CN109055795B - Preparation method of silver tungsten carbide contact alloy containing copper oxide additive - Google Patents
Preparation method of silver tungsten carbide contact alloy containing copper oxide additive Download PDFInfo
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- CN109055795B CN109055795B CN201810935705.0A CN201810935705A CN109055795B CN 109055795 B CN109055795 B CN 109055795B CN 201810935705 A CN201810935705 A CN 201810935705A CN 109055795 B CN109055795 B CN 109055795B
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- UYKQQBUWKSHMIM-UHFFFAOYSA-N silver tungsten Chemical compound [Ag][W][W] UYKQQBUWKSHMIM-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 38
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 38
- 239000000956 alloy Substances 0.000 title claims abstract description 36
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 36
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000654 additive Substances 0.000 title claims abstract description 22
- 230000000996 additive effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 80
- 239000000243 solution Substances 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 239000011259 mixed solution Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 23
- WZSWPMDIARCYDN-UHFFFAOYSA-N copper;oxosilver Chemical compound [Ag].[Cu]=O WZSWPMDIARCYDN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010949 copper Substances 0.000 claims abstract description 21
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 11
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 9
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 9
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 14
- 239000002244 precipitate Substances 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000003628 erosive effect Effects 0.000 description 6
- 230000004927 fusion Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
- C22C32/0005—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 at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
The invention discloses a preparation method of a silver tungsten carbide contact alloy containing a copper oxide additive, which comprises the following steps: preparation of Cu (NO)3)2And AgNO3The mixed solution A is prepared by sequentially adding a polyvinylpyrrolidone solution and an ascorbic acid solution into the mixed solution A, uniformly stirring to obtain a mixed solution B, dropwise adding ammonia water into the mixed solution B, adjusting the pH value to obtain a precipitation product, preparing silver copper oxide composite powder by using the precipitation product, putting the silver copper oxide composite powder and tungsten carbide powder into a ball mill according to a ratio for ball milling and mixing, annealing to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder, and preparing the silver-tungsten carbide-copper oxide composite powder into the silver tungsten carbide electrical contact alloy containing the copper oxide additive. Can save silver consumption, reduce product cost and has simple process.
Description
Technical Field
The invention belongs to the technical field of alloy preparation methods, and relates to a preparation method of a silver tungsten carbide contact alloy containing a copper oxide additive.
Background
The AgWC electrical contact material is a silver-saving contact material popularized in China, and has good fusion welding resistance and arc erosion resistance to successfully replace AgC and AgW alloys, so that the AgWC electrical contact material is widely applied to various circuit breakers.
At present, there are two main processes for producing AgWC contact alloy at home and abroad, and when the weight percentage of WC is less than 30%, for example, AgWC20C3 and AgWC12C3 alloy are prepared, a powder extrusion-sintering process is usually adopted. For example: 1) patent "a method for manufacturing a silver-tungsten carbide-carbon electrical contact material" (application No. 200510024287.2, publication No. CN1658346, publication No. 2005.8.24); 2) the patent relates to a silver tungsten carbide graphite electrical contact and a production process thereof (application No. 201210220964.8, publication No. CN102737864, published Japanese 2012.10.17). When the WC weight percentage is more than 30%, such as AgW40, AgW50 and AgW55 alloy, an infiltration sintering process is generally adopted. For example: 3) document AgWC contact material for small circuit breaker (electrical material [ J ], 2004 (4)): 18-20); 4) the patent refers to the field of 'processes for preparing silver-tungsten carbide contact materials' (application No. CN201410711779.8, publication No. CN104384512A, published as 2015.03.04). When the weight percentage of WC in the AgWC alloy is less than 30%, the alloy can be manufactured by adopting a simpler powder extrusion-sintering process, but the arc ablation resistance and the temperature rise resistance of the obtained alloy are not ideal, and when the weight percentage of WC in the AgWC alloy is more than 30%, an infiltration sintering process is required, and although the alloy prepared by adopting the process has good arc erosion resistance, the process has the defects of complicated preparation process, complex process and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a silver tungsten carbide contact alloy containing a copper oxide additive, which can improve the arc erosion resistance of the alloy.
The invention adopts the technical scheme that the preparation method of the silver tungsten carbide contact alloy containing the copper oxide additive comprises the following steps:
step 1, preparing Cu (NO)3)2And AgNO3The mixed solution A of (1);
step 2, sequentially adding a polyvinylpyrrolidone solution and an ascorbic acid solution into the mixed solution A, and uniformly stirring to obtain a mixed solution B;
step 3, dropwise adding ammonia water into the mixed solution B and adjusting the pH value to obtain a precipitate;
step 4, preparing silver copper oxide composite powder by using the precipitation product;
step 5, putting the silver copper oxide composite powder and the tungsten carbide powder into a ball mill in proportion for ball milling and powder mixing, and annealing to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder;
and 6, preparing the silver-tungsten carbide-copper oxide composite powder into the silver-tungsten carbide electrical contact alloy containing the copper oxide additive.
The present invention is also characterized in that,
the specific steps of the step 1 are as follows: firstly, adding Cu powder into HNO with the mass fraction of 40-60%3Fully dissolving in the solution to obtain 1mol/L Cu (NO)3)2A solution; then adding Cu (NO)3)2The solution was slowly added to a 1mol/L aqueous solution of AgNO3 to obtain a mixed solution A.
In the step 2: the concentration of the polyvinylpyrrolidone solution is 0.4-6 mol/L, and the concentration of the ascorbic acid is 1.5-2.5 mol/L.
The step 3 specifically comprises the following steps: and ultrasonically stirring the mixed solution B at 55-75 ℃ for 1-2 h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 8-10, and stirring for 1-2 h after dropwise adding is completed until the precipitation is complete to obtain a precipitation product.
The step 4 specifically comprises the following steps: putting the precipitate product into a vacuum drying oven, and drying at 70-90 ℃ to obtain dry powder; then, putting the dried powder into a muffle furnace, and calcining for 2-4 h at 500-650 ℃; and finally, taking out the powder obtained after calcination, grinding and refining to obtain the silver-copper oxide composite powder.
In the step 5: the mass fraction of the silver-copper oxide composite powder is 70-85%, the mass fraction of the tungsten carbide powder is 15-30%, and the sum of the mass fractions of the silver-copper oxide composite powder and the tungsten carbide powder is 100%.
Step 5, in the ball milling process: the grinding balls are alumina grinding balls, the diameters of the grinding balls are 12mm, 8mm and 6mm respectively, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 12-20: 1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8-10 h.
In the step 5: the annealing temperature is 500 ℃, and the annealing time is 2 h.
The step 6 specifically comprises the following steps: and preparing the silver-tungsten carbide-copper oxide composite powder by adopting a pressing-sintering-extruding process to obtain the silver-tungsten carbide electrical contact alloy containing the copper oxide additive.
The invention has the beneficial effects that:
the preparation method of the silver tungsten carbide contact alloy containing the copper oxide additive adopts a sol-gel process, takes polyvinylpyrrolidone as a dispersing agent to control the size and the dispersibility of generated colloid, and simultaneously adopts citric acid as a reducing agent to prepare silver copper oxide powder; the contact material has the advantages of high fusion welding resistance and arc erosion resistance, and the contact alloy achieves the purposes of high electric conductivity and heat conductivity and easy processing and forming; the preparation method of the silver tungsten carbide contact alloy containing the copper oxide additive can save the silver consumption, reduce the product cost and has simple process.
Drawings
FIG. 1 is an electron micrograph of an embodiment of a method of making a silver tungsten carbide contact alloy containing a copper oxide additive according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a silver tungsten carbide contact alloy containing a copper oxide additive, which is implemented according to the following steps:
step 1, preparing Cu (NO)3)2And AgNO3The mixed solution A of (1);
firstly, adding Cu powder into HNO with the mass fraction of 40-60%3Fully dissolving in the solution to obtain 1mol/L Cu (NO)3)2A solution; then adding Cu (NO)3)2The solution is slowly added to 1mol/L AgNO3And (4) obtaining a mixed solution A in the aqueous solution.
Step 2, adding a polyvinylpyrrolidone solution into the mixed solution A as a dispersing agent, uniformly stirring, adding an ascorbic acid solution into the mixed solution A as a reducing agent, and continuously and uniformly stirring to obtain a mixed solution B;
the concentration of the polyvinylpyrrolidone solution is 0.4-0.6 mol/L, and the concentration of the ascorbic acid is 1.5-2.5 mol/L.
Step 3, dropwise adding ammonia water into the mixed solution B and adjusting the pH value to obtain a precipitate;
the method specifically comprises the following steps: and ultrasonically stirring the mixed solution B at 55-75 ℃ for 1-2 h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 8-10, and stirring for 1-2 h after dropwise adding is completed until the precipitation is complete to obtain a precipitation product.
Step 4, preparing silver copper oxide composite powder by using the precipitation product;
the method specifically comprises the following steps: putting the precipitate product into a vacuum drying oven, and drying at 70-90 ℃ until water is evaporated to obtain dry powder; then, putting the dried powder into a muffle furnace, and calcining for 2-4 h at 500-650 ℃; and finally, taking out the powder obtained after calcination, grinding and refining to obtain the silver-copper oxide composite powder.
Step 5, mixing 70-85% of silver-copper oxide composite powder and 15-30% of tungsten carbide powder, wherein the sum of the mass fractions of the silver-copper oxide composite powder and the tungsten carbide powder is 100%; proportionally placing the powder into a planetary ball mill for ball milling and mixing, and annealing in a vacuum atmosphere to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder, wherein the annealing temperature is 500 ℃ and the annealing time is 2 hours.
In the ball milling process: the grinding balls are alumina grinding balls, the diameters of the grinding balls are 12mm, 8mm and 6mm respectively, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 12-20: 1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8-10 h.
And 6, preparing the silver-tungsten carbide-copper oxide composite powder into the silver-tungsten carbide electrical contact alloy containing the copper oxide additive.
The method specifically comprises the following steps: and preparing the silver-tungsten carbide-copper oxide composite powder by adopting a pressing-sintering-extruding process to obtain the silver-tungsten carbide electrical contact alloy containing the copper oxide additive.
According to the preparation method of the silver tungsten carbide contact alloy containing the copper oxide additive, the polyvinylpyrrolidone is used as the dispersing agent by adopting the sol-gel process to control the size and the dispersibility of generated colloid, and the citric acid is used as the reducing agent to prepare silver copper oxide powder; the contact material has the advantages of high fusion welding resistance and arc erosion resistance, and the contact alloy achieves the purposes of high electric conductivity and heat conductivity and easy processing and forming; the preparation method of the silver tungsten carbide contact alloy containing the copper oxide additive can save the silver consumption, reduce the product cost and has simple process.
As shown in FIG. 1, the oxide structure in the alloy is uniformly distributed, and the particles are fine, so that the fusion welding resistance and the arc erosion resistance are obviously improved.
Example 1
Step 1, adding Cu powder into HNO with the mass fraction of 40%3Fully dissolving in the solution to obtain 1mol/L Cu (NO)3)2A solution; then adding Cu (NO)3)2The solution is slowly added to 1mol/L AgNO3Obtaining a mixed solution A in the aqueous solution;
step 2, adding a polyvinylpyrrolidone solution with the concentration of 0.4mol/L into the mixed solution A, stirring uniformly, adding an ascorbic acid solution with the concentration of 1.5mol/L into the mixed solution A, and continuously stirring uniformly to obtain a mixed solution B;
step 3, ultrasonically stirring the mixed solution B at 55 ℃ for 1h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 8, and stirring for 1h after dropwise adding is finished until the precipitation is complete to obtain a precipitation product;
step 4, putting the precipitate product into a vacuum drying oven, and drying at 90 ℃ until water is evaporated to obtain dry powder; then putting the dried powder into a muffle furnace, and calcining for 2 hours at 500 ℃; finally, taking out the powder obtained after calcination, grinding and refining to obtain silver-copper oxide composite powder;
step 5, mixing 85% of silver-copper oxide composite powder and 15% of tungsten carbide powder; putting the powder into a planetary ball mill in proportion for ball milling and mixing, and annealing in a vacuum atmosphere to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder, wherein the annealing temperature is 500 ℃ and the annealing time is 2 hours;
in the ball milling process: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 6mm, the grinding balls are proportioned according to the quantity ratio of 2:3:1, the ball-material ratio is 12:1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8 hours;
and step 6, preparing the silver-tungsten carbide-copper oxide composite powder by adopting a pressing-sintering-extruding process to obtain the silver-tungsten carbide electrical contact alloy containing the copper oxide additive and containing Ag82-WC15-CuO 3.
Example 2
Step 1, adding Cu powder into HNO with the mass fraction of 50%3Fully dissolving in the solution to obtain 1mol/L Cu (NO)3)2A solution; then adding Cu (NO)3)2The solution is slowly added to 1mol/L AgNO3Obtaining a mixed solution A in the aqueous solution;
step 2, adding a polyvinylpyrrolidone solution with the concentration of 0.5mol/L into the mixed solution A, stirring uniformly, adding an ascorbic acid solution with the concentration of 2mol/L into the mixed solution A, and continuously stirring uniformly to obtain a mixed solution B;
step 3, ultrasonically stirring the mixed solution B at 65 ℃ for 2 hours, dropwise adding ammonia water in the process to adjust the pH value of the solution to 8.5, and stirring for 1.5 hours after dropwise adding is finished until the precipitation is complete to obtain a precipitation product;
step 4, putting the precipitate product into a vacuum drying oven, and drying at 80 ℃ until water is evaporated to obtain dry powder; then putting the dried powder into a muffle furnace, and calcining for 4 hours at 600 ℃; finally, taking out the powder obtained after calcination, grinding and refining to obtain silver-copper oxide composite powder;
step 5, mixing 80% of silver copper oxide composite powder and 20% of tungsten carbide powder; putting the powder into a planetary ball mill in proportion for ball milling and mixing, and annealing in a vacuum atmosphere to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder, wherein the annealing temperature is 500 ℃ and the annealing time is 2 hours;
in the ball milling process: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 6mm, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 18:1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 10 hours;
and step 6, preparing the silver-tungsten carbide-copper oxide composite powder by adopting a pressing-sintering-extruding process to obtain the silver-tungsten carbide electrical contact alloy containing the copper oxide additive and containing Ag72-WC20-CuO 8.
Example 3
Step 1, adding Cu powder into 60 mass percent of HNO3Fully dissolving in the solution to obtain 1mol/L Cu (NO)3)2A solution; then adding Cu (NO)3)2The solution is slowly added to 1mol/L AgNO3Obtaining a mixed solution A in the aqueous solution;
step 2, adding a polyvinylpyrrolidone solution with the concentration of 0.6mol/L into the mixed solution A, stirring uniformly, adding an ascorbic acid solution with the concentration of 2.5mol/L into the mixed solution A, and continuously stirring uniformly to obtain a mixed solution B;
step 3, ultrasonically stirring the mixed solution B at 75 ℃ for 2h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 10, and stirring for 2h after dropwise adding is finished until the precipitation is complete to obtain a precipitation product;
step 4, putting the precipitate product into a vacuum drying oven, and drying at 90 ℃ until water is evaporated to obtain dry powder; then putting the dried powder into a muffle furnace, and calcining for 4 hours at 650 ℃; finally, taking out the powder obtained after calcination, grinding and refining to obtain silver-copper oxide composite powder;
step 5, mixing 70% of silver-copper oxide composite powder and 30% of tungsten carbide powder; putting the powder into a planetary ball mill in proportion for ball milling and mixing, and annealing in a vacuum atmosphere to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder, wherein the annealing temperature is 500 ℃ and the annealing time is 2 hours;
in the ball milling process: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 6mm, the grinding balls are proportioned according to the quantity ratio of 2:3:1, the ball-material ratio is 20:1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 10 hours;
and step 6, preparing the silver-tungsten carbide-copper oxide composite powder by adopting a pressing-sintering-extruding process to obtain the silver-tungsten carbide electrical contact alloy containing the copper oxide additive and containing Ag60-WC30-CuO 10.
Claims (2)
1. A preparation method of a silver tungsten carbide contact alloy containing a copper oxide additive is characterized by comprising the following steps:
step 1, adding Cu powder into HNO with the mass fraction of 40-60%3Fully dissolving in the solution to obtain 1mol/L Cu (NO)3)2A solution; then adding the Cu (NO)3)2Slowly adding the solution into 1mol/L AgNO3 aqueous solution to obtain mixed solution A;
step 2, sequentially adding a polyvinylpyrrolidone solution with the concentration of 0.4-6 mol/L and an ascorbic acid solution with the concentration of 1.5-2.5 mol/L into the mixed solution A, and uniformly stirring to obtain a mixed solution B;
step 3, ultrasonically stirring the mixed solution B at 55-75 ℃ for 1-2 hours, dropwise adding ammonia water in the process to adjust the pH value of the solution to 8-10, and stirring for 1-2 hours after dropwise adding is finished until the precipitation is complete to obtain a precipitation product;
step 4, putting the precipitation product into a vacuum drying oven, and drying at 70-90 ℃ to obtain dry powder; then, putting the dried powder into a muffle furnace, and calcining for 2-4 h at 500-650 ℃; finally, taking out the powder obtained after calcination, grinding and refining to obtain silver-copper oxide composite powder;
step 5, putting the silver copper oxide composite powder with the mass fraction of 70-85% and the tungsten carbide powder with the mass fraction of 15-30% into a ball mill according to a proportion for ball milling and mixing, wherein the sum of the mass fractions of the silver copper oxide composite powder and the tungsten carbide powder is 100%; annealing at 500 ℃ for 2h to obtain uniformly mixed silver-tungsten carbide-copper oxide composite powder;
and 6, preparing the silver-tungsten carbide-copper oxide composite powder by adopting a pressing-sintering-extruding process to obtain the silver-tungsten carbide electrical contact alloy containing the copper oxide additive.
2. The method of claim 1, wherein the ball milling process of step 5 comprises: the grinding balls are alumina grinding balls, the diameters of the grinding balls are 12mm, 8mm and 6mm respectively, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 12-20: 1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8-10 h.
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|---|---|---|---|---|
| JPS5688209A (en) * | 1979-12-21 | 1981-07-17 | Tokyo Shibaura Electric Co | Electric contactor |
| JP2653486B2 (en) * | 1988-08-19 | 1997-09-17 | 株式会社東芝 | Contact material for vacuum valve |
| CN1658346A (en) * | 2005-03-10 | 2005-08-24 | 上海大学 | Manufacturing method of silver-tungsten carbide-carbon electrical contact material |
| CN106807953B (en) * | 2017-01-23 | 2018-07-10 | 西安工程大学 | A kind of preparation method of tin oxide disperse enhancing silver-based electric contact alloy |
| CN106876199B (en) * | 2017-01-23 | 2018-10-02 | 西安工程大学 | A kind of preparation method of the siller tin oxide alloy as electric contact material of even tissue |
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2018
- 2018-08-16 CN CN201810935705.0A patent/CN109055795B/en active Active
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| CN109055795A (en) | 2018-12-21 |
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