infiltration of copper, and it is restricted that the densification difference of its product also makes it widely use, and also has no report simultaneously and utilize infiltration method to prepare the documents and materials of tungsten molybdenum copper composite material.
Namely powder metallurgic method prepares tungsten copper, molybdenum copper or tungsten copper composite powder, then compression moulding, liquid phase sintering is fine and close and carry out subsequent densification or processing treatment (V.I.Nizhenko, V.Ya.Petrishchev, and V.V.Shorokhod.Effect of Liquid Phase on theDensification of Tungsten-Copper and Molybdenum-Copper Pseudoalloys inSingtering.Powder Metallurgy and Metal Ceramics, 2008, Vol.47, NOS.3-4).Investigator's ammonium metawolframate and cupric nitrate is had to make precursor solution, dry obtained precursor powder, then carry out calcining, hydrogen reduction obtains W-Cu composite powder (Su Weifeng, Xiong Ning, Zhou Wuping etc. a kind of novel process preparing W-Cu matrix material. Materials Science and Engineering of Powder Metallurgy, 2007,12 (6): 369 ~ 373).Have research directly utilize the oxide powder of tungsten, molybdenum and copper in a hydrogen atmosphere coreduction prepare tungsten copper, molybdenum cuprum composite powder (Li Yuan, Zhai Yuchun, Tian Yanwen, etc. Preparation of W-Cu Composite Powders by Hydrogen Reduction of W-Cu Compound is studied. material Leader, 2004,18(1): 95 ~ 99).Also have research and utilization sol-gel method prepare tungsten copper, molybdenum cuprum composite powder (preparation of sol-gel of the .WCu composite granule such as Zhao Ming, Wang Jinshu, Liu Wei and reduction act research thereof. Rare Metals Materials and engineering, 2011,2:362-366; Highly account for English, Chen Wenge, fourth is held political power. Fabrication of Composite Nanopowders of MoCu by Sol-Gel. and Rare Metals Materials and engineering, 2005,34 (6): 990 ~ 993).In addition high-energy ball milling machinery alloying (MA) legal system was also once widely studied (Li Yunping for tungsten copper, molybdenum copper powder, Qu Xuanhui, Zheng Zhoushun etc. Thermomechanical process producing W-Cu composite powder with ultrafine dispersion structure. powder metallurgy technology, 2004,22(5): 266 ~ 269; Zhou Xianliang, is full of sea, Hua little Zhen etc. and mechanical alloying is on the impact of Mo-Cu alloy property. powder metallurgy technology, 2007,25(1): 21 ~ 23).Above-mentionedly prepare in tungsten copper, molybdenum cuprum composite powder MATERIALS METHODS, the method of presoma calcining reduction is utilized to introduce the method for chemistry, its advantage is can by mixed powder disperse refinement, likely improve the homogeneity of tungsten copper, molybdenum copper sintered compact, but extend composite material preparation process flow process, add uncontrollable factor, also there is not yet the report of extensive application.The factors the such as during Reduction of Oxide of oxide compound hydrogen co-reducing process due to tungsten, molybdenum, copper, reduction temperature difference is comparatively large, Thermodynamics is complicated, atmosphere is wayward cause reducing process complicated, the defects such as simultaneously the composite granule character prepared of this method is unstable, and the tungsten copper causing following liquid-phase to sinter as powder size skewness, plasticity difference etc., the microtexture of molybdenum copper are uneven are more.Sol-gel method is still in the R and D of laboratory stage, and industrial applications need further investigation.High-energy ball milling machinery alloying (MA) method is expected to utilize collision energy in Process During High Energy Ball Milling by tungsten powder, molybdenum powder and copper powder carry out cold welding, or friction welding etc. is adhered and forms mechanical alloying powder, or by tungsten powder, molybdenum powder, copper powder is milled to ultra-fine or Nano grade, but due to the ball milling tank body in Process During High Energy Ball Milling, abrading-ball or agitator arm use stainless steel usually, the materials such as zirconium white or other alloy, inevitably by Fe, Ni, Zr, the impurity such as Si are brought in mixed powder, significantly worsen the heat conduction of the finished product, the performances such as conduction, simultaneously for pursue mixed powder ultra-fine size and for a long time ball milling powder O content also can be made sharply to increase, and mixed powder can be made to be adhered on the wall of ball milling chamber, or to be adhered on abrading-ball not easily collecting.In general powder metallurgic method prepare tungsten copper, molybdenum copper powder after overmolding, the density that liquid phase sintering can acquire a certain degree, its advantage only needs less processing or do not need to carry out machining, thus improve 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 completely, and sintered compact is difficult to complete densification.The preparation method of these tungsten coppers above-mentioned, molybdenum copper, tungsten molybdenum copper composite material is in laboratory development mostly at present, the production that equal prematurity is a large amount of and application.
Summary of the invention
Technical problem to be solved by this invention is, for above-mentioned the deficiencies in the prior art, to provide a kind of preparation method of tungsten molybdenum copper composite material.The method eliminates machining procedure, saved material, simplify technique and easy to implement, the powder that employing is 1: 2 through screening process acquisition tungsten powder and the ratio of the Fisher particle size of molybdenum powder is raw material, eliminate tungsten powder, molybdenum powder and cause the problem of batch mixing inequality due to difference of specific gravity, compared with common batch mixing, significantly reduce mixing time thus C, O content in powder can be reduced; Pre-burning skeleton step adopts the sintering method of first vacuum, rear hydrogen atmosphere, is conducive to molybdenum skeleton and forms through hole thus be beneficial to follow-up infiltration process; Adopt vacuum atmosphere in the vacuum infiltration stage, immersed in liquid phase copper by pre-burning skeleton, be conducive to liquid phase copper and fully spread in molybdenum hole, prepared tungsten molybdenum 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 molybdenum copper composite material, is characterized in that, the method comprises the following steps:
Step one, tungsten powder and molybdenum powder carried out respectively screening process, then by obtain after screening process tungsten powder and molybdenum powder add in ball grinder, obtain tungsten mixed powder after ball milling mixing 60min ~ 240min; The ratio of the tungsten powder obtained after screening process and the Fisher particle size of molybdenum powder is 1: 2;
Step 2, the mixed powder of tungsten described in step one is pressed into tungsten biscuit;
Step 3, the biscuit of tungsten described in step 2 is placed on smooth silicon nitride hanging scaffold, then be together placed in process furnace, 60min ~ 240min is incubated after being warming up to 800 DEG C ~ 1600 DEG C with the temperature rise rate of 10 DEG C/min ~ 30 DEG C/min under vacuum, then vacuum is closed, hydrogen is filled with in process furnace, continue insulation 60min ~ 240min, last furnace cooling, obtains tungsten skeleton;
Step 4, the silicon nitride crucible being placed with no-oxygen copper plate is placed in process furnace, and adopt silicon nitride hanging scaffold to be placed in directly over silicon nitride crucible by the skeleton of tungsten described in step 3, with the temperature rise rate of 10 DEG C/min ~ 30 DEG C/min, in-furnace temperature is risen to 1100 DEG C ~ 1400 DEG C under vacuum, then the tungsten skeleton be arranged on silicon nitride hanging scaffold is sent into copper liquid with the fall off rate of 1mm/min ~ 2mm/min to infiltrate, the infiltration time is 20min ~ 120min;
Step 5, after having infiltrated described in step 4, close vacuum, argon gas is filled with in process furnace, promoting silicon nitride hanging scaffold makes it be separated with copper liquid, then process furnace is down to less than 1000 DEG C with the rate of temperature fall of 15 DEG C/min ~ 30 DEG C/min, finally naturally cool to discharging after room temperature, obtain tungsten molybdenum copper composite material.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, the material of ball grinder described in step one is molybdenum.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, the mixing of ball milling described in step one adopts molybdenum abrading-ball, and ratio of grinding media to material is 1: 1.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, compacting described in step 2 adopts the height of spacing pressing mode restriction tungsten biscuit.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, the pressure suppressed described in step 2 is 150MPa ~ 200MPa, and the press time is 5s ~ 8s.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, the porosity of the biscuit of tungsten described in step 2 is 35% ~ 45%.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, the flow of hydrogen described in step 3 is 0.2m
3/ h ~ 0.4m
3/ h, the charge of hydrogen is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, the flow 0.2m of argon gas described in step 5
3/ h ~ 0.4m
3/ h, the charge of argon gas is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
The preparation method of above-mentioned a kind of tungsten molybdenum copper composite material, in tungsten molybdenum copper composite material described in step 5, the mass percentage of tungsten is 10% ~ 60%, and the mass percentage of molybdenum is 20% ~ 50%, and the mass percentage 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 adjust 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 obtains tungsten powder Fisher particle size through screening process: molybdenum powder Fisher particle size is the powder of 1: 2, eliminate tungsten powder, molybdenum powder and cause the uneven problem of batch mixing due to difference of specific gravity, compared with common batch mixing, significantly reduce mixing time thus C, O content in powder can be reduced; Molybdenum batch can and abrading-ball is adopted in mixed powder process, stainless steel batch can is used with common, the method of the material such as zirconium white, wolfram varbide abrading-ball is compared, can not increase the impurity such as Fe, the Ni brought due to tank body and Ball wear effect in mixed powder process, in the tungsten molybdenum copper composite material of preparation, the impurity content such as C, O, Fe, Ni is low.
3, pre-burning skeleton step of the present invention adopts the sintering method of first vacuum, rear hydrogen atmosphere, is conducive to molybdenum skeleton and forms through hole thus be beneficial to follow-up infiltration process.
4, the present invention adopts vacuum atmosphere in the vacuum infiltration stage, pre-burning skeleton is immersed in liquid phase copper, be conducive to liquid phase copper fully to spread in molybdenum hole, prepared tungsten molybdenum 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, the carbonization phenomenon of molybdenum in the infiltration stage can be eliminated, ensure that the thing of tungsten molybdenum copper composite material is stablized mutually.
5, tungsten molybdenum copper composite material is separated with liquid phase copper by the present invention after infiltration completes, argon gas atmosphere is utilized to cool fast, inhibit the volatilization of copper phase in the rear tungsten molybdenum copper composite material of infiltration, compared with traditional tungsten copper, the follow-up method also needing machining to remove copper of molybdenum infiltration of copper, eliminate machining procedure, saved material, simplify technique and easy to implement.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the SEM photo of W60Mo20Cu20 matrix material nature fracture prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM photo of W30Mo40Cu30 matrix material nature fracture prepared by the embodiment of the present invention 2.
Fig. 3 is the SEM photo of W10Mo50Cu40 matrix material nature fracture prepared by the embodiment of the present invention 3.
Embodiment
Embodiment 1
The preparation of W60Mo20Cu20 matrix material
Step one, to be the tungsten powder of 1.0 μm and Fisher particle size by Fisher particle size be, and the molybdenum powder of 3.5 μm utilizes 200 order/400, the order/300 multistage sieves of order to carry out screening process respectively, to obtain Fisher particle size be the tungsten powder of 1.5 μm and Fisher particle size is the molybdenum powder of 3 μm, then to be the tungsten powder of 1.5 μm and 2kg Fisher particle size by 6kg Fisher particle size be, and the molybdenum powder of 3 μm adds in molybdenum ball grinder, obtains tungsten mixed powder after adopting the molybdenum abrading-ball ball milling mixing 60min of 8kg Ф 5;
Step 2, take tungsten mixed powder described in 1100g step one, load length and width and be respectively in the die cavity of 50mm, 100mm, adopt oil press to carry out spacing compacting, maximum height limit is 20mm, obtains 20 × 50 × 100mm tungsten biscuit that porosity is 35%; The pressure of described compacting is 200MPa, and the press time is 5s;
Step 3, the biscuit of tungsten described in step 2 is placed on smooth silicon nitride hanging scaffold, then be together placed in process furnace, be evacuated to 0.02Pa, 60min is incubated after being warming up to 1600 DEG C with the temperature rise rate of 30 DEG C/min, then close vacuum pump set, in process furnace, be filled with hydrogen, continue insulation 60min, last furnace cooling, obtains tungsten skeleton; The flow of described hydrogen is 0.2m
3/ h, the charge of hydrogen is not more than 0.5 × 10 for making process furnace internal pressure
3pa;
Step 4, the silicon nitride crucible being placed with no-oxygen copper plate is placed in process furnace, and adopt silicon nitride hanging scaffold to be placed in directly over silicon nitride crucible by the skeleton of tungsten described in step 3, with the temperature rise rate of 30 DEG C/min, in-furnace temperature is risen to 1200 DEG C after being evacuated to 0.02Pa, then the tungsten skeleton be arranged on silicon nitride hanging scaffold is sent into copper liquid with the fall off rate of 1mm/min to infiltrate, the infiltration time is 20min;
Step 5, after having infiltrated described in step 4, close vacuum pump set, argon gas is filled with in process furnace, promoting silicon nitride hanging scaffold makes it be separated with copper liquid, then furnace temperature of heating furnace is down to less than 1000 DEG C with the rate of temperature fall of 30 DEG C/min, finally naturally cool to discharging after room temperature, obtain tungsten molybdenum copper composite material; The flow 0.2m of described argon gas
3/ h, the charge of argon gas is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
After testing, in tungsten molybdenum copper composite material obtained in the present embodiment, W content is 59wt%, and molybdenum content is 20wt%, and copper content is 21wt%, and relative density is 99.3%.Fig. 1 is the SEM photo of W60Mo20Cu20 matrix material nature fracture prepared by the present embodiment.As can be seen from Figure 1, in W60Mo20Cu20 matrix material, W, Mo phase is uniformly distributed, and Cu phase is with latticed by W, Mo particle encapsulation, and residual porosity is few.
Embodiment 2
The preparation of W30Mo40Cu30 matrix material
Step one, to be the tungsten powder of 1.0 μm and Fisher particle size by Fisher particle size be, and the molybdenum powder of 3.5 μm utilizes 200 order/400, the order/300 multistage sieves of order to carry out screening process respectively, to obtain Fisher particle size be the tungsten powder of 1.5 μm and Fisher particle size is the molybdenum powder of 3 μm, then to be the tungsten powder of 1.5 μm and 4kg Fisher particle size by 3kg Fisher particle size be, and the molybdenum powder of 3 μm adds in molybdenum ball grinder, obtains tungsten mixed powder after adopting the molybdenum abrading-ball ball milling mixing 120min of 7kg Ф 5;
Step 2, take tungsten mixed powder described in 1250g step one, load length and width and be respectively in the die cavity of 50mm, 100mm, adopt oil press to carry out spacing compacting, maximum height limit is 30mm, obtains 30 × 50 × 100mm tungsten biscuit that porosity is 41%; The pressure of described compacting is 180MPa, and the press time is 6s;
Step 3, the biscuit of tungsten described in step 2 is placed on smooth silicon nitride hanging scaffold, then be together placed in process furnace, be evacuated to 0.02Pa, 120min is incubated after being warming up to 1200 DEG C with the temperature rise rate of 15 DEG C/min, then close vacuum pump set, in process furnace, be filled with hydrogen, continue insulation 120min, last furnace cooling, obtains tungsten skeleton; The flow of described hydrogen is 0.3m
3/ h, the charge of hydrogen is not more than 0.5 × 10 for making process furnace internal pressure
3pa;
Step 4, the silicon nitride crucible being placed with no-oxygen copper plate is placed in process furnace, and adopt silicon nitride hanging scaffold to be placed in directly over silicon nitride crucible by the skeleton of tungsten described in step 3, with the temperature rise rate of 15 DEG C/min, in-furnace temperature is risen to 1100 DEG C after being evacuated to 0.02Pa, then the tungsten skeleton be arranged on silicon nitride hanging scaffold is sent into copper liquid with the fall off rate of 1.5mm/min to infiltrate, the infiltration time is 60min;
Step 5, after having infiltrated described in step 4, close vacuum pump set, argon gas is filled with in process furnace, promoting silicon nitride hanging scaffold makes it be separated with copper liquid, then furnace temperature of heating furnace is down to less than 1000 DEG C with the rate of temperature fall of 15 DEG C/min, finally naturally cool to discharging after room temperature, obtain tungsten molybdenum copper composite material; The flow 0.3m of described argon gas
3/ h, the charge of argon gas is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
After testing, in tungsten molybdenum copper composite material obtained in the present embodiment, W content is 30.5wt%, and molybdenum content is 41wt%, and copper content is 28.5wt%, and relative density is 99.2%.Fig. 2 is the SEM photo of W30Mo40Cu30 matrix material nature fracture prepared by the present embodiment.As can be seen from Figure 2, in W30Mo40Cu30 matrix material, W, Mo phase is uniformly distributed, and Cu phase is with latticed by W, Mo particle encapsulation, and residual porosity is few.
Embodiment 3
The preparation of W10Mo50Cu40 matrix material
Step one, to be the tungsten powder of 1.0 μm and Fisher particle size by Fisher particle size be, and the molybdenum powder of 3.5 μm utilizes 200 order/400, the order/300 multistage sieves of order to carry out screening process respectively, to obtain Fisher particle size be the tungsten powder of 1.5 μm and Fisher particle size is the molybdenum powder of 3 μm, then to be the tungsten powder of 1.5 μm and 6kg Fisher particle size by 1.2kg Fisher particle size be, and the molybdenum powder of 3 μm adds in molybdenum ball grinder, obtains tungsten mixed powder after adopting the molybdenum abrading-ball ball milling mixing 240min of 7.2kg Ф 5;
Step 2, take tungsten mixed powder described in 1250g step one, load length and width and be respectively in the die cavity of 50mm, 100mm, adopt oil press to carry out spacing compacting, maximum height limit is 40mm, obtains 40 × 50 × 100mm tungsten biscuit that porosity is 45%; The pressure of described compacting is 150MPa, and the press time is 8s;
Step 3, the biscuit of tungsten described in step 2 is placed on smooth silicon nitride hanging scaffold, then be together placed in process furnace, be evacuated to 0.02Pa, 240min is incubated after being warming up to 800 DEG C with the temperature rise rate of 10 DEG C/min, then close vacuum pump set, in process furnace, be filled with hydrogen, continue insulation 240min, last furnace cooling, obtains tungsten skeleton; The flow of described hydrogen is 0.4m
3/ h, the charge of hydrogen is not more than 0.5 × 10 for making process furnace internal pressure
3pa;
Step 4, the silicon nitride crucible being placed with no-oxygen copper plate is placed in process furnace, and adopt silicon nitride hanging scaffold to be placed in directly over silicon nitride crucible by the skeleton of tungsten described in step 3, with the temperature rise rate of 10 DEG C/min, in-furnace temperature is risen to 1400 DEG C after being evacuated to 0.02Pa, then the tungsten skeleton be arranged on silicon nitride hanging scaffold is sent into copper liquid with the fall off rate of 2mm/min to infiltrate, the infiltration time is 120min;
Step 5, after having infiltrated described in step 4, close vacuum pump set, argon gas is filled with in process furnace, promoting silicon nitride hanging scaffold makes it be separated with copper liquid, then furnace temperature of heating furnace is down to less than 1000 DEG C with the rate of temperature fall of 20 DEG C/min, finally naturally cool to discharging after room temperature, obtain tungsten molybdenum copper composite material; The flow 0.4m of described argon gas
3/ h, the charge of argon gas is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
After testing, in tungsten molybdenum copper composite material obtained in the present embodiment, W content is 10wt%, and molybdenum content is 50.3wt%, and copper content is 39.7wt%, and relative density is 99.5%.Fig. 3 is the SEM photo of W10Mo50Cu40 matrix material nature fracture prepared by the present embodiment.As can be seen from Figure 3, in W10Mo50Cu40 matrix material, W, Mo phase is uniformly distributed, and Cu phase is with latticed by W, Mo particle encapsulation, and residual porosity is few.
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (8)
1. a preparation method for tungsten molybdenum copper composite material, is characterized in that, the method comprises the following steps:
Step one, tungsten powder and molybdenum powder carried out respectively screening process, be then that tungsten powder and the molybdenum powder of 1: 2 adds in ball grinder by the ratio of the Fisher particle size obtained after screening process, after ball milling mixing 60min ~ 240min, obtain tungsten mixed powder;
Step 2, the mixed powder of tungsten described in step one is pressed into tungsten biscuit; Described compacting adopts the height of spacing pressing mode restriction tungsten biscuit;
Step 3, the biscuit of tungsten described in step 2 is placed on smooth silicon nitride hanging scaffold, then be together placed in process furnace, 60min ~ 240min is incubated after being warming up to 800 DEG C ~ 1600 DEG C with the temperature rise rate of 10 DEG C/min ~ 30 DEG C/min under vacuum, then vacuum is closed, hydrogen is filled with in process furnace, continue insulation 60min ~ 240min, last furnace cooling, obtains tungsten skeleton;
Step 4, the silicon nitride crucible being placed with no-oxygen copper plate is placed in process furnace, and adopt silicon nitride hanging scaffold to be placed in directly over silicon nitride crucible by the skeleton of tungsten described in step 3, with the temperature rise rate of 10 DEG C/min ~ 30 DEG C/min, in-furnace temperature is risen to 1100 DEG C ~ 1400 DEG C under vacuum, then the tungsten skeleton be arranged on silicon nitride hanging scaffold is sent into copper liquid with the fall off rate of 1mm/min ~ 2mm/min to infiltrate, the infiltration time is 20min ~ 120min;
Step 5, after having infiltrated described in step 4, close vacuum, argon gas is filled with in process furnace, promoting silicon nitride hanging scaffold makes it be separated with copper liquid, then process furnace is down to less than 1000 DEG C with the rate of temperature fall of 15 DEG C/min ~ 30 DEG C/min, finally naturally cool to discharging after room temperature, obtain tungsten molybdenum copper composite material.
2. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, is characterized in that, the material of ball grinder described in step one is molybdenum.
3. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, is characterized in that, the mixing of ball milling described in step one adopts molybdenum abrading-ball, and ratio of grinding media to material is 1: 1.
4. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, is characterized in that, the pressure suppressed described in step 2 is 150MPa ~ 200MPa, and the press time is 5s ~ 8s.
5. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, is characterized in that, the porosity of the biscuit of tungsten described in step 2 is 35% ~ 45%.
6. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, is characterized in that, the flow of hydrogen described in step 3 is 0.2m
3/ h ~ 0.4m
3/ h, the charge of hydrogen is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
7. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, is characterized in that, the flow 0.2m of argon gas described in step 5
3/ h ~ 0.4m
3/ h, the charge of argon gas is not more than 0.5 × 10 for making process furnace internal pressure
3pa.
8. the preparation method of a kind of tungsten molybdenum copper composite material according to claim 1, it is characterized in that, in tungsten molybdenum copper composite material described in step 5, the mass percentage of tungsten is 10% ~ 60%, and the mass percentage of molybdenum is 20% ~ 50%, and the mass percentage of copper is 20% ~ 40%.
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| CN107904466A (en) * | 2017-12-05 | 2018-04-13 | 安徽恒利增材制造科技有限公司 | A kind of high intensity tungsten molybdenum alloy |
| CN109261974B (en) * | 2018-08-23 | 2021-02-19 | 长沙升华微电子材料有限公司 | Multi-element pseudo alloy composite material and preparation method and application thereof |
| 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 |
| 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 |
| CN114657481B (en) * | 2022-03-08 | 2023-03-24 | 厦门欧斯拓科技有限公司 | Preparation method of rare earth composite material |
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| US5912399A (en) * | 1995-11-15 | 1999-06-15 | Materials Modification Inc. | Chemical synthesis of refractory metal based composite powders |
| JP2003213360A (en) * | 2002-01-23 | 2003-07-30 | Yamaha Corp | High thermoconductive alloy |
| CN100355924C (en) * | 2003-09-05 | 2007-12-19 | 上海材料研究所 | Tungsten copper functional composite material and its preparation technology |
| CN100436616C (en) * | 2006-11-03 | 2008-11-26 | 北京科技大学 | Preparation method of near fully densificated high W or Mo content W-Cu or Mo-Cu composite material |
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