CN105483421A - In-situ TaC/Ta2C binary nano hard-phase strengthened copper-matrix composite material and preparation method thereof - Google Patents

In-situ TaC/Ta2C binary nano hard-phase strengthened copper-matrix composite material and preparation method thereof Download PDF

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CN105483421A
CN105483421A CN201510951847.2A CN201510951847A CN105483421A CN 105483421 A CN105483421 A CN 105483421A CN 201510951847 A CN201510951847 A CN 201510951847A CN 105483421 A CN105483421 A CN 105483421A
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tac
powder
preparation
ball
ta2c
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CN105483421B (en
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倪俊杰
张昊
刘瑞环
刘海涛
贾正锋
黄宝旭
王长征
马杰
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Liaocheng University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • 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
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Abstract

The invention belongs to the field of non-ferrous metal materials, and relates to an in-situ TaC/Ta2C binary nano hard-phase strengthened copper-matrix composite material and a preparation method thereof. An in-situ precipitated TaC/Ta2C binary nano hard-phase strengthened copper-matrix composite material with the volume percentage being 1-40vol% is prepared by adopting a multi-process synthesizing technology of mechanical ball-milling, mould pressing and sintering. The preparation method for the material comprises the steps of carrying out multi-step mechanical ball-milling on reactant powder in a certain proportion; adopting a mode of mould pressing and isostatic pressing at the room temperature to prepare a reaction green body; and finally carrying out sintering and cooling to obtain the TaC/Ta2C binary nano hard-phase strengthened copper-matrix composite material. The in-situ TaC/Ta2C binary nano hard-phase strengthened copper-matrix composite material has the main characteristics that nano-scale TaC/Ta2C is generated in situ, is uniformly distributed in matrix, is clean in particle surface, has binary hard-phase synergistic effects, has high bonding strength with a copper matrix interface, has high hardness and has good electrical conductivity.

Description

Original position TaC/Ta 2c bielement nano hard phases strengthening Cu-base composites and preparation method thereof
Technical field
The invention belongs to nonferrous materials field, relate to a kind of original position TaC/Ta 2c bielement nano hard phases strengthening Cu-base composites and preparation method thereof.
Background technology
Copper and its alloy has excellent thermal conductivity, electroconductibility and erosion resistance concurrently, of many uses in fields such as electronics, electrical equipment, heat-transfer device, contact material and space materials, has a extensive future.But the hardness of material, intensity, wear resistance, thermotolerance, mechanical behavior under high temperature are on the low side, its range of application is restricted, the fast development of current information technology and Metallurgical Industry, exacerbate the demand of society to brass works such as conticaster crystallizer, grid for welding, circuit lead frames, highlight the urgency and importance that overcome copper product shortcoming.
At present, composition of material solves one of in-problem important channel in copper and alloy thereof.In general, the Composite of copper introduces hard phase (as Al usually through in material 2o 3, SiC etc.) or high-melting-point phase (as carbon nanotube, Graphene etc.) realize, hard phase is also often high-melting-point phase, and their incorporation way includes outer addition and interior addition.Wherein, outer addition refers to and directly adds in copper product by the hard phase synthesized separately, the method is simple to operate, be easy to control, but because of the wettability between additional hard phase and Copper substrate poor, have impact on the microtexture of material, be unfavorable for the electroconductibility of Cu-base composites, in addition, hard phase needs to synthesize preparation under the high temperature conditions usually, improves the preparation cost of copper product.Interior addition separates out strengthening copper product by target hard phase in material preparation process, the method overcome the shortcoming of the outer addition of hard phase, but the carbide hard phases such as SiC, WC are but difficult to realize original position separates out because formation temperature is high, although carbide hard phase has high strength, high rigidity, high abrasion, corrosion-resistant, low density and the better advantage such as thermal conductivity concurrently, not easily pass through interior addition and be applied in copper product Composite.
There are some researches show, in Cu-base composites, the yardstick of hard phase and distribution, be the important factor affecting the mechanics of materials and electrical property.When hard phase yardstick is nanometer scale, strengthening effect is better than the strengthening effect of micro-meter scale, but the nano-powder of additional hard phase is but easily reunited, this is unfavorable for the strengthening effect giving full play to nanometer hard phase, also can reduce the homogeneity of material property, but this shortcoming can be avoided by interior addition.To sum up, be necessary to find a kind of method separating out nano-carbide strengthening phase at Cu-base composites situ.
Summary of the invention
For Problems existing in the above-mentioned state of the art, the invention provides the physicochemical characteristic of a kind of Ji Yu Tantalum and carbon reaction, utilize Tan Tantalum melting point compound high and compared with the feature of other carbide good conductivity, wild phase original position separates out the TaC/Ta being beneficial to densifying materials 2high hard copper based composites of C nano hard phase cooperative reinforcing and preparation method thereof.
Technical solution of the present invention is: original position TaC/Ta 2c bielement nano hard phases strengthening Cu-base composites, consists of: Cu 100-x[(TaC) y(Ta 2c) 100-y] x; X is the volume percent of Ta-C compound in Cu-base composites, and 1vol.%≤x≤40vol.%, y is the atomic percent in TaC Tan Tantalum compound, 5at.%≤y≤60at.%.
Foregoing original position TaC/Ta 2c bielement nano hard phases strengthening Cu-base composites, preferred scheme is, 5vol.%≤x≤30vol.% (preferred, 10vol.%≤x≤20vol.%).
Foregoing original position TaC/Ta 2c bielement nano hard phases strengthening Cu-base composites, preferred scheme is, 10at.%≤y≤40at.% (preferred, 20at.%≤y≤30at.%).
Present invention also offers described original position TaC/Ta 2the preparation method of C bielement nano hard phases strengthening Cu-base composites, step is as follows:
Step 1: according to Cu 100-x[(TaC) y(Ta 2c) 100-y] xin composition proportion, weigh Cu, Ta and C powder, and weigh stearic acid, measure ethanol according to the ratio of every 100 grams 0.5 ~ 5 milliliter, modulate the mechanical milling process control agent that stearic acid mixes with ethanol;
Step 2: Ta, C starting material that step 1 is prepared, steel ball and Mechanical Milling Process control agent, load vacuum sphere grinding jar, rear seal-cover, vacuumize, be filled with high-purity argon, carry out high-energy mechanical ball milling, Ball-milling Time 30 ~ 150 hours, rotational speed of ball-mill 250 ~ 500 revs/min, obtains the high-activity nano crystalline flour body that Ta wraps C; In oxygen-free environment, Cu powder Ta/C nanometer crystal powder and step 1 prepared mixes, load in the vacuum tank with mechanical milling process control agent, vacuumize afterwards and be filled with high-purity argon, and on ball mill, carry out mixed powder, ratio of grinding media to material 6:1 ~ 20:1 in mechanical milling process, Ball-milling Time 5 ~ 30 hours, rotational speed of ball-mill 50 ~ 150 revs/min, obtains the powder that Cu, Ta and C are evenly distributed.
Step 3: powder die mould step 2 prepared, obtains briquetting and on oil press, carries out the isostatic pressed of 100-250MPa, preparing closely knit pressed compact;
Step 4: vacuum tightness put into by pressed compact step 3 prepared is 10 -3~ 10 -4sinter in the high vacuum sintering furnace of the pa order of magnitude, pass into argon gas afterwards and carry out rapid cooling, speed of cooling is 100 DEG C/min, is cooled to room temperature, obtains high rigidity and the good Cu-base composites of electroconductibility.
Described preparation method, preferably: step 1:Cu, Ta and C powder are that particle diameter is about 10 microns, and purity is more than 99%.
Described preparation method, preferably: step 1: stearic acid dosage is the 0.1 ~ 5%(preferably 0.5 ~ 4% of Cu, Ta and C powder total mass, is more preferably 1 ~ 3%)
Described preparation method, preferably: step 2: Ta, C starting material step 1 prepared, steel ball and Mechanical Milling Process control agent, loads vacuum sphere grinding jar, ratio of grinding media to material 8:1 ~ 40:1, preferably, and ratio of grinding media to material 10:1 ~ 30:1; Be more preferably, ratio of grinding media to material 15:1 ~ 20:1.
Described preparation method, preferably: step 3: powder die mould step 2 be prepared into, molding pressure is 150-400MPa, and preferably, molding pressure is 200-300MPa; Be more preferably, molding pressure is 250MPa.
Described preparation method, preferably: step 4: sintering temperature is 650-1000 DEG C, sintering time is 1-5 hour, and preferably, sintering temperature is 750-950 DEG C, and sintering time is 2-4 hour.
The invention belongs to nonferrous materials field, relate to a kind of original position TaC/Ta 2c binary hard phases strengthening Cu-base composites and preparation method thereof.The present invention adopts mechanical ball milling, mold pressing, sintering multiple operation synthetic technology, has prepared the original position precipitation TaC/Ta that volume percent is 1-40vol% 2c bielement nano hard phase strengthens Cu-base composites.The preparation method of material is: first reactant powder is carried out multi-step mechanical ball milling in proportion, after at room temperature adopt " mold pressing-isostatic pressed " mode prepare reaction base substrate, finally sinter cooling, obtain TaC/Ta 2the Cu-base composites that C nano hard phase strengthens.Principal feature of the present invention: the TaC/Ta of nanoscale 2c in-situ preparation, is evenly distributed in the base, and particle surface is clean, and binary hard phase acts synergistically, and high with Copper substrate interface bond strength, material hardness is high and electroconductibility is good.
Excellent effect of the present invention is, owing to adopting technique scheme, compared with the Cu-base composites that the present invention obtains strengthens Cu-base composites with additional micron TaC, has higher hardness and electroconductibility; Simultaneously compared with conventional additional strengthening phase Cu-base composites preparation method, eliminate the high―temperature nuclei link of hard phase, saved the energy, reduced production cost.
Accompanying drawing explanation
Fig. 1 is that the original position of the embodiment of the present invention 1 separates out TaC/Ta 2the organization chart of C bielement nano hard phases strengthening Cu-base composites.
Embodiment
Below with reference to embodiment, the present invention will be further described, and embodiments of the invention are only for illustration of technical scheme of the present invention, and non-limiting the present invention.
Raw materials usedly in embodiment all can to buy from market.
Cu of the present invention 100-x[(TaC) y(Ta 2c) 100-y] xthe preparation method of material, conventional steps is as follows:
Step 1: according to Cu 100-x[(TaC) y(Ta 2c) 100-y] xin composition proportion, weigh Cu, Ta and C powder of purity more than 99% that particle diameter is about 10 microns, and weigh the stearic acid suitable with Cu, Ta and C powder total mass 0.1 ~ 5%, measure ethanol according to the ratio of every 100 grams 0.5 ~ 5 milliliter, modulate the mechanical milling process control agent that stearic acid mixes with ethanol;
Step 2: Ta, C starting material that step 1 is prepared, steel ball and Mechanical Milling Process control agent, load vacuum sphere grinding jar, ratio of grinding media to material 8:1 ~ 40:1, rear seal-cover, vacuumize, be filled with high-purity argon, carry out high-energy mechanical ball milling, Ball-milling Time 30 ~ 150 hours, rotational speed of ball-mill 250 ~ 500 revs/min, obtains the high-activity nano crystalline flour body that Ta wraps C; In oxygen-free environment, Cu powder Ta/C nanometer crystal powder and step 1 prepared mixes, load in the vacuum tank with mechanical milling process control agent, vacuumize afterwards and be filled with high-purity argon, and on ball mill, carry out mixed powder, ratio of grinding media to material 6:1 ~ 20:1 in mechanical milling process, Ball-milling Time 5 ~ 30 hours, rotational speed of ball-mill 50 ~ 150 revs/min, obtains the powder that Cu, Ta and C are evenly distributed.
Step 3: the powder die mould that step 2 is prepared into, molding pressure is 150-400MPa, obtains briquetting and on oil press, carries out the isostatic pressed of 100-250MPa, preparing closely knit pressed compact;
Step 4: vacuum tightness put into by pressed compact step 3 be prepared into is 10 -3~ 10 -4sinter in the high vacuum sintering furnace of the pa order of magnitude, sintering temperature is 650-1000 DEG C, and sintering time is 1-5 hour, pass into argon gas afterwards and carry out rapid cooling, speed of cooling is 100 DEG C/min, is cooled to room temperature, obtains high rigidity and the good Cu-base composites of electroconductibility.
Embodiment 1:
(1) preparation of Ta bag C nano crystalline flour body: based on Cu 90[(TaC) 20(Ta 2c) 80] 10composition proportion, to take particle diameter be the purity of 10 microns be 99.5% Ta and C powder, and vacuum sphere grinding jar is put into together with mechanical milling process control agent, in mechanical milling process control agent, stearic quality is 1% of Ta/C powder quality, and the quantity of ethanol measures by every 100 grams 2 milliliters; The quantity simultaneously loading steel ball in vacuum tank weighs by ball powder ratio 15:1; Ball material loads vacuum tank rear seal-cover and vacuumizes, and vacuum tightness reaches 5 × 10 - 1pa, afterwards applying argon gas; Rotational speed of ball-mill 400 revs/min, ball milling 96 hours, obtained Ta wraps C high-activity nano crystalline flour material.
(2) mixed powder: according to (TaC) in matrix material 20(Ta 2c) 80volume fraction be 10%, take Ta bag C nano crystalline flour, take the Cu powder that volume fraction is 90%, and load in vacuum tank together with steel ball, mechanical milling process control agent, ball material tinning process is carried out in oxygen-free environment, and process control agent is 0.5% of powder total mass, and ball powder ratio presses 10:1; Charging rear seal-cover vacuumizes, and vacuum tightness reaches 5 × 10 -1pa, is filled with argon gas; Start ball mill mixing, rotating speed 100 revs/min, batch mixing 5 hours, obtain the powder that Cu, Ta and C are evenly distributed.
(3) compression moulding: be placed on press by the powder mixed, suppress, molding pressure is 250MPa, and afterwards, briquetting carries out the isostatic pressed of 200MPa on oil press, prepares closely knit pressed compact.
(4) sinter: it is 10 that the pressed compact that step 3 is obtained is put into vacuum tightness -4sinter in the high vacuum sintering furnace of the pa order of magnitude, sintering temperature 950 DEG C, sintering time 2 hours, pass into argon gas afterwards and carry out rapid cooling, initial speed of cooling is 100 DEG C/min, obtains Cu-base composites.
Comparative example 1:
Adopting additional method to prepare containing volume fraction is the Cu-base composites of 10%TaC, wherein TaC grain size average out to 8 microns, and mixed powder in comparative example 1, compression moulding, sintering preparation technology parameter are identical with the parameter in the preparation process of example 1.
Adopt THV-100XS Vickers' hardness Standard Machine to measure hardness, during test, on-load pressure is 1.96N, and the hold-time is 15S; Adopt FQR7501A eddy current conductivity apparatus to measure the electroconductibility of material, result is as shown in table 1.
The hardness of table 1. example 1 and comparative example 1 and conductivity test data
The data of contrast table 1 are known, and original position separates out TaC/Ta 2the hardness of C bielement nano hard phases strengthening Cu-base composites and electric conductivity are higher than the respective value of Cu-base composites in comparative example, and compared with comparative example 1, the hardness of embodiment 1 improves 54.3%, and electric conductivity improves 105%.
Fig. 1 is that the original position of the embodiment of the present invention 1 separates out TaC/Ta 2the tissue topography of C bielement nano hard phases strengthening Cu-base composites.Material is fine and close as seen from Figure 1, and granular structure is evenly distributed.
Embodiment 2:
(1) preparation of Ta bag C nano crystalline flour body: based on Cu 85[(TaC) 30(Ta 2c) 70] 15composition proportion, to take particle diameter be the purity of 10 microns be 99.5% Ta and C powder, and vacuum sphere grinding jar is put into together with mechanical milling process control agent, in mechanical milling process control agent, stearic quality is 1.5% of Ta/C powder quality, and the quantity of ethanol measures by every 100 grams 1.5 milliliters; The quantity simultaneously loading steel ball in vacuum tank weighs by ball powder ratio 15:1; Ball material loads vacuum tank rear seal-cover and vacuumizes, and vacuum tightness reaches 5 × 10 -1pa, afterwards applying argon gas; Rotational speed of ball-mill 380 revs/min, ball milling 120 hours, obtained Ta wraps C high-activity nano crystalline flour material.
(2) mixed powder: according to (TaC) in matrix material 30(Ta 2c) 70volume fraction be 15%, take Ta bag C nano crystalline flour, take the Cu powder that volume fraction is 85%, and load in vacuum tank together with steel ball, mechanical milling process control agent, ball material tinning process is carried out in oxygen-free environment, and process control agent is 1.0% of powder total mass, and ball powder ratio presses 10:1; Charging rear seal-cover vacuumizes, and vacuum tightness reaches 5 × 10 -1pa, is filled with argon gas; Start ball mill mixing, rotating speed 200 revs/min, batch mixing 2 hours, obtain the powder that Cu, Ta and C are evenly distributed.
(3) compression moulding: be placed on press by the powder mixed, suppress, molding pressure is 300MPa, and afterwards, briquetting carries out the isostatic pressed of 180MPa on oil press, prepares closely knit pressed compact.
(4) sinter: it is 10 that the pressed compact that step 3 is obtained is put into vacuum tightness -4sinter in the high vacuum sintering furnace of the pa order of magnitude, sintering temperature 900 DEG C, sintering time 2 hours, pass into argon gas afterwards and carry out rapid cooling, initial speed of cooling is 100 DEG C/min, obtains Cu-base composites.
Comparative example 2:
Adopting additional method to prepare containing volume fraction is the Cu-base composites of 15%TaC, wherein TaC grain size average out to 8 microns, and mixed powder in comparative example 2, compression moulding, sintering preparation technology parameter are identical with the parameter in the preparation process of example 2.
Adopt THV-100XS Vickers' hardness Standard Machine to measure hardness, during test, on-load pressure is 1.96N, and the hold-time is 15S; Adopt FQR7501A eddy current conductivity apparatus to measure the electroconductibility of material, result is as shown in table 2.
The hardness of table 2. example 2 and comparative example 2 and conductivity test data
The data of contrast table 2 are known, and original position separates out TaC/Ta 2the hardness of C bielement nano hard phases strengthening Cu-base composites and electric conductivity are higher than the respective value of Cu-base composites in comparative example, and compared with comparative example 2, the hardness of embodiment 2 improves 46.1%, and electric conductivity improves 133.6%.
Embodiment 3:
(1) preparation of Ta bag C nano crystalline flour body: based on Cu 95[(TaC) 25(Ta 2c) 75] 5composition proportion, to take particle diameter be the purity of 10 microns be 99.5% Ta and C powder, and vacuum sphere grinding jar is put into together with mechanical milling process control agent, in mechanical milling process control agent, stearic quality is 2% of Ta/C powder quality, and the quantity of ethanol measures by every 100 grams 1 milliliter; The quantity simultaneously loading steel ball in vacuum tank weighs by ball powder ratio 15:1; Ball material loads vacuum tank rear seal-cover and vacuumizes, and vacuum tightness reaches 5 × 10 - 1pa, afterwards applying argon gas; Rotational speed of ball-mill 400 revs/min, ball milling 84 hours, obtained Ta wraps C high-activity nano crystalline flour material.
(2) mixed powder: according to (TaC) in matrix material 25(Ta 2c) 75volume fraction be 5%, take Ta bag C nano crystalline flour, take the Cu powder that volume fraction is 95%, and load in vacuum tank together with steel ball, mechanical milling process control agent, ball material tinning process is carried out in oxygen-free environment, and process control agent is 2% of powder total mass, and ball powder ratio presses 10:1; Charging rear seal-cover vacuumizes, and vacuum tightness reaches 5 × 10 -1pa, is filled with argon gas; Start ball mill mixing, rotating speed 100 revs/min, batch mixing 5 hours, obtain the powder that Cu, Ta and C are evenly distributed.
(3) compression moulding: be placed on press by the powder mixed, suppress, molding pressure is 250MPa, and afterwards, briquetting carries out the isostatic pressed of 100MPa on oil press, prepares closely knit pressed compact.
(4) sinter: it is 10 that the pressed compact that step 3 is obtained is put into vacuum tightness -4sinter in the high vacuum sintering furnace of the pa order of magnitude, sintering temperature 920 DEG C, sintering time 2 hours, pass into argon gas afterwards and carry out rapid cooling, initial speed of cooling is 100 DEG C/min, obtains Cu-base composites.
Comparative example 3:
Adopting additional method to prepare containing volume fraction is the Cu-base composites of 5%TaC, wherein TaC grain size average out to 8 microns, and mixed powder in comparative example 3, compression moulding, sintering preparation technology parameter are identical with the parameter in the preparation process of example 3.
Adopt THV-100XS Vickers' hardness Standard Machine to measure hardness, during test, on-load pressure is 1.96N, and the hold-time is 15S; Adopt FQR7501A eddy current conductivity apparatus to measure the electroconductibility of material, result is as shown in table 3.
The hardness of table 3. example 3 and comparative example 3 and conductivity test data
The data of contrast table 3 are known, and original position separates out TaC/Ta 2the hardness of C bielement nano hard phases strengthening Cu-base composites and electric conductivity are higher than the respective value of Cu-base composites in comparative example, and compared with comparative example 3, the hardness of embodiment 3 improves 66.1%, and electric conductivity improves 69.7%.
The application be based on Shandong Province's development in science and technology planning item (numbering: 2014GGX102016) and Shandong Province's Natural Science Fund In The Light (numbering: ZR2013EMM010) subsidy.

Claims (9)

1. original position TaC/Ta 2c bielement nano hard phases strengthening Cu-base composites, is characterized in that, consist of: Cu 100-x[(TaC) y(Ta 2c) 100-y] x; X is the volume percent of Ta-C compound in Cu-base composites, and 1vol.%≤x≤40vol.%, y is the atomic percent in TaC Tan Tantalum compound, 5at.%≤y≤60at.%.
2. original position TaC/Ta according to claim 1 2c bielement nano hard phases strengthening Cu-base composites, is characterized in that, 5vol.%≤x≤30vol.%(is preferred, 10vol.%≤x≤20vol.%).
3. original position TaC/Ta according to claim 1 2c bielement nano hard phases strengthening Cu-base composites, is characterized in that, 10at.%≤y≤40at.%(is preferred, 20at.%≤y≤30at.%).
4. original position TaC/Ta according to claim 1 2the preparation method of C bielement nano hard phases strengthening Cu-base composites, is characterized in that: step is as follows:
Step 1: according to Cu 100-x[(TaC) y(Ta 2c) 100-y] xin composition proportion, weigh Cu, Ta and C powder, and weigh stearic acid, measure ethanol according to the ratio of every 100 grams 0.5 ~ 5 milliliter, modulate the mechanical milling process control agent that stearic acid mixes with ethanol;
Step 2: Ta, C starting material that step 1 is prepared, steel ball and Mechanical Milling Process control agent, load vacuum sphere grinding jar, rear seal-cover, vacuumize, be filled with high-purity argon, carry out high-energy mechanical ball milling, Ball-milling Time 30 ~ 150 hours, rotational speed of ball-mill 250 ~ 500 revs/min, obtains the high-activity nano crystalline flour body that Ta wraps C; In oxygen-free environment, Cu powder Ta/C nanometer crystal powder and step 1 prepared mixes, load in the vacuum tank with mechanical milling process control agent, vacuumize afterwards and be filled with high-purity argon, and on ball mill, carry out mixed powder, ratio of grinding media to material 6:1 ~ 20:1 in mechanical milling process, Ball-milling Time 5 ~ 30 hours, rotational speed of ball-mill 50 ~ 150 revs/min, obtains the powder that Cu, Ta and C are evenly distributed.
5. step 3: powder die mould step 2 prepared, obtains briquetting and on oil press, carries out the isostatic pressed of 100-250MPa, preparing closely knit pressed compact;
Step 4: vacuum tightness put into by pressed compact step 3 be prepared into is 10 -3~ 10 -4sinter in the high vacuum sintering furnace of the pa order of magnitude, pass into argon gas afterwards and carry out rapid cooling, speed of cooling is 100 DEG C/min, is cooled to room temperature, obtains high rigidity and the good Cu-base composites of electroconductibility.
6. preparation method according to claim 4, is characterized in that: step 1:Cu, Ta and C powder are that particle diameter is about 10 microns, and purity is more than 99%.
7. preparation method according to claim 4, is characterized in that: step 1: stearic acid dosage is the 0.1 ~ 5%(preferably 0.5 ~ 4% of Cu, Ta and C powder total mass, is more preferably 1 ~ 3%)
Preparation method according to claim 4, is characterized in that: step 2: Ta, C starting material step 1 prepared, steel ball and Mechanical Milling Process control agent, loads vacuum sphere grinding jar, and ratio of grinding media to material 8:1 ~ 40:1(is preferred, ratio of grinding media to material 10:1 ~ 30:1; Be more preferably, ratio of grinding media to material 15:1 ~ 20:1).
8. preparation method according to claim 4, is characterized in that: step 3: powder die mould step 2 be prepared into, and molding pressure is that 150-400MPa(is preferred, and molding pressure is 200-300MPa; Be more preferably, molding pressure is 250MPa).
9. preparation method according to claim 4, is characterized in that: step 4: sintering temperature is 650-1000 DEG C, and sintering time is 1-5 hour (preferred, sintering temperature is 750-950 DEG C, and sintering time is 2-4 hour).
CN201510951847.2A 2015-12-18 2015-12-18 TaC/Ta in situ2C bielement nano hard phases strengthening Cu-base composites and preparation method thereof Expired - Fee Related CN105483421B (en)

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