CN109055795A - A kind of preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation - Google Patents
A kind of preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation Download PDFInfo
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- CN109055795A CN109055795A CN201810935705.0A CN201810935705A CN109055795A CN 109055795 A CN109055795 A CN 109055795A CN 201810935705 A CN201810935705 A CN 201810935705A CN 109055795 A CN109055795 A CN 109055795A
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- 239000010949 copper Substances 0.000 title claims abstract description 60
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 48
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 40
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 38
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 32
- 239000000956 alloy Substances 0.000 title claims abstract description 32
- 239000000654 additive Substances 0.000 title claims abstract description 31
- 230000003647 oxidation Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 42
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- WZSWPMDIARCYDN-UHFFFAOYSA-N copper;oxosilver Chemical compound [Ag].[Cu]=O WZSWPMDIARCYDN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 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 20
- 239000008187 granular material Substances 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 18
- UYKQQBUWKSHMIM-UHFFFAOYSA-N silver tungsten Chemical compound [Ag][W][W] UYKQQBUWKSHMIM-UHFFFAOYSA-N 0.000 claims abstract description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 10
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 10
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 10
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 9
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 238000003701 mechanical milling Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 abstract description 6
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 4
- 238000010891 electric arc Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- QVQPKRJIEDPZIN-UHFFFAOYSA-N [C].[W].[Ag] Chemical compound [C].[W].[Ag] QVQPKRJIEDPZIN-UHFFFAOYSA-N 0.000 description 1
- MEOSMFUUJVIIKB-UHFFFAOYSA-N [W].[C] Chemical compound [W].[C] MEOSMFUUJVIIKB-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation methods of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation, comprising the following steps: preparation Cu (NO3)2And AgNO3Mixed solution A, successively polyvinylpyrrolidonesolution solution is added in mixed solution A, ascorbic acid solution, and it stirs evenly, obtain mixed solution B, ammonium hydroxide is added dropwise into mixed solution B and adjusts pH value, obtain precipitated product, silver copper oxide composite granule is prepared using precipitated product, silver copper oxide composite granule and tungsten carbide powder are put into proportion in ball mill and carry out the mixed powder of ball milling, uniformly mixed silver-tungsten carbide-oxidation copper composite powders are obtained after annealing, silver-tungsten carbide-oxidation copper composite powders are prepared into the silver-colored tungsten carbide alloy as electric contact material of the copper additives containing oxidation.Silver consuming amount can be saved, product cost is reduced, technical process is simple.
Description
Technical field
The invention belongs to alloy preparation method technical fields, are related to a kind of silver-colored tungsten carbide contactor of copper additives containing oxidation
The preparation method of gold.
Background technique
AgWC electrical contact material be China promote section silver type contact material, due to its have well resistance fusion welding and
Resistance to arc erosion and success instead of AgC, AgW alloy, have a wide range of applications in all kinds of breakers.
At present both at home and abroad there are mainly two types of the techniques of production AgWC contact alloy, when WC weight percent is less than 30%,
AgWC20C3, AgWC12C3 alloy are such as prepared, powder extruding-sintering process is generallyd use.Such as: 1) patent " a kind of silver-carbonization
Tungsten-carbon electrical contact material manufacturing method " (application number 200510024287.2, publication number CN1658346, publication date
2005.8.24)；2) patent " a kind of silver tungsten carbon graphite electric contact terminal and its production technology " (application number 201210220964.8, it is public
The number of opening CN102737864, publication date 2012.10.17).When WC weight percent is greater than 30%, such as preparation AgW40, AgW50,
AgW55 alloy generallys use melting infiltration sintering technique.Such as: 3) document " AgWC Contact Material Used in Miniature Circuit Breaker " (electrical material
[J], 2004 (4): 18-20)；4) patent " a kind of preparation method of silver-tungsten carbide contact material " (application number
CN201410711779.8, publication number CN104384512A, publication date 2015.03.04).When WC weight percent in AgWC alloy
When than less than 30%, although can be manufactured using relatively simple powder extruding-sintering process, gained alloy arc resistant
Ablation property and temperature rise model are undesirable, and in AgWC alloy WC weight percent be greater than 30% when, it is necessary to using infiltration burn
Knot technique, although having good anti electric arc corrosion performance using alloy obtained by this technique, which, which exists, was prepared
The disadvantages of journey is cumbersome, complex process.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation, can close
The raising anti electric arc corrosion performance of gold.
The technical scheme adopted by the invention is that a kind of preparation side of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation
Method, comprising the following steps:
Step 1, preparation Cu (NO3)2And AgNO3Mixed solution A；
Successively polyvinylpyrrolidonesolution solution, ascorbic acid solution is added in step 2 in mixed solution A, and stirs equal
It is even, obtain mixed solution B；
Ammonium hydroxide is added dropwise into mixed solution B and adjusts pH value for step 3, obtains precipitated product；
Step 4 prepares silver copper oxide composite granule using precipitated product；
Silver copper oxide composite granule and tungsten carbide powder are put into the mixed powder of progress ball milling in ball mill by step 5 in proportion, are moved back
Uniformly mixed silver-tungsten carbide-oxidation copper composite powders are obtained after fire processing；
Step 6, the silver-colored tungsten carbide that silver-tungsten carbide-oxidation copper composite powders are prepared into the copper additives containing oxidation are in electrical contact
Alloy.
The features of the present invention also characterized in that
The specific steps of step 1 are as follows: Cu powder is first added to the HNO that mass fraction is 40%~60%3In solution sufficiently
Cu (the NO of 1mol/L is made in dissolution3)2Solution；Then by Cu (NO3)2Solution is slowly added into the AgNO3 aqueous solution of 1mol/L
In, obtain mixed solution A.
In step 2: the concentration of polyvinylpyrrolidonesolution solution is 0.4~6mol/L, the concentration of ascorbic acid is 1.5~
2.5mol/L。
Step 3 specifically: mixed solution B is carried out to ultrasonic wave at 55~75 DEG C and stirs 1~2h, and is led in this process
Dropwise addition ammonium hydroxide is crossed to adjust solution ph to 8~10,1~2h is stirred for after being added dropwise to complete, is produced until precipitating completely, obtains precipitating
Object.
Step 4 specifically: first precipitated product is put into vacuum oven, obtains dry powder after dry at 70~90 DEG C
End；Then dry powder is put into Muffle furnace, 2~4h is calcined at 500~650 DEG C；The powder that will finally be obtained after calcining
Grinding refinement is taken out, silver copper oxide composite granule is obtained.
In step 5: the mass fraction of silver copper oxide composite granule is 70%~85%, and the mass fraction of tungsten carbide powder is
15%~30%, the sum of mass fraction of the two is 100%.
In step 5 mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 8mm, 6mm, and presses 2:3:1
Quantitative proportion, ratio of grinding media to material be 12~20:1, rotational speed of ball-mill 400r/min, Ball-milling Time be 8~10h.
In step 5: annealing temperature is 500 DEG C, annealing time 2h.
In step 6 specifically: be prepared into silver-tungsten carbide-oxidation copper composite powders using compacting-sintering-extrusion process
To the silver-colored tungsten carbide alloy as electric contact material of the copper additives containing oxidation.
The beneficial effects of the present invention are:
The preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation of the invention, use sol gel process with
Polyvinylpyrrolidone is dispersing agent, to control the size and dispersibility that generate colloid, while using citric acid as reducing agent,
Prepare silver copper oxide powder；The advantages of two kinds of contact materials of silver-colored carbon and siluer metal oxide can be had both simultaneously, touching was both can guarantee
Head material anti-melting welding with higher, anti electric arc corrosion performance, while contact alloy can be made to reach higher conductive, thermal conductivity again
Energy, purpose easily processed into type；The preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation of the invention, can save
Silver consuming amount is saved, product cost is reduced, technical process is simple.
Detailed description of the invention
Fig. 1 is a kind of electricity of the embodiment of the preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation of the present invention
Mirror figure.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation of the present invention, specifically according to the following steps
Implement:
Step 1, preparation Cu (NO3)2And AgNO3Mixed solution A；
Cu powder is first added to the HNO that mass fraction is 40%~60%3It is sufficiently dissolved in solution, the Cu of 1mol/L is made
(NO3)2Solution；Then by Cu (NO3)2Solution is slowly added into the AgNO of 1mol/L3In aqueous solution, mixed solution A is obtained.
Step 2, in mixed solution A be added polyvinylpyrrolidonesolution solution as dispersing agent, after mixing evenly, then to its
Middle addition ascorbic acid solution is stirred evenly as reducing agent, and constantly, obtains mixed solution B；
The concentration of polyvinylpyrrolidonesolution solution is 0.4~0.6mol/L, and the concentration of ascorbic acid is 1.5~2.5mol/
L。
Ammonium hydroxide is added dropwise into mixed solution B and adjusts pH value for step 3, obtains precipitated product；
Specifically: mixed solution B is carried out to ultrasonic wave at 55~75 DEG C and stirs 1~2h, and passes through drop in this process
Add ammonium hydroxide to adjust solution ph to 8~10, is stirred for 1~2h after being added dropwise to complete, until precipitating is completely, obtains precipitated product.
Step 4 prepares silver copper oxide composite granule using precipitated product；
Specifically: first precipitated product is put into vacuum oven, is obtained in 70~90 DEG C of dryings until moisture evaporation
Dry powder；Then dry powder is put into Muffle furnace, 2~4h is calcined at 500~650 DEG C；It will finally be obtained after calcining
The powder arrived takes out grinding refinement, obtains silver copper oxide composite granule.
Step 5, the silver copper oxide composite granule for being 70%~85% by mass fraction and mass fraction are 15%~30%
Tungsten carbide powder, the sum of mass fraction of the two be 100%；It is put into planetary ball mill in proportion and carries out the mixed powder of ball milling,
Uniformly mixed silver-tungsten carbide-oxidation copper composite powders, annealing temperature 500 are obtained in vacuum atmosphere, after annealing
DEG C, annealing time 2h.
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 8mm, 6mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material are 12~20:1, and rotational speed of ball-mill 400r/min, Ball-milling Time is 8~10h.
Step 6, the silver-colored tungsten carbide that silver-tungsten carbide-oxidation copper composite powders are prepared into the copper additives containing oxidation are in electrical contact
Alloy.
Specifically: silver-tungsten carbide-oxidation copper composite powders are prepared using compacting-sintering-extrusion process containing oxidation
The silver-colored tungsten carbide alloy as electric contact material of copper additives.
In the above manner, the preparation method of the silver-colored tungsten carbide contact alloy of the copper additives of the invention containing oxidation, uses
Sol gel process to control the size and dispersibility that generate colloid, while using lemon using polyvinylpyrrolidone as dispersing agent
Lemon acid prepares silver copper oxide powder as reducing agent；Two kinds of contact materials of silver-colored carbon and siluer metal oxide can be had both simultaneously
Advantage not only can guarantee contact material anti-melting welding with higher, anti electric arc corrosion performance, but can make contact alloy reach compared with
High conduction, heating conduction, purpose easily processed into type；The silver-colored tungsten carbide contact alloy of the copper additives containing oxidation of the invention
Preparation method, can save silver consuming amount, reduce product cost, technical process is simple.
As shown in Figure 1, alloy subscale Tissue distribution is uniform, particle is tiny, thus resistance fusion welding and arc resistant are invaded
Corrosion can significantly improve.
Embodiment 1
Step 1, first by Cu powder be added to mass fraction be 40% HNO3It is sufficiently dissolved in solution, the Cu of 1mol/L is made
(NO3)2Solution；Then by Cu (NO3)2Solution is slowly added into the AgNO of 1mol/L3In aqueous solution, mixed solution A is obtained；
Step 2, addition concentration is 0.4mol/L polyvinylpyrrolidonesolution solution in mixed solution A, after mixing evenly, then
The ascorbic acid solution of 1.5mol/L is added thereto, and constantly stirs evenly, obtains mixed solution B；
Step 3, mixed solution B is carried out at 55 DEG C ultrasonic wave stirring 1h, and in this process by be added dropwise ammonium hydroxide with
Solution ph is adjusted to 8,1h is stirred for after being added dropwise to complete, until precipitating is completely, obtains precipitated product；
Precipitated product is first put into vacuum oven by step 4, in 90 DEG C of dryings, until moisture evaporates, is obtained dry
Powder；Then dry powder is put into Muffle furnace, calcines 2h at 500 DEG C；Finally the powder obtained after calcining taking-up is ground
Levigateization obtains silver copper oxide composite granule；
The tungsten carbide powder that step 5, the silver copper oxide composite granule for being 85% by mass fraction and mass fraction are 15%；
It is put into planetary ball mill in proportion and carries out the mixed powder of ball milling, uniformly mixed silver-is obtained in vacuum atmosphere, after annealing
Tungsten carbide-oxidation copper composite powders, annealing temperature are 500 DEG C, annealing time 2h；
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 8mm, 6mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material 12:1, rotational speed of ball-mill 400r/min, Ball-milling Time 8h；
Step 6, silver-tungsten carbide-oxidation copper composite powders are used compacting-sintering-extrusion process be prepared ingredient for
The silver-colored tungsten carbide alloy as electric contact material of the copper additives containing oxidation of Ag82-WC15-CuO3.
Embodiment 2
Step 1, first by Cu powder be added to mass fraction be 50% HNO3It is sufficiently dissolved in solution, the Cu of 1mol/L is made
(NO3)2Solution；Then by Cu (NO3)2Solution is slowly added into the AgNO of 1mol/L3In aqueous solution, mixed solution A is obtained；
Step 2, addition concentration is 0.5mol/L polyvinylpyrrolidonesolution solution in mixed solution A, after mixing evenly, then
The ascorbic acid solution of 2mol/L is added thereto, and constantly stirs evenly, obtains mixed solution B；
Step 3, mixed solution B is carried out at 65 DEG C ultrasonic wave stirring 2h, and in this process by be added dropwise ammonium hydroxide with
Solution ph is adjusted to 8.5,1.5h is stirred for after being added dropwise to complete, until precipitating is completely, obtains precipitated product；
Precipitated product is first put into vacuum oven by step 4, in 80 DEG C of dryings, until moisture evaporates, is obtained dry
Powder；Then dry powder is put into Muffle furnace, calcines 4h at 600 DEG C；Finally the powder obtained after calcining taking-up is ground
Levigateization obtains silver copper oxide composite granule；
The tungsten carbide powder that step 5, the silver copper oxide composite granule for being 80% by mass fraction and mass fraction are 20%；
It is put into planetary ball mill in proportion and carries out the mixed powder of ball milling, uniformly mixed silver-is obtained in vacuum atmosphere, after annealing
Tungsten carbide-oxidation copper composite powders, annealing temperature are 500 DEG C, annealing time 2h；
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 8mm, 6mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material 18:1, rotational speed of ball-mill 400r/min, Ball-milling Time 10h；
Step 6, silver-tungsten carbide-oxidation copper composite powders are used compacting-sintering-extrusion process be prepared ingredient for
The silver-colored tungsten carbide alloy as electric contact material of the copper additives containing oxidation of Ag72-WC20-CuO8.
Embodiment 3
Step 1, first by Cu powder be added to mass fraction be 60% HNO3It is sufficiently dissolved in solution, the Cu of 1mol/L is made
(NO3)2Solution；Then by Cu (NO3)2Solution is slowly added into the AgNO of 1mol/L3In aqueous solution, mixed solution A is obtained；
Step 2, addition concentration is 0.6mol/L polyvinylpyrrolidonesolution solution in mixed solution A, after mixing evenly, then
The ascorbic acid solution of 2.5mol/L is added thereto, and constantly stirs evenly, obtains mixed solution B；
Step 3, mixed solution B is carried out at 75 DEG C ultrasonic wave stirring 2h, and in this process by be added dropwise ammonium hydroxide with
Solution ph is adjusted to 10,2h is stirred for after being added dropwise to complete, until precipitating is completely, obtains precipitated product；
Precipitated product is first put into vacuum oven by step 4, in 90 DEG C of dryings, until moisture evaporates, is obtained dry
Powder；Then dry powder is put into Muffle furnace, calcines 4h at 650 DEG C；Finally the powder obtained after calcining taking-up is ground
Levigateization obtains silver copper oxide composite granule；
The tungsten carbide powder that step 5, the silver copper oxide composite granule for being 70% by mass fraction and mass fraction are 30%；
It is put into planetary ball mill in proportion and carries out the mixed powder of ball milling, uniformly mixed silver-is obtained in vacuum atmosphere, after annealing
Tungsten carbide-oxidation copper composite powders, annealing temperature are 500 DEG C, annealing time 2h；
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 8mm, 6mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material 20:1, rotational speed of ball-mill 400r/min, Ball-milling Time 10h；
Step 6, silver-tungsten carbide-oxidation copper composite powders are used compacting-sintering-extrusion process be prepared ingredient for
The silver-colored tungsten carbide alloy as electric contact material of the copper additives containing oxidation of Ag60-WC30-CuO10.
Claims (9)
1. a kind of preparation method of the silver-colored tungsten carbide contact alloy of the copper additives containing oxidation, which comprises the following steps:
Step 1, preparation Cu (NO3)2And AgNO3Mixed solution A；
Successively polyvinylpyrrolidonesolution solution, ascorbic acid solution is added in step 2 in the mixed solution A, and stirs equal
It is even, obtain mixed solution B；
Ammonium hydroxide is added dropwise into the mixed solution B and adjusts pH value for step 3, obtains precipitated product；
Step 4 prepares silver copper oxide composite granule using the precipitated product；
Silver copper oxide composite granule and tungsten carbide powder are put into ball mill in proportion and carry out ball milling and mix powder by step 5, at annealing
Uniformly mixed silver-tungsten carbide-oxidation copper composite powders are obtained after reason；
Step 6, the silver-colored tungsten carbide that the silver-tungsten carbide-oxidation copper composite powders are prepared into the copper additives containing oxidation are in electrical contact
Alloy.
2. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, the specific steps of step 1 are as follows: Cu powder is first added to the HNO that mass fraction is 40%~60%3It is sufficiently molten in solution
Cu (the NO of 1mol/L is made in solution3)2Solution；Then by the Cu (NO3)2The AgNO3 that solution is slowly added into 1mol/L is water-soluble
In liquid, mixed solution A is obtained.
3. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, in step 2: the concentration of the polyvinylpyrrolidonesolution solution is 0.4~6mol/L, and the concentration of the ascorbic acid is
1.5~2.5mol/L.
4. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, step 3 specifically: the mixed solution B is carried out to ultrasonic wave at 55~75 DEG C and stirs 1~2h, and in this process
By the way that ammonium hydroxide is added dropwise to adjust solution ph to 8~10, it is stirred for 1~2h after being added dropwise to complete, until precipitating is completely, is precipitated
Product.
5. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, step 4 specifically: first the precipitated product is put into vacuum oven, obtains drying after dry at 70~90 DEG C
Powder；Then the powder by the drying is put into Muffle furnace, and 2~4h is calcined at 500~650 DEG C；It will finally be obtained after calcining
Powder take out grinding refinement, obtain silver copper oxide composite granule.
6. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, in step 5: the mass fraction of the silver copper oxide composite granule is 70%~85%, the quality of the tungsten carbide powder
Score is 15%~30%, and the sum of mass fraction of the two is 100%.
7. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, in mechanical milling process described in step 5: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 8mm, 6mm, and presses 2:3:
1 quantitative proportion, ratio of grinding media to material are 12~20:1, and rotational speed of ball-mill 400r/min, Ball-milling Time is 8~10h.
8. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, in step 5: annealing temperature is 500 DEG C, annealing time 2h.
9. a kind of preparation method of the silver-colored tungsten carbide contact alloy of copper additives containing oxidation as described in claim 1, feature
It is, in step 6 specifically: be prepared into the silver-tungsten carbide-oxidation copper composite powders using compacting-sintering-extrusion process
To the silver-colored tungsten carbide alloy as electric contact material of the copper additives containing oxidation.
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Cited By (1)
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| CN115478188A (en) * | 2022-08-24 | 2022-12-16 | 苏州银孚新材料有限公司 | Preparation method of silver tungsten carbide electrical contact material |
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