CN109128213B - Preparation method of silver-carbon tin oxide contact alloy - Google Patents
Preparation method of silver-carbon tin oxide contact alloy Download PDFInfo
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- CN109128213B CN109128213B CN201810936274.XA CN201810936274A CN109128213B CN 109128213 B CN109128213 B CN 109128213B CN 201810936274 A CN201810936274 A CN 201810936274A CN 109128213 B CN109128213 B CN 109128213B
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- 239000000956 alloy Substances 0.000 title claims abstract description 34
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 34
- -1 silver-carbon tin oxide Chemical compound 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 64
- 239000000243 solution Substances 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 39
- 239000011259 mixed solution Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 33
- IVQODXYTQYNJFI-UHFFFAOYSA-N oxotin;silver Chemical compound [Ag].[Sn]=O IVQODXYTQYNJFI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 23
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- 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
- 238000000227 grinding Methods 0.000 claims description 30
- 239000000047 product Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 12
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical compound [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 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
- 239000002245 particle Substances 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 description 8
- RRKGBEPNZRCDAP-UHFFFAOYSA-N [C].[Ag] Chemical compound [C].[Ag] RRKGBEPNZRCDAP-UHFFFAOYSA-N 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 4
- 230000004927 fusion Effects 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
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-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
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- UYKQQBUWKSHMIM-UHFFFAOYSA-N silver tungsten Chemical compound [Ag][W][W] UYKQQBUWKSHMIM-UHFFFAOYSA-N 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- 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
- C22C32/0084—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 carbon or graphite as the main non-metallic constituent
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- 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
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- 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
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
- H01H1/02376—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a preparation method of a silver-carbon tin oxide contact alloy, which comprises the following steps: preparation of Sn (NO)3)4And AgNO3Adding a polyvinylpyrrolidone solution and a sodium borohydride solution into the mixed solution A in sequence, 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 tin oxide composite powder by using the precipitation product, putting the silver tin oxide composite powder and graphite powder into a ball mill according to a ratio, performing ball milling and powder mixing, annealing to obtain uniformly mixed silver-carbon-tin oxide composite powder, and preparing the silver-carbon-tin oxide composite powder into the silver tin oxide carbon electrical contact alloy. 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-carbon tin oxide contact alloy.
Background
The AgC electric contact material is a common contact material in low-voltage electric equipment such as a circuit breaker, a relay, a change-over switch and a contactor.
At present, there are known silver carbon contact material patents: 1) a patent "a preparation method of a silver/graphite/graphene sliding electrical contact material" (application No. CN201710759776.5, publication No. CN107695356A, published No. 2018.02.16); 2) a patent of a preparation method of silver-plated graphene reinforced copper-based electric contact material (application number CN201610527507.1, publication number CN105950904A, published 2016.09.21); 3) a method for preparing a silver graphite electrical contact strip (application No. CN200910153565.2, publication No. CN101693955A, published as 2010.04.14); 4) the patent "a method for manufacturing silver-tungsten carbide-carbon electrical contact material" (application No. 200510024287.2, publication No. CN1658346, published japanese 2005.8.24).
Although the silver-carbon electrical contact alloy has good fusion welding resistance, good electrical conductivity and good temperature rise performance, the alloy has poor arc erosion resistance under the condition of more than medium current.
Disclosure of Invention
The invention aims to provide a preparation method of a silver tin oxycarbide contact alloy, which can improve the arc erosion resistance of the alloy.
The invention adopts the technical scheme that the preparation method of the silver carbon tin oxide contact alloy comprises the following steps:
step 1, preparation of Sn (NO)3)4And AgNO3The mixed solution A of (1);
step 2, adding a polyvinylpyrrolidone solution and a sodium borohydride solution into the mixed solution A in sequence, 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 tin oxide composite powder by using the precipitation product;
step 5, putting the silver tin oxide composite powder and the graphite powder into a ball mill according to a proportion for ball milling and mixing, and annealing to obtain uniformly mixed silver-carbon-tin oxide composite powder;
and 6, preparing the silver-carbon-tin oxide composite powder into the silver-carbon tin oxide electric contact alloy.
The present invention is also characterized in that,
the specific steps of the step 1 are as follows: firstly, adding tin particles into 60-80 mass percent of HNO3Fully dissolving in the solution to obtain 2mol/L Sn (NO)3)4A solution; then Sn (NO)3)4The solution is slowly added to 2mol/L AgNO3And (4) obtaining a mixed solution A in the aqueous solution.
In the step 2: the concentration of the polyvinylpyrrolidone solution is 0.6-1 mol/L, and the concentration of the sodium borohydride is 2-3 mol/L.
The step 3 specifically comprises the following steps: and (3) ultrasonically stirring the mixed solution B at 60 ℃ for 2-3 h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 2-4, and stirring for 1-3 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-tin oxide composite powder.
In the step 5: the mass fraction of the silver tin oxide composite powder is 60-80%, the mass fraction of the graphite powder is 20-40%, and the sum of the mass fractions of the silver tin oxide composite powder and the graphite 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, 10mm and 5mm respectively, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 15-20: 1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8-12 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: the silver-carbon-tin oxide composite powder is prepared into the silver-carbon tin oxide electric contact alloy by adopting the traditional pressing-sintering-extruding process.
The invention has the beneficial effects that:
the preparation method of the silver tin oxide with carbon oxide contact alloy adopts a sol-gel process, takes polyvinyl alcohol as a dispersing agent to control the size and the dispersibility of generated colloid, and simultaneously adopts sodium borohydride as a reducing agent to prepare silver tin oxide powder; the contact material has the advantages of both silver carbon and silver metal oxide, can ensure high fusion welding resistance and arc erosion resistance, and can also enable the contact alloy to achieve high electric conduction and heat conduction performance; the preparation method of the silver-carbon tin oxide contact alloy can save the silver consumption, reduce the product cost and simplify the process.
Drawings
Fig. 1 is an electron microscope image of an embodiment of a method for preparing a silver tin oxycarbide contact alloy of the 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-carbon tin oxide contact alloy, which is implemented according to the following steps:
step 1, preparation of Sn (NO)3)4And AgNO3The mixed solution A of (1);
firstly, adding tin particles into 60-80 mass percent of HNO3 solution for full dissolution to prepare 2mol/L Sn (NO)3)4A solution; then Sn (NO)3)4The solution is slowly added to 2mol/L AgNO3To the aqueous solution, a mixed solution A was obtained.
Step 2, adding a polyvinylpyrrolidone solution into the mixed solution A as a dispersing agent, uniformly stirring, adding a sodium borohydride solution serving as a reducing agent into the mixed solution A, and continuously and uniformly stirring to obtain a mixed solution B;
the concentration of the polyvinylpyrrolidone solution is 0.6-1 mol/L, and the concentration of the sodium borohydride is 2-3 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 50-70 ℃ for 2-3 h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 2-4, and stirring for 1-3 h after dropwise adding is completed until the precipitation is complete to obtain a precipitation product.
Step 4, preparing silver tin 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 500-600 ℃; and finally, taking out the powder obtained after calcination, grinding and refining to obtain the silver-tin oxide composite powder.
Step 5, mixing 60-80% of silver tin oxide composite powder and 20-40% of graphite powder, wherein the sum of the mass fractions of the silver tin oxide composite powder and the graphite powder is 100%; proportionally placing the mixture into a planetary ball mill for ball milling and powder mixing, and annealing the mixture in a vacuum atmosphere to obtain uniformly mixed silver-carbon-tin 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, 10mm and 5mm respectively, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 15-20: 1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8-12 h.
And 6, preparing the silver-carbon-tin oxide composite powder into the silver-carbon tin oxide electric contact alloy.
The method specifically comprises the following steps: the silver-carbon-tin oxide composite powder is prepared into the silver-carbon tin oxide electric contact alloy by adopting the traditional pressing-sintering-extruding process.
According to the preparation method of the silver tin oxide with carbon oxide contact alloy, the size and the dispersity of generated colloid are controlled by adopting a sol-gel process and polyvinyl alcohol as a dispersing agent, and the silver tin oxide powder is prepared by adopting sodium borohydride as a reducing agent; the contact material has the advantages of both silver carbon and silver metal oxide, can ensure high fusion welding resistance and arc erosion resistance, and can also enable the contact alloy to achieve high electric conduction and heat conduction performance; the preparation method of the silver-carbon tin oxide contact alloy can save the silver consumption, reduce the product cost and simplify the process.
As shown in fig. 1, tin dioxide having a black dotted morphology is uniformly distributed in the silver-carbon matrix, so that the ablation resistance and the fusion welding resistance of the alloy under the action of arc erosion can be effectively improved.
Example 1
Step 1, adding tin particles into HNO with the mass fraction of 80%3Fully dissolving in the solution to obtain 2mol/L Sn (NO)3)4A solution; then Sn (NO)3)4The solution is slowly added to 2mol/L AgNO3Obtaining a mixed solution A in the aqueous solution;
step 2, adding a polyvinylpyrrolidone solution with the concentration of 1mol/L into the mixed solution A, uniformly stirring, adding a sodium borohydride solution with the concentration of 3mol/L into the mixed solution A, and continuously and uniformly stirring to obtain a mixed solution B;
step 3, ultrasonically stirring the mixed solution B at 70 ℃ for 3h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 2, and stirring for 3h 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 70 ℃ 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 tin oxide composite powder;
step 5, mixing 80% of silver tin oxide composite powder and 20% of graphite powder; putting the mixture into a planetary ball mill according to a certain proportion for ball milling and powder mixing, and annealing the mixture in a vacuum atmosphere to obtain uniformly mixed silver-carbon-tin 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, 10mm and 5mm, the quantity ratio of the grinding balls to the materials is 2:3:1, the ball-milling rotation speed is 400r/min, and the ball-milling time is 8 hours;
step 6, preparing the silver-carbon-tin oxide composite powder by adopting the traditional pressing-sintering-extruding process to obtain the Ag70-C20-SnO210 silver tin oxycarbide electrical contact alloys.
Example 2
Step 1, adding tin particles into HNO with the mass fraction of 50%3Fully dissolving in the solution to obtain 2mol/L Sn (NO)3)4A solution; then Sn (NO)3)4The solution is slowly added to 2mol/L AgNO3Obtaining a mixed solution A in the aqueous solution;
step 2, adding a polyvinylpyrrolidone solution with the concentration of 0.8mol/L into the mixed solution A, stirring uniformly, adding a sodium borohydride 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 60 ℃ for 3 hours, dropwise adding ammonia water in the process to adjust the pH value of the solution to 3, and stirring for 2 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 500 ℃; finally, taking out the powder obtained after calcination, grinding and refining to obtain silver tin oxide composite powder;
step 5, mixing 70% of silver tin oxide composite powder and 30% of graphite powder; putting the mixture into a planetary ball mill according to a certain proportion for ball milling and powder mixing, and annealing the mixture in a vacuum atmosphere to obtain uniformly mixed silver-carbon-tin 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, 10mm and 5mm, 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;
step 6, preparing the silver-carbon-tin oxide composite powder by adopting the traditional pressing-sintering-extruding process to obtain the Ag62-C30-SnO28 silver tin oxycarbide electrical contact alloys.
Example 3
Step 1, adding tin particles into 60 mass percent of HNO3Fully dissolving in the solution to obtain 2mol/L Sn (NO)3)4A solution; then Sn (NO)3)4The solution is slowly added to 2mol/L AgNO3In aqueous solution to obtainMixing the solution A;
step 2, adding a polyvinylpyrrolidone solution with the concentration of 0.6mol/L into the mixed solution A as a dispersing agent, uniformly stirring, adding a sodium borohydride solution with the concentration of 2mol/L into the mixed solution A, and continuously and uniformly stirring to obtain a mixed solution B;
step 3, ultrasonically stirring the mixed solution B at 50 ℃ for 2h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 4, 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 tin oxide composite powder;
step 5, mixing the silver tin oxide composite powder with the mass fraction of 60% and the graphite powder with the mass fraction of 40%; putting the mixture into a planetary ball mill according to a certain proportion for ball milling and powder mixing, and annealing the mixture in a vacuum atmosphere to obtain uniformly mixed silver-carbon-tin 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, 10mm and 5mm, 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 12 hours;
step 6, preparing the silver-carbon-tin oxide composite powder by adopting the traditional pressing-sintering-extruding process to obtain the Ag55-C40-SnO25 silver tin oxycarbide electrical contact alloys.
Claims (7)
1. A preparation method of a silver tin oxycarbide contact alloy is characterized by comprising the following steps:
step 1, preparation of Sn (NO)3)4And AgNO3The mixed solution A of (1);
step 2, sequentially adding a polyvinylpyrrolidone solution and a sodium borohydride solution into the mixed solution A, and uniformly stirring to obtain a mixed solution B; the concentration of the polyvinylpyrrolidone solution is 0.6-1 mol/L, and the concentration of the sodium borohydride solution is 2-3 mol/L;
step 3, ultrasonically stirring the mixed solution B at 60 ℃ for 2-3 h, dropwise adding ammonia water in the process to adjust the pH value of the solution to 2-4, and stirring for 1-3 h after dropwise adding is finished until the precipitation is complete to obtain a precipitation product;
step 4, preparing silver tin oxide composite powder by using the precipitation product;
step 5, putting the silver tin oxide composite powder and the graphite powder into a ball mill according to a proportion for ball milling and mixing, and annealing to obtain uniformly mixed silver-carbon-tin oxide composite powder;
and 6, preparing the silver-carbon-tin oxide composite powder into the silver-carbon tin oxide electric contact alloy.
2. The method for preparing the silver tin oxycarbide contact alloy according to claim 1, wherein the specific steps in the step 1 are as follows: firstly, adding tin particles into 60-80 mass percent of HNO3Fully dissolving in the solution to obtain 2mol/L Sn (NO)3)4A solution; then adding said Sn (NO)3)4The solution is slowly added to 2mol/L AgNO3And (4) obtaining a mixed solution A in the aqueous solution.
3. The method for preparing the silver tin oxycarbide contact alloy according to claim 1, wherein the step 4 specifically comprises: 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-tin oxide composite powder.
4. The method of claim 1, wherein in step 5: the mass fraction of the silver tin oxide composite powder is 60-80%, the mass fraction of the graphite powder is 20-40%, and the sum of the mass fractions of the silver tin oxide composite powder and the graphite powder is 100%.
5. The method for preparing the silver tin oxycarbide contact alloy according to claim 1, wherein in the ball milling process of the step 5: the grinding balls are alumina grinding balls, the diameters of the grinding balls are 12mm, 10mm and 5mm respectively, the grinding balls are mixed according to the quantity ratio of 2:3:1, the ball-material ratio is 15-20: 1, the ball-milling rotating speed is 400r/min, and the ball-milling time is 8-12 h.
6. The method of claim 1, wherein in step 5: the annealing temperature is 500 ℃, and the annealing time is 2 h.
7. The method for preparing the silver tin oxycarbide contact alloy according to claim 1, wherein the step 6 specifically comprises the following steps: and preparing the silver-carbon-tin oxide composite powder by adopting a traditional pressing-sintering-extruding process to obtain the silver-carbon-tin oxide electrical contact alloy.
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