CN116959804A - Preparation method of silver-saving silver tin oxide electric contact material based on SSF and FAST technologies - Google Patents
Preparation method of silver-saving silver tin oxide electric contact material based on SSF and FAST technologies Download PDFInfo
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- CN116959804A CN116959804A CN202310759249.XA CN202310759249A CN116959804A CN 116959804 A CN116959804 A CN 116959804A CN 202310759249 A CN202310759249 A CN 202310759249A CN 116959804 A CN116959804 A CN 116959804A
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- 239000000463 material Substances 0.000 title claims abstract description 35
- IVQODXYTQYNJFI-UHFFFAOYSA-N oxotin;silver Chemical compound [Ag].[Sn]=O IVQODXYTQYNJFI-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005516 engineering process Methods 0.000 title claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 16
- 229910001128 Sn alloy Inorganic materials 0.000 claims abstract description 15
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical compound [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052709 silver Inorganic materials 0.000 claims abstract description 15
- 239000004332 silver Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 230000005684 electric field Effects 0.000 claims abstract description 9
- 238000005098 hot rolling Methods 0.000 claims abstract description 4
- 238000003723 Smelting Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 241000276425 Xiphophorus maculatus Species 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 4
- 239000011135 tin Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000005282 brightening Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910001887 tin oxide Inorganic materials 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 2
- 239000006104 solid solution Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000007670 refining Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 7
- 229910052738 indium Inorganic materials 0.000 description 5
- 230000004927 fusion Effects 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 229910017750 AgSn Inorganic materials 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000010099 solid forming Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- 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
- C22C32/001—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 only oxides
- C22C32/0015—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 only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
-
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a preparation method of a silver-saving silver tin oxide electric contact material based on SSF and FAST technologies, which comprises the following steps: (1) Preparing semi-solid silver-tin alloy slurry, and forming to obtain a blank; (2) hot rolling the blank into silver-tin alloy flakes; (3) The silver-tin alloy flake is oxidized after deoiling and cleaning to obtain a silver-tin oxide flake; (4) compacting silver tin oxide flakes into ingots to obtain embryonic ingots; (5) And placing the billet into electric field activated sintering equipment to sinter to obtain a silver tin oxide spindle, and processing the silver tin oxide spindle into a wire. The invention processes the alloy raw material with low silver content, thereby refining grains; the spindle is sintered by using the FAST electric field activated sintering technology in the post-oxidation spindle sintering process, so that the spindle has better compactness after secondary molding, each phase of tissue in the material is more tightly combined, and the finally prepared rivet-shaped contact has higher compactness, so that the rivet-shaped contact has more excellent electric life under alternating current or direct current conditions.
Description
Technical Field
The invention belongs to the field of electrical material manufacturing, and particularly relates to a silver-saving silver tin oxide electrical contact material based on SSF and FAST technologies and a preparation method thereof.
Background
Silver-based electrical contact materials have excellent electrical and thermal conductivity, and due to the low hardness of pure silver and poor resistance to electrical wear, it is often necessary to add other additives to the silver matrix to enhance the electrical properties of the material, such as resistance to fusion welding, electrical life, and resistance to arc burn, etc. of the contacts. Silver tin oxide (AgSnO) 2 ) One of them is that it has better resistance to fusion welding and burning loss, can be applied to the relay and the contactor switch of heavy current. At present, agSnO is prepared 2 The main method comprises an alloy internal oxidation method and an atomization method, wherein oxide particles are unevenly distributed in the low-silver-content silver-saving electric contact material manufactured by the process, the particle size is different, the compactness of the material is lower, so that wires are easy to break during processing, the silver layer cracks and other anomalies occur during rivet contact forming, the yield of the material is influenced, and the phenomena of bonding and the like occur during contact service, thereby causing the following phenomenaThe electrical appliance is in failure, and the service life of the electrical appliance is greatly influenced.
The retrieved patent documents for preparing silver tin oxide materials by the related document retrieval are as follows:
the Chinese patent No. CN116083740A discloses a preparation process of a silver tin oxide electric contact material, which adopts an alloy particle internal oxidation process to enable tin oxide particles to react in situ in Ag crystal lattices, and adopts surface activation treatment to enable the surfaces of the alloy particles to be rough, so that internal oxidation can be completed without reaching a high-pressure level through alloy particle homogenizing annealing and activation treatment, the hardness of the prepared material can be ensured to be in a processable range, and the problems of internal oxide particle uniformity, material compactness and processability of the silver-saving electric contact material with low silver content can not be solved.
In the traditional process, due to the increase of the oxide content in the preparation of the alloy material with low silver content, the material has the problems of lower compactness and difficult processing, the problems of incapability of realizing batch production and poor electric life on a final electric product and the high cost caused by longer production time are caused, so that the prior electric contact material preparation process needs to be improved.
Disclosure of Invention
The invention aims to overcome the defects and the shortcomings of the prior art and provide a silver-saving silver-tin oxide electric contact material based on SSF (semi-solid forming) and FAST (electric field activated sintering) technologies and a preparation method thereof.
The first aspect of the invention provides a preparation method of a silver-saving silver tin oxide electric contact material based on SSF and FAST technologies, which comprises the following steps:
(1) Preparing semi-solid silver-tin alloy slurry, and forming to obtain a blank;
(2) Hot rolling the blank into silver-tin alloy flakes;
(3) The silver-tin alloy flake is oxidized after deoiling and cleaning to obtain a silver-tin oxide flake;
(4) Pressing silver tin oxide flakes into ingots to obtain embryonic ingots;
(5) And placing the billet into electric field activated sintering equipment to sinter to obtain a silver tin oxide spindle, and processing the silver tin oxide spindle into a wire.
Preferably, the step (1) specifically includes the following steps: according to the proportion of silver-tin alloy, adding silver plate, tin ingot and additive into a crucible of a smelting furnace, smelting, cooling after forming alloy solution, stirring after the solution becomes semi-solid state, pouring the semi-solid state slurry into a mould after stirring is completed, and forming into a platy blank.
Preferably, the components of silver, tin and additives are calculated according to weight percentage, wherein the weight percentage of silver is 65-80 wt%, the weight percentage of tin oxide is 16.5-27.5 wt%, and the weight percentage of the additives is 3.5-7.5-wt%; the additive is one or more of indium oxide, bismuth oxide, copper oxide and rare earth.
Preferably, the smelting furnace is an SSF semi-solid electromagnetic smelting furnace, and the smelting heating is performed by using medium-frequency induction current.
Preferably, the smelting current is 50-100A, the intermediate frequency voltage is 0.8-1.5 KV, and the temperature of the semi-solid alloy slurry is maintained at 500-700 ℃.
Preferably, the semisolid solution is stirred by an EMS electromagnetic stirring device, and the semisolid alloy slurry breaks up dendritic structures in the alloy under the action of electromagnetic force to form non-dendritic structures; the stirring rate is set to 50-100 rad/min and the stirring time is set to 5-10 min.
Preferably, the step (2) specifically includes the following steps: heating the plate blank to 600-700 ℃, placing the plate blank into a roller for rolling, setting the speed to be 2-5mm/s, taking out the plate blank when the plate blank is rolled to be 1-2mm thick, and processing the sheet into a sheet with the length of 3-6mm by using a punching machine.
Preferably, the step (3) specifically includes the following steps: cleaning and drying the silver-tin alloy sheet by using an oil remover and a brightening agent, and then placing the silver-tin alloy sheet into oxidation furnace equipment, wherein the heating temperature is set to be 500-700 ℃, the oxygen pressure amplitude is set to be 0.1-1.5MPa, and the oxidation time is set to be 8-30h;
the step (4) specifically comprises the following steps: cleaning the silver tin oxide flake, and forming into a cylindrical blank by using a four-column hydraulic press, wherein the hydraulic press pressure is set to be 30-50MPa, and the dwell time is set to be 10-20s.
Preferably, the step (5) specifically includes the following steps: putting the billet into electric field activated sintering equipment, setting pulse voltage to be 3-30V, current to be 200-600A, pulse time to be 50-200ms and sintering time to be 0.5-1h; and heating the sintered silver tin oxide spindle at 700-800 ℃ for 3-5 h, and then forming into a wire with the specification of phi 6mm by using an extruder.
The second aspect of the invention provides the silver tin oxide electric contact material prepared by the preparation method.
The beneficial effects of the invention are as follows:
firstly, refining grains is achieved by processing alloy raw materials with low silver content, so that air holes and shrinkage holes of cast ingots generated by the increase of the proportion of the second phase component in the low silver content material in the traditional process are reduced, the compactness of an alloy blank structure is improved, and a spherical or nearly spherical non-dendritic structure is obtained;
secondly, the FAST electric field activated sintering technology is used for sintering the spindle in the post-oxidation spindle sintering process, so that the spindle has better compactness after secondary forming, the sintering process is activated, the combination among all phase tissues in the material is tighter, meanwhile, the sintering time is short, the production time is shortened, the oxide distribution of the finished wire is more uniform, the prepared low-silver-content electric contact material has good extensibility, no fracture occurs in the wire processing process, and the rivet-shaped contact prepared finally has more excellent electric life under the alternating current or direct current conditions due to the high compactness and spherical oxide tissues.
The service life of the electric contact material prepared by the invention reaches more than 13 ten thousand times under a certain current condition, and the electric contact material has better fusion welding resistance and burning loss resistance.
Detailed Description
The present invention will be described in further detail below for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
Example 1
A preparation method of a silver-saving silver tin oxide electric contact material based on SSF and FAST technologies comprises the following steps:
(1) Preparation of SSF semi-solid alloy billets: according to the formula Ag65 wt% of AgSn alloy, snO 2 27.5 wt%,In 2 O 3 6. 6 wt% of CuO 1.5. 1.5 wt%. Adding silver plates, tin ingots, indium ingots and other raw materials into an SSF semi-solid electromagnetic smelting furnace crucible for smelting, adjusting the power of the smelting furnace after alloy solution is formed, reducing the temperature of the molten solution to 650 ℃, starting an EMS electromagnetic device after the molten solution becomes semi-solid, setting the stirring speed to be 100 rad/min, setting the stirring time to be 10 min, pouring the semi-solid slurry into a prepared mould after stirring is completed, and forming into a platy blank;
(2) And (3) hot rolling: heating the platy blank obtained in the step (1) to 600 ℃, putting the platy blank into a roller for rolling, setting the speed to be 3.5 mm/s, taking out the platy blank when the platy blank is rolled to the thickness of 2mm, and processing the sheet into a sheet with the length of 4.5 mm by using a punching machine;
(3) Deoiling and cleaning: cleaning the thin sheet obtained in the step (2) by using an oil remover and a brightening agent, and drying;
(4) Oxidizing: placing the AgSn alloy sheet obtained in the step (3) into oxidation furnace equipment, wherein the heating temperature is set to 700 ℃, the oxygen pressure amplitude is set to 1.5MPa, and the oxidation time is set to 26 h;
(5) Cleaning and ingot pressing: agSnO obtained in the step (4) is processed 2 Cleaning the thin sheet, forming the thin sheet into a cylindrical blank by using a four-column hydraulic press, wherein the pressure of the hydraulic press is set to 40 MPa, and the dwell time is set to 15 s;
(6)AgSnO 2 electric Field Activated Sintering (FAST): placing the cylindrical billet obtained in the step (5) into FAST sintering equipment, setting pulse voltage to be 25V, current to be 400A, pulse time to be 100 ms and sintering time to be 1h;
sintering AgSnO 2 Spindle heating at 800 deg.c for 3 hr, extruding to form silk of phi 6mm specificationAnd (3) material.
Example 2
The difference from example 1 is that the raw materials are added in different amounts, and the mixture is prepared by 10kg for 1 time, and the ratio of the added formula is Ag:75 wt%, snO 2 :20.5wt %,In 2 O 3 :3 wt%,CuO:1.5 wt%。
Example 3
The difference from example 1 is that the amount of the raw materials charged is different, and the composition is prepared according to 10kg for 1 time, wherein Ag:80 wt%, snO 2 :16.5 wt%,In 2 O 3 :3 wt%,CuO:0.5 wt%。
Comparative example
The difference from example 1 is that:
in the step (1), silver plates, tin ingots, indium ingots and other raw materials are added into a traditional medium-frequency smelting furnace, the materials are heated to 1400 ℃ until the materials are melted into liquid slurry, and the liquid slurry is poured into a prepared mould to be molded into a platy blank;
in the step (6), the cylindrical billet obtained in the step (5) is placed in a traditional resistance furnace, and the temperature is set to 900 ℃ for 15 h.
Preparation of AgSnO from the silver tin oxide electric contact Material prepared in examples 1-3 and comparative example 2 The Cu rivet contact is subjected to an electrical simulation performance experiment, and the rivet specification is that a movable contact R4.2x1.5 (0.5) +2.6x1.7SR15 and a static contact F4.2x1.5 (0.5) +2.6x1.2.
The experimental conditions for simulating the electrical properties are as follows: 250 VAC, 10A, closing force 90 g, breaking force 55 g, contact frequency 30 times/min; 20 VDC, 5A, closing force 90 g, breaking force 40 g, contact frequency 30 times/min, experimental results are shown in table 1.
The service life of the electric contact material prepared by the invention reaches more than 13 ten thousand times under the current condition, and the electric contact material has better fusion welding resistance and burning loss resistance.
The foregoing disclosure is illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. The preparation method of the silver-saving silver tin oxide electric contact material based on the SSF and FAST technologies is characterized by comprising the following steps of:
(1) Preparing semi-solid silver-tin alloy slurry, and forming to obtain a blank;
(2) Hot rolling the blank into silver-tin alloy flakes;
(3) The silver-tin alloy flake is oxidized after deoiling and cleaning to obtain a silver-tin oxide flake;
(4) Pressing silver tin oxide flakes into ingots to obtain embryonic ingots;
(5) And placing the billet into FAST electric field activated sintering equipment to sinter to obtain a silver tin oxide spindle, and processing the silver tin oxide spindle into a wire.
2. The method of manufacturing according to claim 1, characterized in that:
the step (1) specifically comprises the following steps: according to the proportion of silver-tin alloy, adding silver plate, tin ingot and additive into a crucible of a smelting furnace, smelting, cooling after forming alloy solution, stirring after the solution becomes semi-solid state, pouring the semi-solid state slurry into a mould after stirring is completed, and forming into a platy blank.
3. The preparation method according to claim 2, characterized in that: the components of silver, tin and additives are calculated according to weight percentage, wherein the weight percentage of silver is 65-80 wt%, the weight percentage of tin oxide is 16.5-27.5 wt%, and the weight percentage of the additives is 3.5-7.5 wt%; the additive is one or more of indium oxide, bismuth oxide, copper oxide and rare earth.
4. The preparation method according to claim 2, characterized in that: the smelting furnace is an SSF semi-solid electromagnetic smelting furnace, and medium-frequency induction current is used for heating in smelting and heating.
5. The method of manufacturing according to claim 4, wherein: the smelting current is 50-100A, the intermediate frequency voltage is 0.8-1.5 KV, and the temperature of the semi-solid alloy slurry is maintained to be 500-700 ℃.
6. The preparation method according to claim 2, characterized in that: the method comprises the steps that an EMS electromagnetic stirring device is used for stirring the semi-solid solution, and the semi-solid alloy slurry breaks up dendritic structures in the alloy under the action of electromagnetic force to form non-dendritic structures; the stirring rate is set to 50-100 rad/min and the stirring time is set to 5-10 min.
7. The preparation method according to claim 1, wherein the step (2) specifically comprises the steps of: heating the plate blank to 600-700 ℃, placing the plate blank into a roller for rolling, setting the speed to be 2-5mm/s, taking out the plate blank when the plate blank is rolled to be 1-2mm thick, and processing the sheet into a sheet with the length of 3-6mm by using a punching machine.
8. The preparation method according to claim 1, wherein the step (3) specifically comprises the steps of: cleaning and drying the silver-tin alloy sheet by using an oil remover and a brightening agent, and then placing the silver-tin alloy sheet into oxidation furnace equipment, wherein the heating temperature is set to be 500-700 ℃, the oxygen pressure amplitude is set to be 0.1-1.5MPa, and the oxidation time is set to be 8-30h;
the step (4) specifically comprises the following steps: cleaning the silver tin oxide flake, and forming into a cylindrical blank by using a four-column hydraulic press, wherein the hydraulic press pressure is set to be 30-50MPa, and the dwell time is set to be 10-20s.
9. The preparation method according to claim 1, wherein the step (5) specifically comprises the steps of: putting the billet into electric field activated sintering equipment, setting pulse voltage to be 3-30V, current to be 200-600A, pulse time to be 50-200ms and sintering time to be 0.5-1h; and heating the sintered silver tin oxide spindle at 700-800 ℃ for 3-5 h, and then forming into a wire with the specification of phi 6mm by using an extruder.
10. The silver tin oxide electrical contact material prepared by the preparation method according to any one of claims 1 to 9.
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