CN114932222B - Method for improving density of tungsten-copper alloy - Google Patents
Method for improving density of tungsten-copper alloy Download PDFInfo
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- CN114932222B CN114932222B CN202210691729.2A CN202210691729A CN114932222B CN 114932222 B CN114932222 B CN 114932222B CN 202210691729 A CN202210691729 A CN 202210691729A CN 114932222 B CN114932222 B CN 114932222B
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- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 65
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 62
- 238000005245 sintering Methods 0.000 claims abstract description 73
- 230000008569 process Effects 0.000 claims abstract description 37
- 239000011148 porous material Substances 0.000 claims abstract description 34
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 22
- 238000011049 filling Methods 0.000 claims abstract description 19
- 239000000523 sample Substances 0.000 claims description 57
- 238000001035 drying Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 241000080590 Niso Species 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000012496 blank sample Substances 0.000 claims description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 23
- 229910052721 tungsten Inorganic materials 0.000 abstract description 18
- 229910052802 copper Inorganic materials 0.000 abstract description 17
- 229910002482 Cu–Ni Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 4
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 229910052759 nickel Inorganic materials 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 239000006104 solid solution Substances 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 230000007547 defect Effects 0.000 description 7
- 239000010937 tungsten Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003657 tungsten Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
- B22F2201/013—Hydrogen
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/02—Nitrogen
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a method for improving the compactness of a tungsten-copper alloy, which comprises the steps of preparing a filling solution, soaking a tungsten-copper alloy rough blank, sintering the tungsten-copper rough blank and the like. According to the method for improving the density of the tungsten-copper alloy, the tungsten-copper alloy rough blank is placed in the pore filling solution for soaking, then is dried and sintered, and various oxides at the pores can be reduced into Cu, W and Ni by utilizing a three-step sintering process, so that the pores are filled and the density is improved. In addition, the addition of Ni can increase the activity of the powder, improve the flow property of Cu and the diffusion migration speed of Cu, and meanwhile, ni and Cu can form a Cu-Ni solid solution phase so that W has a certain solubility in the Cu-Ni phase to increase the interface structure between W and Cu, thereby further improving the compactness. The invention has simple process, can process alloy parts with complex shapes, has lower cost and high production efficiency, and is suitable for mass production.
Description
Technical Field
The invention relates to the technical field of tungsten-copper alloy preparation, in particular to a method for improving the compactness of tungsten-copper alloy.
Background
The tungsten-copper alloy is a pseudo alloy composed of high-melting-point, high-hardness and low-expansion tungsten and high-electric and heat-conducting copper, integrates the advantages of tungsten and copper, and is widely applied to the fields of electric contact materials, electronic packaging materials, armor-piercing materials, nuclear fusion materials and the like. In recent years, with the rapid development of the national chip industry, the demand for high-performance tungsten copper alloy materials for electronic packaging is increasing.
Tungsten is difficult to prepare by conventional smelting methods because the melting point of tungsten is far higher than that of copper and because tungsten is not miscible with copper. At present, the main processes for preparing tungsten-copper alloy are an infiltration method and a powder metallurgy method. The infiltration method is to infiltrate liquid copper into a porous tungsten skeleton prepared in advance, but the defects of pores, copper lakes, tungsten clusters and the like are easily generated, so that the density of the prepared tungsten-copper alloy is not high, and the performance of the prepared material is seriously reduced. The powder metallurgy method is to fill uniformly mixed tungsten powder and copper powder into a die cavity, and then heat and sinter the mixed powder, but the density of the prepared material is not high due to mutual insolubility and poor wettability of tungsten and copper, and although auxiliary sintering modes such as liquid phase sintering, microwave sintering, activated sintering and the like are also developed, the density of the obtained tungsten-copper alloy still does not meet the requirements in some special application occasions. Therefore, the development of a method for improving the compactness of the tungsten-copper alloy has very important significance.
Disclosure of Invention
The invention aims at: a method for improving the compactness of tungsten-copper alloy is provided to solve the defects.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for improving the compactness of tungsten-copper alloy, comprising the following steps:
s1, preparing a filling solution: cuNO is to 3 、H 28 N 6 O 41 W 12 、NiSO 4 Preparing an aqueous solution with filled pores according to a certain proportion;
s2, soaking a tungsten-copper alloy rough blank: placing the pre-mixed powder and the pressed tungsten-copper alloy rough blank into the pore filling solution prepared in the step S1 for soaking for 2-6 h at 20-60 ℃;
s3, sintering a tungsten copper rough blank: drying the tungsten copper alloy rough blank sample soaked in the step S2 in a drying box to remove water of the sample, and then placing the sample in a sintering furnace for sectional sintering; and after sintering is finished, the whole process of improving the density of the tungsten-copper alloy can be completed.
Preferably, in step S1, the raw material CuNO 3 、H 28 N 6 O 41 W 12 、NiSO 4 The weight ratio of the deionized water is (5-10): (5-10): (0-5): (75-90).
Preferably, in step S3, the sintering adopts a continuous three-step sintering process, and the first-step sintering process is as follows: heating the sample to 280-420 ℃ and preserving heat for 1-3 hours, wherein the sintering atmosphere is nitrogen; the second sintering process comprises the following steps: heating the sample to 600-850 ℃ and preserving heat for 1-3 hours, wherein the sintering atmosphere is nitrogen; the third sintering process is as follows: heating the sample to 1100-1350 ℃ and preserving heat for 2-6 h, wherein the sintering atmosphere is hydrogen.
The invention has the beneficial effects that:
according to the method for improving the density of the tungsten-copper alloy, the pore filling solution is prepared, the tungsten-copper alloy rough blank is placed in the pore filling solution for soaking for a certain time, the solution is filled into the pores of the rough blank under the action of a capillary tube, and then the sample is dried and sintered. Through the three-step sintering process, various oxides at the pores can be reduced into Cu, W and Ni, so that the pores are filled and the compactness is improved. In addition, the addition of Ni can increase the activity of the powder, improve the flow property of Cu and the diffusion migration speed of Cu, and meanwhile, ni and Cu can form a Cu-Ni solid solution phase so that W has a certain solubility in the Cu-Ni phase to increase the interface structure between W and Cu, thereby further improving the compactness. The invention has simple process, can process alloy parts with complex shapes, has lower cost and high production efficiency, and is suitable for mass production.
Drawings
Fig. 1: microstructure morphology (200 times magnification) of tungsten-copper alloy sample prepared in example 3 of the present invention;
fig. 2: microstructure morphology (1000-fold magnification) of the tungsten-copper alloy sample prepared in example 3 of the present invention.
Detailed Description
The invention is further described below with reference to examples, which are merely illustrative and explanatory of the principles of the invention, and various modifications and additions may be made to the described embodiments by those skilled in the art, or similar thereto, without departing from the spirit of the invention or beyond the scope of the appended claims.
Example 1:
the method for improving the compactness of the tungsten-copper alloy specifically comprises the following steps:
s1, preparing a filling solution: cuNO is to 3 、H 28 N 6 O 41 W 12 The (ammonium metatungstate) is prepared into an aqueous solution with filled pores according to a certain proportion; wherein the raw material CuNO 3 、H 28 N 6 O 41 W 12 The weight ratio of (ammonium meta-tungstate) to deionized water is 5:5:90; the configuration process comprises respectively configuring CuNO according to the requirement of predetermined proportion 3 、H 28 N 6 O 41 W 12 Aqueous solution, then the two aqueous solutions are mixed.
S2, soaking a tungsten-copper alloy rough blank: placing the pre-mixed powder and the pressed tungsten-copper alloy rough blank into the pore filling solution prepared in the step S1 for soaking for 4 hours at the soaking temperature of 60 ℃; weighing analysis finds that the weight of the sample increases by 31%;
s3, sintering a tungsten copper rough blank: and (3) drying the tungsten-copper alloy rough blank sample after the soaking in the step (S2) in a drying box, and weighing and analyzing to find that the sample is only increased by 10.5% compared with the sample before the soaking due to evaporation of the water. Then placing the mixture in a sintering furnace for sectional sintering; the sintering adopts a continuous three-step sintering process, and the first-step sintering process comprises the following steps: heating the sample to 300 ℃ and preserving heat for 3 hours, wherein the sintering atmosphere is nitrogen; the second sintering process comprises the following steps: heating the sample to 700 ℃ and preserving heat for 1h, wherein the sintering atmosphere is nitrogen; the third sintering process is as follows: the sample was heated to 1300 ℃ and incubated for 4h with hydrogen as the sintering atmosphere.
After sintering, observing the prepared tungsten-copper alloy sample microstructure by using a scanning electron microscope, wherein W, cu is uniformly distributed and has no defects such as crack and pore; the compactness of the tungsten-copper alloy sample measured by the drainage method is as high as 99.1 percent.
Example 2:
the method for improving the compactness of the tungsten-copper alloy specifically comprises the following steps:
s1, preparing a filling solution: cuNO is to 3 、H 28 N 6 O 41 W 12 (ammonium meta-tungstate), niSO 4 Preparing an aqueous solution with filled pores according to a certain proportion; wherein the raw material CuNO 3 、H 28 N 6 O 41 W 12 (ammonium meta-tungstate), niSO 4 The weight ratio of deionized water is 8:5:3:84; the configuration process comprises respectively configuring CuNO according to the requirement of predetermined proportion 3 、H 28 N 6 O 41 W 12 、NiSO 4 Aqueous solutions, and then mixing the three aqueous solutions.
S2, soaking a tungsten-copper alloy rough blank: placing the pre-mixed powder and the pressed tungsten-copper alloy rough blank into the pore filling solution prepared in the step S1 for soaking for 6 hours at the soaking temperature of 60 ℃; weighing analysis finds that the weight of the sample increases by 38%;
s3, sintering a tungsten copper rough blank: and (3) drying the tungsten-copper alloy rough blank sample soaked in the step (S2) in a drying box, and weighing and analyzing to find that the weight of the sample is only increased by 12.3% compared with that of the sample before being soaked due to evaporation of the moisture. Then placing the mixture in a sintering furnace for sectional sintering; the sintering adopts a continuous three-step sintering process, and the first-step sintering process comprises the following steps: heating the sample to 350 ℃ and preserving heat for 3 hours, wherein the sintering atmosphere is nitrogen; the second sintering process comprises the following steps: heating the sample to 750 ℃ and preserving heat for 2 hours, wherein the sintering atmosphere is nitrogen; the third sintering process is as follows: the sample was heated to 1350 ℃ and incubated for 4h with hydrogen as the sintering atmosphere.
After sintering, observing the prepared tungsten-copper alloy sample microstructure by using a scanning electron microscope, wherein W, cu is uniformly distributed and has no defects such as crack and pore; the compactness of the tungsten-copper alloy sample measured by the drainage method is as high as 99.4 percent.
Example 3:
the method for improving the compactness of the tungsten-copper alloy specifically comprises the following steps:
s1, preparing a filling solution: cuNO is to 3 、H 28 N 6 O 41 W 12 (ammonium meta-tungstate), niSO 4 Preparing an aqueous solution with filled pores according to a certain proportion; wherein the raw material CuNO 3 、H 28 N 6 O 41 W 12 (ammonium meta-tungstate), niSO 4 The weight ratio of deionized water is 8:10:5:77; the configuration process comprises respectively configuring CuNO according to the requirement of predetermined proportion 3 、H 28 N 6 O 41 W 12 、NiSO 4 Aqueous solutions, and then mixing the three aqueous solutions.
S2, soaking a tungsten-copper alloy rough blank: placing the pre-mixed powder and the pressed tungsten-copper alloy rough blank into the pore filling solution prepared in the step S1 for soaking for 3 hours at the soaking temperature of 40 ℃; weighing analysis finds that the weight of the sample increases by 28%;
s3, sintering a tungsten copper rough blank: and (3) drying the tungsten-copper alloy rough blank sample after the soaking in the step (S2) in a drying box, and weighing and analyzing to find that the sample is only increased by 9.4% compared with the sample before the soaking due to evaporation of the water. Then placing the mixture in a sintering furnace for sectional sintering; the sintering adopts a continuous three-step sintering process, and the first-step sintering process comprises the following steps: heating the sample to 350 ℃ and preserving heat for 3 hours, wherein the sintering atmosphere is nitrogen; the second sintering process comprises the following steps: heating the sample to 800 ℃ and preserving heat for 2 hours, wherein the sintering atmosphere is nitrogen; the third sintering process is as follows: the sample was heated to 1350 ℃ and incubated for 6h with hydrogen as the sintering atmosphere.
And after sintering, observing the prepared tungsten-copper alloy sample microstructure by using a scanning electron microscope. FIG. 1 is a microstructure morphology (200 times magnification) of a tungsten copper alloy sample prepared in this example; fig. 2 is a microstructure morphology (magnified 1000 times) of the tungsten copper alloy sample prepared in this example. As shown in fig. 1 and 2, W, cu is found to be distributed uniformly, the tungsten particles are connected with each other and the original spherical shape is retained, the whole tungsten-copper interface is well bonded without defects such as crack and pore. And the compactness of the tungsten-copper alloy sample measured by a drainage method is as high as 99.7 percent.
Example 4:
a method for improving the compactness of a tungsten-copper alloy, which is basically the same as that of example 3, except that:
in this example, in step S1, cuNO is used as a raw material 3 、H 28 N 6 O 41 W 12 (ammonium meta-tungstate), niSO 4 The weight ratio of deionized water is 5:5:0:90. in the step S2, soaking the tungsten-copper alloy rough blank in a pore filling solution for 2 hours at 20 ℃; the weight gain of the sample was found to be 23% by weight analysis. In step S3, the dry water in the drying oven is evaporated, and the weighing analysis finds that the sample only increases by 6.8% compared with the sample before soaking. The subsequent continuous three-step sintering process is carried out, in the first step, the sample is heated to 280 ℃ and is kept for 1h; in the second step, heating the sample to 600 ℃ and preserving heat for 1h; in the third step, the sample is heated to 1100 ℃ and incubated for 2 hours.
After sintering, observing the prepared tungsten-copper alloy sample microstructure by using a scanning electron microscope, wherein W, cu is uniformly distributed and has no defects such as crack and pore; the compactness of the tungsten-copper alloy sample measured by the drainage method is as high as 98.9%.
Example 5:
a method for improving the compactness of a tungsten-copper alloy, which is basically the same as that of example 3, except that:
in this example, in step S1, cuNO is used as a raw material 3 、H 28 N 6 O 41 W 12 (ammonium meta-tungstate), niSO 4 The weight ratio of deionized water is 10:10:5:75. in the step S2, soaking the tungsten-copper alloy rough blank in a pore filling solution for 6 hours at the soaking temperature of 60 ℃; the weight gain of the sample was found to be 29% by weight analysis. In step S3, the dry water in the drying oven is evaporated, and the weighing analysis finds that the sample only increases by 10.3% compared with the sample before soaking. The subsequent continuous three-step sintering process is carried out, in the first step, the sample is heated to 420 ℃ and is kept for 3 hours; in the second step, heating the sample to 850 ℃ and preserving heat for 3 hours; in the third step, the sample was heated to 1350℃and incubated for 6h.
After sintering, observing the prepared tungsten-copper alloy sample microstructure by using a scanning electron microscope, wherein W, cu is uniformly distributed and has no defects such as crack and pore; the compactness of the tungsten-copper alloy sample measured by the drainage method is as high as 99.8 percent.
In examples 1-5, the tungsten-copper alloy sample material prepared by the method for improving the density of the tungsten-copper alloy has excellent high-density performance through detection. The invention relates to a method for improving the density of a tungsten-copper alloy, which comprises the steps of preparing a pore filling solution, placing a tungsten-copper alloy rough blank in the pore filling solution for soaking for a certain time, filling the solution into pores of the rough blank under the action of a capillary, then drying a sample, and drying water in the solution. The subsequent sintering process is critical and is divided into three steps, the first step of low-temperature sintering can decompose CuNO3 at the pores into CuO, the second step of medium-temperature sintering can decompose H28N6O41W12 and NiSO4 at the pores into WO3 and NiO, the oxide generated by the above can be uniformly dispersed at the pores, and the third step of sintering is performed at a temperature higher than the melting point of copper and in a reducing atmosphere (hydrogen) to reduce various oxides at the pores into Cu, W and Ni, so that the pores are filled and the compactness is improved. In addition, the addition of Ni can increase the activity of the powder, improve the flow property of Cu and the diffusion migration speed of Cu, and meanwhile, ni and Cu can form a Cu-Ni solid solution phase so that W has a certain solubility in the Cu-Ni phase to increase the interface structure between W and Cu, thereby further improving the compactness. The process is simple, can process aluminum alloy parts with complex shapes, has low cost and high production efficiency, and is suitable for large-scale production.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (2)
1. A method for improving the compactness of a tungsten-copper alloy, which is characterized by comprising the following steps:
s1, preparing a filling solution: cuNO is to 3 、H 28 N 6 O 41 W 12 、NiSO 4 Preparing an aqueous solution with filled pores according to a certain proportion;
s2, soaking a tungsten-copper alloy rough blank: placing the pre-mixed powder and the pressed tungsten-copper alloy rough blank into the pore filling solution prepared in the step S1 for soaking for 2-6 h at 20-60 ℃;
s3, sintering a tungsten copper rough blank: drying the tungsten copper alloy rough blank sample soaked in the step S2 in a drying box to remove water of the sample, and then placing the sample in a sintering furnace for sectional sintering; after sintering is finished, the whole process of improving the density of the tungsten-copper alloy can be completed;
the sintering adopts a continuous three-step sintering process, and the first-step sintering process comprises the following steps: heating the sample to 280-420 ℃ and preserving heat for 1-3 hours, wherein the sintering atmosphere is nitrogen; the second sintering process comprises the following steps: heating the sample to 600-850 ℃ and preserving heat for 1-3 hours, wherein the sintering atmosphere is nitrogen; the third sintering process is as follows: heating the sample to 1100-1350 ℃ and preserving heat for 2-6 h, wherein the sintering atmosphere is hydrogen.
2. A method for improving the compactness of a tungsten copper alloy according to claim 1, wherein in step S1, the raw material CuNO 3 、H 28 N 6 O 41 W 12 、NiSO 4 The weight ratio of the deionized water is (5-10): (5-10): (0-5): (75-90).
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|---|---|---|---|---|
| DE2712555A1 (en) * | 1977-03-22 | 1978-09-28 | Siemens Ag | Mfr. of sintered tungsten compact contg. silver and copper - by sintering the metal powders and impregnating with silver-copper alloy to form alloy used to mfr. electric contacts |
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