CN116904787A - Preparation method of silver-saving high-performance silver tungsten carbide nickel contact - Google Patents
Preparation method of silver-saving high-performance silver tungsten carbide nickel contact Download PDFInfo
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- CN116904787A CN116904787A CN202310866494.0A CN202310866494A CN116904787A CN 116904787 A CN116904787 A CN 116904787A CN 202310866494 A CN202310866494 A CN 202310866494A CN 116904787 A CN116904787 A CN 116904787A
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- tungsten carbide
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 116
- UYKQQBUWKSHMIM-UHFFFAOYSA-N silver tungsten Chemical compound [Ag][W][W] UYKQQBUWKSHMIM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 60
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims abstract description 51
- 230000008595 infiltration Effects 0.000 claims abstract description 46
- 238000001764 infiltration Methods 0.000 claims abstract description 46
- 238000005245 sintering Methods 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 38
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000007493 shaping process Methods 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 100
- 238000001816 cooling Methods 0.000 claims description 56
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 34
- 239000002270 dispersing agent Substances 0.000 claims description 14
- 230000014759 maintenance of location Effects 0.000 claims description 14
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011812 mixed powder Substances 0.000 claims description 9
- 230000006835 compression Effects 0.000 claims description 7
- 238000007906 compression Methods 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
- 238000003754 machining Methods 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000007580 dry-mixing Methods 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 17
- 239000004332 silver Substances 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 72
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000012467 final product Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 238000013461 design Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- VILAVOFMIJHSJA-UHFFFAOYSA-N dicarbon monoxide Chemical compound [C]=C=O VILAVOFMIJHSJA-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- QNVRIHYSUZMSGM-UHFFFAOYSA-N hexan-2-ol Chemical compound CCCCC(C)O QNVRIHYSUZMSGM-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BSWXAWQTMPECAK-UHFFFAOYSA-N 6,6-diethyloctyl dihydrogen phosphate Chemical compound CCC(CC)(CC)CCCCCOP(O)(O)=O BSWXAWQTMPECAK-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005088 metallography Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
-
- 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
- H01H1/0233—Composite material having a noble metal as the basic material and containing carbides
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a silver-saving high-performance silver tungsten carbide nickel contact, and belongs to the technical field of manufacturing of electrical contacts. The preparation process comprises the following steps: preparing raw materials: the raw materials comprise silver powder, nickel powder and tungsten carbide powder; mixing materials; granulating; shaping; presintering; sintering; infiltration; shaping and post-treatment; wherein, the mass fraction of silver powder in the raw materials is 47-53%, the mass fraction of nickel powder is 8-22%, and the balance is tungsten carbide powder. Nickel is adopted to replace part of silver, so that the effects of saving silver and reducing cost are achieved; meanwhile, nickel is used for replacing part of silver to obtain a silver tungsten carbide nickel contact, the performance of the silver tungsten carbide nickel contact is equivalent to that of the traditional silver tungsten carbide contact, and the use requirement can be met; in addition, the electrical life is additionally improved over conventional silver tungsten carbide contacts.
Description
Technical Field
The invention belongs to the technical field of manufacturing of electrical contacts, and particularly relates to a preparation method of a silver-saving high-performance silver tungsten carbide nickel contact.
Background
The silver tungsten carbide contact is used as a common electrical contact material and has wide application in electrical equipment such as switches, relays and the like. The main components of the silver-tungsten carbide contact are silver and tungsten carbide, wherein the silver has excellent electric and heat conduction properties, and the tungsten carbide has high melting point and high electric corrosion resistance, so that the silver-tungsten carbide contact has the properties of high electric conduction, high heat conduction, high melting point, high electric corrosion resistance and the like.
The preparation process of the silver-tungsten carbide contact mainly comprises a mixed powder sintering method and an infiltration method, wherein the infiltration method is more commonly applied, a tungsten carbide framework is firstly prepared, then the tungsten carbide framework and a silver block or silver flake are placed together for sintering, and silver with a low melting point is melted and then goes deep into the tungsten carbide framework to form the silver-tungsten carbide contact. However, the wettability of silver to tungsten carbide is poor, trace metal elements are generally required to be added when preparing a tungsten carbide skeleton, so that silver can be fully infiltrated into the tungsten carbide skeleton in the infiltration process, a more compact silver tungsten carbide contact is obtained, and when the addition amount of the trace elements is too high, the performance of the silver tungsten carbide contact can be rapidly reduced, and the usability of the silver tungsten carbide contact is affected; and in the silver tungsten carbide contact, the price of silver is high, so that the production cost of the silver tungsten carbide contact is high.
Disclosure of Invention
The invention aims to provide a preparation method of a silver-saving high-performance silver tungsten carbide nickel contact, which aims to solve the technical problems in the background technology.
In order to achieve the above purpose, the invention discloses a preparation method of a silver-saving high-performance silver tungsten carbide nickel contact, which comprises the following steps:
(1) Preparing raw materials: the raw materials comprise silver powder, nickel powder and tungsten carbide powder;
(2) Mixing: mixing by adopting a dry mixing process, adding raw materials into a dry mixer, and then adding zirconia balls and a dispersing agent;
(3) Granulating: granulating the uniformly mixed powder materials;
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: feeding the formed pressed compact into a sintering furnace for presintering;
(6) Sintering: sending the presintered product into a sintering furnace for sintering;
(7) Infiltration: delivering the sintered product into an infiltration furnace for infiltration operation;
(8) Shaping: machining the infiltrated product, and performing structural shaping;
(9) Post-treatment: and (5) performing post-treatment such as deburring on the shaped product to obtain a final product.
Wherein, the mass fraction of silver powder in the raw materials is 47-53%, the mass fraction of nickel powder is 8-22%, and the balance is tungsten carbide powder.
Wherein the grain diameter of the silver powder is 0.1-3 microns, and the grain diameter of the tungsten carbide powder is 0.5-2 microns.
Further, in the step (2), firstly, nickel powder is premixed, and during the premixing, the nickel powder and beryllium powder are uniformly mixed, wherein the addition amount of the beryllium powder is 0.2-0.5% of the total mass of the raw materials. Wherein the beryllium powder has a size of 250-325 mesh, preferably 300 mesh.
Further, in the step (2), in the end of mixing, adding an organic solvent accounting for 0.5-2.5% of the total mass of the raw materials into the uniformly mixed materials, uniformly stirring, and then drying and sieving.
Further, the nickel powder is nickel carbonyl, and the particle size of the nickel powder is 1-3 microns.
Further, the tungsten carbide powder comprises tungsten carbide powder with the particle size of 0.8 micron and tungsten carbide powder with the particle size of 1.5 micron; and the mass ratio of the tungsten carbide powder with the particle size of 0.8 micron to the tungsten carbide powder with the particle size of 1.5 micron is 1:3.5-4.5.
Further, in the mixing process, the volume of the zirconia balls accounts for 30-40% of the total volume of the mixing barrel.
Further, the zirconia balls comprise zirconia balls with the diameter of phi 5mm and zirconia balls with the diameter of phi 15mm, and the quantity ratio of the zirconia balls to the zirconia balls is 1:3.5-4.5.
Further, in the presintering process, the presintering temperature is 600-650 ℃ and the presintering time is 0.5-1.5h.
Further, in the sintering process, the sintering temperature is 800-850 ℃ and the sintering time is 1.0-2.5h.
Further, the infiltration process is carried out in an infiltration furnace, and the infiltration furnace comprises a heating zone, a high-temperature zone, a rapid cooling zone and a cooling zone, wherein the length of the heating zone is 450mm, the height of the heating zone is Wen Ouchang ℃ for 1350mm, the length of the rapid cooling zone is 500mm, and the length of the cooling zone is 2000mm; the sintered product passes through a heating zone, the retention time of the heating zone is 20-30min, then the sintered product enters a high temperature zone, the heating temperature is 1000-1010 ℃, and the retention time of the sintered product in the high temperature zone is 120-150min; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 80-100 ℃, and the residence time is 60-90min; and finally, the product enters a cooling area, the residence time of the cooling area is about 240-360min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
Compared with the prior art, the preparation method of the silver-saving high-performance silver tungsten carbide nickel contact has the following beneficial effects:
(1) In the invention, nickel is adopted to replace part of silver, thereby playing the roles of saving silver and reducing cost.
(2) In the invention, nickel is used for replacing part of silver to obtain the silver tungsten carbide nickel contact, the performance of the silver tungsten carbide nickel contact is equivalent to that of the traditional silver tungsten carbide nickel contact, and the use requirement can be met; in addition, the electrical life is additionally improved over conventional silver tungsten carbide contacts.
(3) In the invention, the infiltration process is low-temperature infiltration, so that on one hand, product dry cracking caused by smaller grain size of silver powder in the infiltration process can be prevented, and on the other hand, the internal stress of a pressed compact obtained by press molding can be eliminated, the product is further prevented from cracking, and the yield of the product is improved.
Detailed Description
Embodiments of the present invention will now be described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer.
The preparation method of the silver-saving high-performance silver tungsten carbide nickel contact comprises the following steps:
(1) Preparing raw materials: silver powder, nickel powder and tungsten carbide powder.
Wherein, the grain diameter of the silver powder is 0.1-3 microns, the grain diameter of the tungsten carbide powder is 0.5-2 microns, the nickel powder is nickel carbonyl, and the grain diameter of the nickel powder is 1-3 microns.
Wherein the mass fraction of silver powder is 47-53%, the mass fraction of nickel powder is 8-22%, and the balance is tungsten carbide powder. Preferably, the mass fraction of the silver powder is 50%, the mass fraction of the nickel powder is 10-15%, and the balance is tungsten carbide powder.
In the invention, nickel is selected because nickel has close performance to silver, nickel has low price, and other metals such as copper, iron and the like have poor conductivity and ductility, so that the performance is difficult to meet the requirements.
In a preferred embodiment, the tungsten carbide powder comprises tungsten carbide powder having a particle size of 0.8 microns, and tungsten carbide powder having a particle size of 1.5 microns, and the mass ratio of tungsten carbide powder having a particle size of 0.8 microns to tungsten carbide powder having a particle size of 1.5 microns is 1:3.5-4.5, preferably 1:4. Simultaneously, two kinds of tungsten carbide powder with thick and thin dimensions are added, so that the superfine silver powder in the raw materials can be ensured to be mixed more uniformly during mixing, and finally a silver tungsten carbide nickel contact product with uniform metallography can be obtained.
(2) Mixing: mixing by adopting a dry mixing process, adding raw materials into a dry mixer, and then adding zirconia balls and a dispersing agent for mixing.
In a preferred embodiment, the nickel powder is first premixed, and the nickel powder and the beryllium powder are uniformly mixed during the premixing, wherein the addition amount of the beryllium powder accounts for 0.2-0.5% of the total mass of the raw materials. Wherein the size of beryllium powder is 250-325 mesh, preferably 300 mesh. The nickel powder and the beryllium powder are premixed in advance, dispersion strengthening can be performed, and the electric corrosion resistance of the final product is improved.
In a preferred embodiment, the dry mixer is a three-dimensional powder mixer, so that powder can be mixed in three dimensions, and the mixing efficiency and mixing quality are improved.
The volume of the zirconia balls accounts for 30-40% of the total volume of the mixing barrel, so that the space in the mixing barrel can be fully utilized, and when the equipment is operated, the powder has sufficient space for full mixing.
In a preferred embodiment, the zirconia balls comprise 5mm and 15mm zirconia balls, and the number ratio of 5mm zirconia balls to 15mm zirconia balls is 1:3.5-4.5, preferably 1:4. When mixing materials, raw material powder is filled in the gap between the zirconia balls with large size and small size, so that the zirconia balls and the raw material powder have larger contact area, and the surface energy of the raw material powder is improved.
The addition mass of the dispersing agent is 0.05-0.5% of the total mass of the raw materials in the step (1), and the dispersing agent is selected from organic dispersing agents such as triethylhexyl phosphoric acid, sodium dodecyl sulfate, methyl amyl alcohol and the like, and is preferably sodium dodecyl sulfate.
In a preferred embodiment, after the compounding is completed, 0.5 to 2.5wt% of an organic solvent such as benzene, toluene, pentane, hexane, methanol, ethanol, isopropanol, diethyl ether, ethyl acetate, acetone, carbon tetrachloride, etc., preferably ethanol, is added. Adding an organic solvent and the mixed materials, uniformly stirring, and then drying and sieving to obtain mixed powder with sufficient fluidity.
(3) Granulating: granulating the uniformly mixed powder materials;
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: and (3) feeding the formed pressed compact into a sintering furnace to perform presintering in a hydrogen atmosphere, wherein the presintering temperature is 600-650 ℃, and the presintering time is 0.5-1.5h, preferably 1h.
(6) Sintering: and (3) feeding the pre-sintered product into a sintering furnace to be sintered in a hydrogen atmosphere, wherein the sintering temperature is 800-850 ℃, and the sintering time is 1.0-2.5h, preferably 1.5h.
(7) Infiltration: and sending the sintered product into an infiltration furnace for infiltration operation. The infiltration furnace adopts special design, and is divided into heating zone, high temperature zone, quick cooling zone and cooling zone, wherein the heating zone length is 450mm, and the height is Wen Ouchang degree 1350mm, and quick cooling zone length is 500mm, and cooling zone length is 2000mm.
The sintered product passes through a heating area, the retention time of the heating area is 20-30min, then the sintered product enters a high temperature area, the heating temperature is 1000-1010 ℃, and the retention time, namely the heat preservation time, in the high temperature area is 120-150min; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 80-100 ℃, and the residence time is 60-90min; and finally, the product enters a cooling area, the residence time of the cooling area is about 240-360min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
(8) Shaping: and machining the infiltrated product, and performing structural shaping to ensure that the size and the structure of the product meet the requirements.
(9) Post-treatment: and (5) performing post-treatment such as deburring on the shaped product to obtain a final product.
The silver tungsten carbide nickel contact obtained by the method is equivalent to the traditional silver tungsten carbide nickel contact in the aspects of density, hardness, electric conductivity, heat conductivity coefficient and the like, and meanwhile, the electric life is additionally prolonged, so that the requirements of actual production can be met.
Example 1
The silver-saving high-performance silver tungsten carbide nickel contact is prepared, and specifically comprises the following steps:
(1) Preparing raw materials:
silver powder with mass fraction of 50% and particle size of 0.1-3 μm;
nickel powder with mass fraction of 10% and carbonyl carbon and particle size of 1-3 μm;
beryllium powder with the mass fraction of 0.2% and the size of 300 meshes;
the mass fraction of the tungsten carbide powder is 39.8%, the tungsten carbide powder comprises tungsten carbide powder with the particle size of 0.8 microns and tungsten carbide powder with the particle size of 1.5 microns, and the mass ratio of the tungsten carbide powder with the particle size of 0.8 microns to the tungsten carbide powder with the particle size of 1.5 microns is 1:4.
(2) Mixing: firstly, premixing nickel powder, and uniformly mixing the nickel powder and beryllium powder; then adding all the raw materials into a three-dimensional powder mixer, adding zirconia balls and a dispersing agent, and carrying out three-dimensional mixing and stirring;
the zirconia balls comprise zirconia balls with the diameter of phi 5mm and zirconia balls with the diameter of phi 15mm, the quantity ratio of the zirconia balls with the diameter of phi 5mm to the zirconia balls with the diameter of phi 15mm is 1:4, and the volume of the zirconia balls accounts for 40% of the total volume of the mixing barrel; the dispersing agent is sodium dodecyl sulfate accounting for 0.1 percent of the total mass of the raw materials.
After the mixing, adding organic solvent ethanol accounting for 1% of the total mass of the raw materials into the powder materials, uniformly stirring the mixture with the mixed materials, and then drying and sieving the mixture for later use.
(3) Granulating: granulating the uniformly mixed powder materials.
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: and (3) sending the formed pressed compact into a sintering furnace for presintering in a hydrogen atmosphere, wherein the presintering temperature is 650 ℃, and the presintering time is 1h.
(6) Sintering: and (3) sending the pre-sintered product into a sintering furnace to be sintered in a hydrogen atmosphere, wherein the sintering temperature is 850 ℃, and the sintering time is 1.5h.
(7) Infiltration: and sending the sintered product into an infiltration furnace for infiltration operation. The infiltration furnace adopts special design, and is divided into heating zone, high temperature zone, quick cooling zone and cooling zone, wherein the heating zone length is 450mm, and the height is Wen Ouchang degree 1350mm, and quick cooling zone length is 500mm, and cooling zone length is 2000mm.
The sintered product passes through a heating zone, the retention time of the heating zone is 30min, then the sintered product enters a high-temperature zone, the heating temperature is 1000 ℃, and the retention time, namely the heat preservation time, in the high-temperature zone is 150min; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 80 ℃, and the residence time is 90min; and finally, the product enters a cooling zone, the residence time of the cooling zone is about 360min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
(8) Shaping: and machining the infiltrated product, and performing structural shaping to ensure that the size and the structure of the product meet the requirements.
(9) Post-treatment: and (5) performing post-treatment such as deburring on the shaped product to obtain a final product.
Example 2
The silver-saving high-performance silver tungsten carbide nickel contact is prepared, and specifically comprises the following steps:
(1) Preparing raw materials:
silver powder with mass fraction of 50% and particle size of 0.1-3 μm;
15% of nickel powder, wherein the nickel powder is carbonyl carbon, and the particle size is 1-3 microns;
the mass fraction of the tungsten carbide powder is 35%, the tungsten carbide powder comprises tungsten carbide powder with the particle size of 0.8 micron and tungsten carbide powder with the particle size of 1.5 micron, and the mass ratio of the tungsten carbide powder with the particle size of 0.8 micron to the tungsten carbide powder with the particle size of 1.5 micron is 1:4.5.
(2) Mixing: adding raw materials into a three-dimensional powder mixer, adding zirconia balls and a dispersing agent, and carrying out three-dimensional mixing and stirring;
the zirconia balls comprise zirconia balls with the diameter of phi 5mm and zirconia balls with the diameter of phi 15mm, the quantity ratio of the zirconia balls with the diameter of phi 5mm to the zirconia balls with the diameter of phi 15mm is 1:3.5, and the volume of the zirconia balls accounts for 35% of the total volume of the mixing barrel; the dispersant is triethylhexyl phosphoric acid accounting for 0.3% of the total mass of the raw materials.
(3) Granulating: granulating the uniformly mixed powder materials.
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: and (3) sending the formed pressed compact into a sintering furnace to perform presintering in a hydrogen atmosphere, wherein the presintering temperature is 600 ℃, and the presintering time is 1.5h.
(6) Sintering: and (3) sending the pre-sintered product into a sintering furnace to be sintered in a hydrogen atmosphere, wherein the sintering temperature is 800 ℃, and the sintering time is 2.5h.
(7) Infiltration: and sending the sintered product into an infiltration furnace for infiltration operation. The infiltration furnace adopts special design, and is divided into heating zone, high temperature zone, quick cooling zone and cooling zone, wherein the heating zone length is 450mm, and the height is Wen Ouchang degree 1350mm, and quick cooling zone length is 500mm, and cooling zone length is 2000mm.
The sintered product passes through a heating zone, the retention time of the heating zone is 20min, then the sintered product enters a high-temperature zone, the heating temperature is 1010 ℃, and the retention time, namely the heat preservation time, is 130min in the high-temperature zone; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 90 ℃, and the residence time is 80min; and finally, the product enters a cooling zone, the residence time of the cooling zone is about 300min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
(8) Shaping: and machining the infiltrated product, and performing structural shaping to ensure that the size and the structure of the product meet the requirements.
(9) Post-treatment: and (5) performing post-treatment such as deburring on the shaped product to obtain a final product.
Example 3
The silver-saving high-performance silver tungsten carbide nickel contact is prepared, and specifically comprises the following steps:
(1) Preparing raw materials:
silver powder with mass fraction of 50% and particle size of 0.1-3 μm;
nickel powder with mass fraction of 8% and carbonyl carbon and particle size of 1-3 μm;
beryllium powder with the mass fraction of 0.5% and the size of 280 mesh;
the mass fraction of the tungsten carbide powder is 41.5 percent, and the particle size is 1.5 microns;
(2) Mixing: firstly, premixing nickel powder, and uniformly mixing the nickel powder and beryllium powder; then adding all the raw materials into a three-dimensional powder mixer, adding zirconia balls and a dispersing agent, and carrying out three-dimensional mixing and stirring;
the zirconia balls comprise zirconia balls with the diameter of phi 5mm and zirconia balls with the diameter of phi 15mm, the quantity ratio of the zirconia balls with the diameter of phi 5mm to the zirconia balls with the diameter of phi 15mm is 1:4.5, and the volume of the zirconia balls accounts for 30% of the total volume of the mixing barrel; the dispersant is methyl amyl alcohol accounting for 0.5% of the total mass of the raw materials.
(3) Granulating: granulating the uniformly mixed powder materials.
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: and (3) sending the formed pressed compact into a sintering furnace to perform presintering in a hydrogen atmosphere, wherein the presintering temperature is 620 ℃, and the presintering time is 1.3h.
(6) Sintering: and (3) sending the pre-sintered product into a sintering furnace to be sintered in a hydrogen atmosphere, wherein the sintering temperature is 820 ℃, and the sintering time is 2.2h.
(7) Infiltration: and sending the sintered product into an infiltration furnace for infiltration operation. The infiltration furnace adopts special design, and is divided into heating zone, high temperature zone, quick cooling zone and cooling zone, wherein the heating zone length is 450mm, and the height is Wen Ouchang degree 1350mm, and quick cooling zone length is 500mm, and cooling zone length is 2000mm.
The sintered product passes through a heating zone, the retention time of the heating zone is 25min, then the sintered product enters a high-temperature zone, the heating temperature is 1005 ℃, and the retention time, namely the heat preservation time, of the sintered product is 120min; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 100 ℃, and the residence time is 60min; and finally, the product enters a cooling zone, the residence time of the cooling zone is about 240min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
(8) Shaping: and machining the infiltrated product, and performing structural shaping to ensure that the size and the structure of the product meet the requirements.
(9) Post-treatment: and (5) performing post-treatment such as deburring on the shaped product to obtain a final product.
Comparative example 1
Selecting tungsten carbide powder with the particle size of 1 micron and silver powder with the particle size of 200 meshes, and mixing the tungsten carbide powder with the silver powder according to the following steps: taking silver=40:60 weight ratio, placing powder into a mixer, mixing for 2.5h, placing the mixed silver tungsten carbide powder, high-purity nickel balls (the nickel content is 99.99%) and water into a roller ball mill together for ball milling for 60h, taking out the powder, drying at 150 ℃ for 2h, placing the dried powder into a hydrogen atmosphere for annealing at 850 ℃ for 3h, detecting that the nickel content in the powder material is 1.46%, then pressing the powder to obtain a pressed compact, placing the pressed compact and the silver pieces into a graphite boat according to the structure that the silver pieces are arranged below and above, and infiltrating for 20min at 1040 ℃ in the hydrogen atmosphere, thereby obtaining the silver tungsten carbide 40 contact.
Comparative example 2
The silver-saving high-performance silver tungsten carbide nickel contact is prepared, and specifically comprises the following steps:
(1) Preparing raw materials:
silver powder with mass fraction of 50% and particle size of 0.1-3 μm;
nickel powder with mass fraction of 11% and carbonyl carbon and particle size of 1-3 μm;
the tungsten carbide powder has the mass fraction of 39% and the particle size of 0.5-2 microns.
(2) Mixing: adding raw materials into a three-dimensional powder mixer, adding zirconia balls and a dispersing agent, and carrying out three-dimensional mixing and stirring;
the zirconia balls comprise zirconia balls with the diameter of phi 5mm and zirconia balls with the diameter of phi 15mm, the quantity ratio of the zirconia balls with the diameter of phi 5mm to the zirconia balls with the diameter of phi 15mm is 1:3.8, and the volume of the zirconia balls accounts for 40% of the total volume of the mixing barrel; the dispersing agent is sodium dodecyl sulfate accounting for 0.3 percent of the total mass of the raw materials.
(3) Granulating: granulating the uniformly mixed powder materials.
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: and (3) sending the formed pressed compact into a sintering furnace to perform presintering in a hydrogen atmosphere, wherein the presintering temperature is 610 ℃, and the presintering time is 1.2h.
(6) Sintering: and (3) sending the pre-sintered product into a sintering furnace to be sintered in a hydrogen atmosphere, wherein the sintering temperature is 820 ℃, and the sintering time is 1.8h.
(7) Infiltration: and sending the sintered product into an infiltration furnace for infiltration operation. The infiltration furnace adopts special design, and is divided into heating zone, high temperature zone, quick cooling zone and cooling zone, wherein the heating zone length is 450mm, and the height is Wen Ouchang degree 1350mm, and quick cooling zone length is 500mm, and cooling zone length is 2000mm.
The sintered product passes through a heating zone, the retention time of the heating zone is 25min, then the sintered product enters a high-temperature zone, the heating temperature is 1080 ℃, and the retention time, namely the heat preservation time, in the high-temperature zone is 140min; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 85 ℃, and the residence time is 85min; and finally, the product enters a cooling zone, the residence time of the cooling zone is about 300min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
(8) Shaping: and machining the infiltrated product, and performing structural shaping to ensure that the size and the structure of the product meet the requirements.
(9) Post-treatment: and (5) performing post-treatment such as deburring on the shaped product to obtain a final product.
The final products obtained in examples 1-3 and comparative examples 1-2 were subjected to performance tests for density, hardness, electrical conductivity, thermal conductivity, electrical life, etc.
The density, hardness, electric conductivity, heat conductivity coefficient and the like are tested according to the standard test methods of the national standard JB/T12073-2014 silver tungsten carbide electric contact material technical condition and the like.
In the electrical life test, the contact material is pressed into a sheet contact with the specification phi 6*2 in advance, and then the sheet contact is subjected to the electrical life test under the conditions of 125A of current, 380V of voltage, 0.51 of power factor and 30 times/min of operation frequency.
The test results are shown in Table 1.
TABLE 1 Performance test results for the contacts obtained in examples 1-3 and comparative examples 1-2
Therefore, compared with the traditional silver tungsten carbide contact, the silver tungsten carbide nickel contact obtained by the method has the advantages that the density, the hardness, the electric conductivity, the heat conductivity coefficient and the like are not obviously reduced, the electric life is additionally prolonged, and the actual production requirements can be met.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the invention, but any modifications, equivalent substitutions, improvements, etc. within the design concept of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the silver-saving high-performance silver tungsten carbide nickel contact is characterized by comprising the following steps of:
(1) Preparing raw materials: the raw materials comprise silver powder, nickel powder and tungsten carbide powder;
(2) Mixing: mixing by adopting a dry mixing process, adding raw materials into a dry mixer, and then adding zirconia balls and a dispersing agent;
(3) Granulating: granulating the uniformly mixed powder materials;
(4) And (3) forming: adding the granulated granules into a forming press for compression forming to obtain a pressed blank;
(5) Presintering: feeding the formed pressed compact into a sintering furnace for presintering;
(6) Sintering: sending the presintered product into a sintering furnace for sintering;
(7) Infiltration: delivering the sintered product into an infiltration furnace for infiltration operation;
(8) Shaping: machining the infiltrated product, and performing structural shaping;
(9) Post-treatment;
wherein, the mass fraction of silver powder in the raw materials is 47-53%, the mass fraction of nickel powder is 8-22%, and the balance is tungsten carbide powder.
2. The method for manufacturing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein in the step (2), firstly, nickel powder is premixed, and the nickel powder and beryllium powder are uniformly mixed during the premixing, wherein the addition amount of the beryllium powder is 0.2-0.5% of the total mass of raw materials.
3. The method for preparing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein in the step (2), in the end of mixing, an organic solvent accounting for 0.5-2.5% of the total mass of raw materials is added into the uniformly mixed materials, and the materials are uniformly stirred, dried and sieved.
4. The method for manufacturing a silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein the nickel powder is nickel carbonyl, and the particle size of the nickel powder is 1-3 microns.
5. The method for manufacturing a silver-saving high-performance silver tungsten carbide nickel contact according to claim 3, wherein the tungsten carbide powder comprises tungsten carbide powder with a particle size of 0.8 microns and tungsten carbide powder with a particle size of 1.5 microns; and the mass ratio of the tungsten carbide powder with the particle size of 0.8 micron to the tungsten carbide powder with the particle size of 1.5 micron is 1:3.5-4.5.
6. The method for preparing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein in the mixing process, the volume of the zirconia balls accounts for 30-40% of the total volume of the mixing barrel.
7. The method for manufacturing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 6, wherein the zirconia balls comprise zirconia balls with the diameter of 5mm and zirconia balls with the diameter of 15mm, and the quantity ratio of the zirconia balls to the zirconia balls is 1:3.5-4.5.
8. The method for manufacturing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein the presintering temperature is 600-650 ℃ and the presintering time is 0.5-1.5h in the presintering process.
9. The method for preparing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein in the sintering process, the sintering temperature is 800-850 ℃ and the sintering time is 1.0-2.5h.
10. The method for preparing the silver-saving high-performance silver tungsten carbide nickel contact according to claim 1, wherein the infiltration process is performed in an infiltration furnace, and the infiltration furnace comprises a heating zone, a high-temperature zone, a rapid cooling zone and a cooling zone, wherein the heating zone is 450mm in length, wen Ouchang mm in height and 1350mm in length, the rapid cooling zone is 500mm in length and the cooling zone is 2000mm in length; the sintered product passes through a heating zone, the retention time of the heating zone is 20-30min, then the sintered product enters a high temperature zone, the heating temperature is 1000-1010 ℃, and the retention time of the sintered product in the high temperature zone is 120-150min; then the product slides down to a rapid cooling area along with a hearth track, the temperature of the rapid cooling area is 80-100 ℃, and the residence time is 60-90min; and finally, the product enters a cooling area, the residence time of the cooling area is about 240-360min, the product is cooled to the room temperature, and then the product is discharged from the furnace to finish the infiltration process.
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