CN114438359A - Preparation method of silver tin oxide electrical contact material - Google Patents
Preparation method of silver tin oxide electrical contact material Download PDFInfo
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- CN114438359A CN114438359A CN202111618853.8A CN202111618853A CN114438359A CN 114438359 A CN114438359 A CN 114438359A CN 202111618853 A CN202111618853 A CN 202111618853A CN 114438359 A CN114438359 A CN 114438359A
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- silver
- tin oxide
- ingot blank
- silver tin
- sintering
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- IVQODXYTQYNJFI-UHFFFAOYSA-N oxotin;silver Chemical compound [Ag].[Sn]=O IVQODXYTQYNJFI-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 148
- 239000004332 silver Substances 0.000 claims abstract description 146
- 229910052709 silver Inorganic materials 0.000 claims abstract description 140
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 230000009467 reduction Effects 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 36
- 238000005488 sandblasting Methods 0.000 claims abstract description 31
- 238000000576 coating method Methods 0.000 claims abstract description 30
- 239000011248 coating agent Substances 0.000 claims abstract description 28
- 238000003825 pressing Methods 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 14
- 230000001590 oxidative effect Effects 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000012778 molding material Substances 0.000 claims abstract description 6
- 238000001192 hot extrusion Methods 0.000 claims description 19
- 238000000462 isostatic pressing Methods 0.000 claims description 17
- 230000000754 repressing effect Effects 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 15
- 230000002441 reversible effect Effects 0.000 claims description 15
- 239000000654 additive Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 230000036961 partial effect Effects 0.000 claims description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 5
- 238000005253 cladding Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 54
- 238000001125 extrusion Methods 0.000 description 15
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical compound [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 description 14
- 238000000137 annealing Methods 0.000 description 12
- 230000002829 reductive effect Effects 0.000 description 12
- 238000005096 rolling process Methods 0.000 description 12
- 238000003466 welding Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000004080 punching Methods 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- 239000011812 mixed powder Substances 0.000 description 8
- 229910001128 Sn alloy Inorganic materials 0.000 description 7
- 238000005097 cold rolling Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000005098 hot rolling Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ASMQPJTXPYCZBL-UHFFFAOYSA-N [O-2].[Cd+2].[Ag+] Chemical compound [O-2].[Cd+2].[Ag+] ASMQPJTXPYCZBL-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910015427 Mo2O3 Inorganic materials 0.000 description 1
- MCQLERHPPNKJHT-UHFFFAOYSA-N [Ag].[Sn].[Ag]=O Chemical compound [Ag].[Sn].[Ag]=O MCQLERHPPNKJHT-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 235000012438 extruded product Nutrition 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 150000003378 silver Chemical group 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Images
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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
-
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- 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
-
- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
-
- 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
- C23C8/12—Oxidising using elemental oxygen or ozone
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
- H01H1/02376—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
The invention relates to the technical field of electric contact materials, in particular to a preparation method of a silver tin oxide electric contact material. The method comprises the following steps: (1) mixing silver and tin oxide, pressing into ingots, and sintering to obtain silver tin oxide ingot blanks; (2) coating a silver layer on the surface of the silver tin oxide ingot blank to prepare a silver-coated ingot blank; (3) preparing the silver-coated ingot blank into a molding material; the step (2) comprises the following steps: reduction: placing the silver tin oxide ingot blank in a hydrogen atmosphere for reduction treatment; sand blasting: carrying out sand blasting treatment on the surface of the silver tin oxide ingot blank; coating silver: coating a silver layer on the surface of the silver tin oxide ingot blank; oxidizing and sintering: and (3) placing the silver tin oxide ingot blank coated with the silver layer on the outer layer in an oxygen-containing atmosphere for oxidation and sintering. This application is through the processing mode of reduction, sandblast, covering silver and oxidation sintering for silver tin oxide ingot base and cladding silver layer combine closely, have guaranteed the homogeneity of silver layer thickness simultaneously, have improved silver tin oxide electrical contact material's reliability and uniformity.
Description
Technical Field
The invention relates to the technical field of electric contact materials, in particular to a preparation method of a silver tin oxide electric contact material.
Background
The silver cadmium oxide electric contact material plays an important role in the whole low-voltage electric contact material by virtue of comprehensive electrical properties such as unique arc extinguishing performance, welding resistance, low and stable contact resistance and the like, but the cadmium element is harmful to human bodies and the environment, so that the cadmium element is gradually limited to be used or replaced. The silver tin oxide electric contact material has become an environment-friendly nontoxic electric contact material which is hopefully to replace silver cadmium oxide due to the excellent arc erosion resistance, wear resistance and fusion welding resistance, and is widely applied to the fields of relays, contactors, circuit breakers and the like. When the silver tin oxide material is applied to the field of contactors or circuit breakers with larger current grades, the silver tin oxide material generally needs to be processed into a sheet contact form, and then is assembled after being welded with a contact bridge. Due to poor wettability among the silver tin oxide material, the solder and the copper contact bridge, the welding strength and the welding area between the contact and the contact bridge cannot meet the requirements after direct welding. Therefore, in order to ensure the welding strength of the silver tin oxide and the contact bridge, reduce the contact resistance and temperature rise of the contact, and improve the reliability and electrical property of the electric appliance, a pure silver layer needs to be compounded on the welding surface as a transition layer in the contact processing process.
Patent document No. CN103643074A discloses a method for preparing silver tin oxide sheet-like contactnO2The mixed powder is made into an ingot blank by a conventional method, sintered at high temperature in an oxygen-containing atmosphere, and subjected to hot extrusion and hot rolling compounding to obtain AgSnO2The Ag/Ag composite strip is subjected to cold rolling, finish rolling and punch forming to obtain the required AgSnO2A blade-like contact. It is difficult to ensure AgSnO in the production process2The silver layer and the Ag are tightly combined, a gap exists between the silver layer and the Ag, a small amount of air can be remained in the extrusion process, and the silver layer can easily generate a bubbling phenomenon after extrusion; and AgSnO2And Ag, a small amount of oil stains and impurities are easily introduced in the production process, the interface bonding strength between the Ag and the Ag is influenced, the phenomenon that the bonding strength of a local area is low exists, and the risk that a contact falls off exists in the use process of an electric appliance.
The patent document with the publication number of CN111468719A discloses a silver tin oxide sheet-shaped electrical contact and a preparation method thereof, the method comprises the steps of firstly preparing a silver tin oxide powder spindle, sintering and repressing the silver tin oxide powder spindle, obtaining the silver tin oxide spindle with the surface coated with a silver tin alloy layer by adopting a hydrogen reduction mode, extruding the silver tin oxide spindle into a silver tin oxide strip with three surfaces coated with the silver tin alloy layer by adopting a back extrusion device after repressing treatment, and finally processing the silver tin oxide strip into the sheet-shaped electrical contact with a working layer of silver tin oxide and a welding layer of the silver tin alloy layer by rolling, punching and surface treatment. Although the problem of consistency of welding performance and composite strength can be solved, the problem of consistency of thickness of a welding surface cannot be solved, because the surface-coated silver-tin alloy layer is obtained in a hydrogen reduction mode, the reduction temperature, time, gas flow, placement mode and the like can influence the thickness of the surface-coated silver-tin alloy layer, the requirement on control precision of the preparation process is high, and the uniformity of the thickness of the surface-coated silver-tin alloy layer is difficult to ensure. In addition, because the processing plasticity of the silver tin oxide material is poor, the hot extrusion temperature is high in general, but the melting point of the silver tin alloy layer coated on the surface is low, so that the hot extrusion temperature of the material is limited, and the problems of difficult material extrusion, low material yield and high manufacturing cost in the hot extrusion process are caused.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a silver tin oxide electric contact material.
The technical scheme for solving the problems is to provide a preparation method of the silver tin oxide electric contact material, which comprises the following steps:
(1) mixing silver and tin oxide, pressing into ingots, and sintering to obtain silver tin oxide ingot blanks;
(2) coating a silver layer on the surface of the silver tin oxide ingot blank to prepare a silver-coated ingot blank;
(3) preparing the silver-coated ingot blank into a molding material;
the step (2) comprises the following steps:
reduction: placing the silver tin oxide ingot blank in a hydrogen atmosphere for reduction treatment;
sand blasting: carrying out sand blasting treatment on the surface of the silver tin oxide ingot blank subjected to reduction treatment;
coating silver: coating a silver layer on the surface of the silver tin oxide ingot blank subjected to sand blasting treatment;
oxidizing and sintering: and (3) placing the silver tin oxide ingot blank coated with the silver layer on the outer layer in an oxygen-containing atmosphere for internal oxidation and sintering treatment.
In the application, firstly, the silver tin oxide ingot blank is subjected to hydrogen reduction treatment, mainly in order to form a thin silver tin reduction layer on the surface of the ingot blank, and when silver is coated subsequently, the coated silver layer is in contact with the silver tin reduction layer, so that the wettability of the silver tin oxide ingot blank and the coated silver layer can be improved, and the combination tightness between the silver tin oxide ingot blank and the coated silver layer is improved. Preferably, in the reduction step, the reduction temperature is 680-820 ℃, and the reduction time is 10-30 min.
On the one hand, an active surface can be obtained, the adhesive force of silver powder coated with a silver layer subsequently is further improved, and meanwhile, the effective combination of an interface can be promoted in the subsequent sintering process; on the other hand, the thickness of the reduced silver-tin layer formed by hydrogen reduction treatment can be leveled, the problem of uneven thickness of the reduced silver-tin layer is solved, and the thickness uniformity of the whole silver layer is improved. Preferably, in the sand blasting step, the alumina abrasive is adopted for dry sand blasting, the grain diameter of the alumina abrasive is 20-150 μm, and the sand blasting pressure is 0.4-1.5 MPa.
After hydrogen reduction and sand blasting treatment are finished, the silver layer is coated on the surface of the silver tin oxide ingot blank, and the coated silver layer with tight combination and uniform thickness can be obtained. The silver coating mode can adopt any one of the prior art, and as the optimization of the invention, in the silver coating step, the isostatic pressing treatment process is adopted to coat the silver layer on the surface of the silver tin oxide ingot blank. The ingot blank is coated with the silver layer in an isostatic pressing mode, an extra isolating device is not needed for powder loading, the ingot blank is only needed to be fixed in an isostatic pressing die sleeve in a centering mode, the operation is easy, the problems of coating and matching of the silver layer and the silver tin oxide ingot blank are solved, the thickness of the coated silver layer is uniform and controllable, and the problem of uneven thickness caused by hydrogen reduction treatment of the ingot blank is further solved. In the present invention, the isostatic pressure is preferably 50 to 300 MPa. Preferably, in the present invention, the diameter of the silver coated ingot obtained after the silver coating is increased by 10 to 25mm with respect to the silver tin oxide ingot.
After silver is coated, oxidation sintering treatment is carried out to promote the coated silver layer and the reduced silver-tin layer to form good metallurgical bonding, and all reduced elements in the reduced silver-tin layer are oxidized into corresponding oxides again, so that the melting point of the material is improved, the extrusion temperature of the material can be increased, the processing plasticity of the material is improved, the yield of the material is further improved, and the production cost is reduced. And the silver tin oxide and the silver are still integrated after sintering, foreign matter pollutants influencing the bonding strength cannot be introduced into the composite interface, and the bonding strength of the interface between the silver tin oxide and the silver is ensured. Preferably, in the step of oxidizing and sintering, the oxygen partial pressure of the oxygen-containing atmosphere is 0.02-2.0 MPa, the sintering temperature is 680-820 ℃, and the sintering time is 2-4 h.
Through the treatment steps, the interface bonding strength between the silver tin oxide ingot blank and the coated silver layer can be effectively improved.
In order to further improve the interface bonding strength between the silver tin oxide ingot blank and the coated silver layer, the silver tin oxide and the additive are mixed, pressed into an ingot and sintered to prepare the silver tin oxide silver coated silver coating in the step (1)A silver tin oxide ingot blank; the additive comprises one or more of transition metal oxide and rare earth oxide. In the reduction process, oxides of the transition metal and the rare earth are also reduced to form the transition metal and the rare earth, the transition metal and the rare earth have an empty d orbit, unpaired electrons in the empty d orbit have extremely high activity, and are easy to form chemical bonds with silver powder coated with a silver layer subsequently, so that the interface bonding strength between the silver tin oxide ingot blank and the coated silver layer is further improved. Among them, the more the number of unpaired electrons in the d-orbital in the additive increases, the more easily the bond is formed with the silver atom. Preferably, the additive includes NiO, CuO, ZnO and In2O3、Bi2O3、WO3、Mo2O3、La2O3、Y2O3、CeO2One or more of them. Preferably, the silver tin oxide ingot comprises 4-16% by mass of tin oxide, no more than 3% by mass of additives, and the balance of silver.
Although the ingot blank after the oxidation sintering can be directly used for forming a profile, the ingot blank shrinks to different degrees along the diameter and the length direction due to the sintering, and in order to further improve the bonding tightness between the silver tin oxide ingot blank and the silver coating, the step (2) preferably further comprises the following steps: and after the step of oxidizing sintering, carrying out hot repressing treatment on the obtained sintered ingot blank to obtain the silver-coated ingot blank. The silver-coated ingot blank with a regular shape can be obtained through the hot re-pressing treatment, and is convenient to be made into a section bar subsequently. The preferable temperature of the hot repressing is 750-900 ℃, and the pressure maintaining time is 20-60 s.
Preferably, in step (3), the silver-coated ingot blank is subjected to reverse hot extrusion to obtain a strip, and the strip is made into the profile, so that the reliability and consistency of the bonding strength between the silver tin oxide ingot blank and the silver-coated layer are further improved through large-deformation extrusion. In the backward extrusion, because there is no relative movement between the surface layer of the ingot blank and the inner lining of the extrusion container, the mechanical condition of metal flowing in the extrusion container is changed, the non-uniformity of deformation and extrusion force are reduced, and simultaneously, because the metal flows uniformly, the outer surface layer of the ingot blank can completely enter the surface layer of the extruded product. The heating temperature of the reverse hot extrusion is preferably 750-900 ℃.
After the strip is produced by hot backward extrusion, the strip is preferably trimmed at the ends and rolled on a rolling mill to a desired thickness, and as a preference of the present invention, annealing is performed at least once midway to stabilize the dimensions. The annealing temperature is preferably 600-800 ℃, and the time is 1-6 h.
After rolling to the desired thickness, the profile can be formed by any means, for example, by punching the profile with a punching die.
In addition, since the ingot blank shrinks to different degrees in the diameter and length directions during the sintering process of step (1), the reduction process is directly performed on the silver tin oxide ingot blank with uneven surface, and the uniformity of the thickness of the subsequent silver tin layer and the silver coating layer is still affected, therefore, as a preferred aspect of the present invention, the reduction process is performed after the turning process is performed on the silver tin oxide ingot blank. The turning can eliminate the difference of the shrinkage size of the sintered silver tin oxide ingot blank in the diameter direction, and can ensure the consistent diameter size of the silver tin oxide ingot blank.
In the present invention, it is preferable that the silver and the tin oxide are mixed in step (1) in a dry mixing manner for 1.5 to 5 hours. Preferably, when silver and tin oxide are mixed and then are subjected to ingot pressing and sintering to prepare a silver tin oxide ingot blank, the diameter of the ingot blank obtained by ingot pressing is 60-110 mm, and the length of the ingot blank is 150-550 mm; the sintering temperature is 850-920 ℃, and the sintering time is 2-6 h.
The invention has the beneficial effects that:
1. this application is through hydrogen reduction, sandblast, cover silver and oxidation sintering's processing method for silver tin oxide ingot base and cladding silver layer combine closely, have guaranteed the homogeneity of silver layer thickness simultaneously, have improved silver tin oxide electrical contact material's reliability and uniformity.
2. In the application, the additive is added into the silver tin oxide ingot blank to be matched with the silver coated with the silver layer, and the interface bonding strength between the silver tin oxide ingot blank and the silver coated layer is further enhanced through chemical bonding.
3. The method and the device have the advantages that the advantages of the reverse hot extrusion composite process and the isostatic pressing silver covering process are integrated, the size proportion of the silver tin oxide ingot blank to the silver covering layer can be adjusted according to the requirements of customers, the extrusion ratio is increased, the extrusion specification of the strip is reduced, the production period is shortened, and the yield and the production efficiency are improved.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a silver tin oxide electrical contact material;
fig. 2 is a 200-fold metallographic structure diagram of the silver tin oxide electrical contact profile produced in example 1.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
A preparation method of a silver tin oxide electric contact material is shown in figure 1, and comprises the following steps:
(1) mixing silver and tin oxide, pressing into ingots, and sintering to obtain silver tin oxide ingot blanks;
4 parts of tin oxide, 3 parts of NiO and 93 parts of silver were dry-mixed in parts by mass for 1.5 hours to obtain a mixed powder. Pressing the mixed powder into an ingot blank in an isostatic pressing device, wherein the diameter of the ingot blank is 60mm, the length of the ingot blank is 150mm, and the isostatic pressing pressure is 50 MPa. And sintering the ingot blank at 850 ℃ for 6h to obtain the silver tin oxide ingot blank.
(2) Coating a silver layer on the surface of the silver tin oxide ingot blank to prepare a silver-coated ingot blank;
reduction: and (3) turning the prepared silver tin oxide ingot blank, and then placing the ingot blank in a hydrogen atmosphere for reduction treatment, wherein the reduction temperature is 820 ℃, and the reduction time is 10 min.
Sand blasting: and carrying out sand blasting treatment on the surface of the reduced silver tin oxide ingot blank, wherein the sand blasting mode is a dry method, the grain diameter of the aluminum oxide abrasive is 20 mu m, and the sand blasting pressure is 0.4 MPa.
Coating silver: and placing the silver tin oxide ingot blank subjected to sand blasting treatment in isostatic pressing equipment, and pressing the silver tin oxide ingot blank into a silver-coated ingot blank under the isostatic pressing pressure of 50MPa, wherein the diameter of the silver-coated ingot blank is 85mm, and the length of the silver-coated ingot blank is 150 mm.
Oxidizing and sintering: and carrying out internal oxidation and sintering on the silver-coated ingot blank obtained by coating silver in an oxygen atmosphere, wherein the oxygen partial pressure is 0.02MPa, the sintering temperature is 820 ℃, and the sintering time is 2 h.
Hot repressing: and carrying out hot repressing treatment on the sintered silver-coated ingot blank, wherein the hot repressing temperature is 750 ℃, and the pressure maintaining time is 20 s.
(3) Preparing a molding material from the silver-coated ingot blank;
and performing reverse hot extrusion on the silver-coated ingot blank subjected to the hot re-pressing treatment to obtain a silver tin oxide/silver strip, wherein the heating temperature is 750 ℃ during the reverse hot extrusion. Cutting off the head and the tail of the silver tin oxide/silver strip obtained by reverse hot extrusion, rolling the silver tin oxide/silver strip on a cold rolling mill to a required thickness, and annealing at least once midway at the annealing temperature of 600 ℃ for 6 hours. And punching the strip rolled to the required thickness by adopting a stamping die to obtain the silver tin oxide/silver electric contact profile.
The metallographic structure diagram of the silver tin oxide/silver electric contact section bar which is 200 times is shown in figure 2, and it can be seen that the metallographic structure of the silver tin oxide/silver electric contact section bar prepared by the method is uniform, has no cracks, interlayers, aggregates and air holes, and has good thickness consistency of a silver layer.
Example 2
This embodiment is substantially the same as embodiment 1, except that:
in the step (1), 4 parts by mass of tin oxide and 96 parts by mass of silver are dry-mixed for 1.5 hours to obtain mixed powder.
Example 3
This embodiment is substantially the same as embodiment 1, except that:
the hot repressurization step was not performed.
Example 4
This embodiment is substantially the same as embodiment 1, except that:
no turning process is performed.
Example 5
This embodiment is substantially the same as embodiment 1, except that:
and (3) cutting off the head and the tail of the silver tin oxide/silver strip obtained by reverse hot extrusion, rolling the silver tin oxide/silver strip on a cold rolling mill to a required thickness, and not annealing in the midway. And punching the strip rolled to the required thickness by adopting a stamping die to obtain the silver tin oxide/silver electric contact profile.
Example 6
A preparation method of a silver tin oxide electric contact material is shown in figure 1, and comprises the following steps:
(1) mixing silver and tin oxide, pressing into ingots, and sintering to obtain silver tin oxide ingot blanks;
according to the parts by mass, 12 parts of tin oxide and 1 part of Y2O30.5 part of La2O3And 86.5 parts of silver were mixed by a dry method for 3 hours to obtain a mixed powder. Pressing the mixed powder into an ingot blank in an isostatic pressing device, wherein the diameter of the ingot blank is 80mm, the length of the ingot blank is 350mm, and the isostatic pressing pressure is 200 MPa. And sintering the ingot blank at 880 ℃ for 4h to obtain the silver tin oxide ingot blank.
(2) Coating a silver layer on the surface of the silver tin oxide ingot blank to prepare a silver-coated ingot blank;
reduction: and (3) turning the prepared silver tin oxide ingot blank, and then placing the ingot blank in a hydrogen atmosphere for reduction treatment, wherein the reduction temperature is 750 ℃, and the reduction time is 20 min.
Sand blasting: and carrying out sand blasting treatment on the surface of the reduced silver tin oxide ingot blank, wherein the sand blasting mode is a dry method, the grain diameter of the aluminum oxide abrasive is 100 mu m, and the sand blasting pressure is 1.0 MPa.
Coating silver: and placing the silver tin oxide ingot blank subjected to sand blasting treatment in isostatic pressing equipment, and pressing the silver tin oxide ingot blank into a silver-coated ingot blank under the isostatic pressing pressure of 200MPa, wherein the diameter of the silver-coated ingot blank is 98mm, and the length of the silver-coated ingot blank is 350 mm.
Oxidizing and sintering: and carrying out internal oxidation and sintering on the silver-coated ingot blank obtained by coating silver in an oxygen atmosphere, wherein the oxygen partial pressure is 1.0MPa, the sintering temperature is 750 ℃, and the sintering time is 3 h.
Hot repressing: and carrying out hot repressing treatment on the sintered silver-coated ingot blank, wherein the hot repressing temperature is 850 ℃, and the pressure maintaining time is 40 s.
(3) Preparing a molding material from the silver-coated ingot blank;
and performing reverse hot extrusion on the silver-coated ingot blank subjected to the hot re-pressing treatment to obtain a silver tin oxide/silver strip, wherein the heating temperature is 850 ℃ during the reverse hot extrusion. Cutting off the head and the tail of the silver tin oxide/silver strip obtained by reverse hot extrusion, rolling the silver tin oxide/silver strip on a cold rolling mill to a required thickness, and annealing at least once midway at the annealing temperature of 700 ℃ for 3 hours. And punching the strip rolled to the required thickness by adopting a stamping die to obtain the silver tin oxide/silver electric contact profile.
Example 7
A preparation method of a silver tin oxide electric contact material is shown in figure 1, and comprises the following steps:
(1) mixing silver and tin oxide, pressing into ingots, and sintering to obtain silver tin oxide ingot blanks;
16 parts by mass of tin oxide, 0.1 part by mass of NiO and 83.9 parts by mass of silver were dry-mixed for 5 hours to obtain a mixed powder. Pressing the mixed powder into an ingot blank in an isostatic pressing device, wherein the diameter of the ingot blank is 110mm, the length of the ingot blank is 550mm, and the isostatic pressing pressure is 300 MPa. And sintering the ingot blank at 920 ℃ for 2h to obtain the silver tin oxide ingot blank.
(2) Coating a silver layer on the surface of the silver tin oxide ingot blank to prepare a silver-coated ingot blank;
reduction: and (3) turning the prepared silver tin oxide ingot blank, and then placing the ingot blank in a hydrogen atmosphere for reduction treatment, wherein the reduction temperature is 680 ℃, and the reduction time is 30 min.
Sand blasting: and carrying out sand blasting treatment on the surface of the reduced silver tin oxide ingot blank, wherein the sand blasting mode is a dry method, the grain diameter of the aluminum oxide grinding material is 150 mu m, and the sand blasting pressure is 1.5 MPa.
Coating silver: and placing the silver tin oxide ingot blank subjected to sand blasting into isostatic pressing equipment, and pressing the silver tin oxide ingot blank into a silver-coated ingot blank under the isostatic pressing pressure of 300MPa, wherein the diameter of the silver-coated ingot blank is 120mm, and the length of the silver-coated ingot blank is 550 mm.
Oxidizing and sintering: and internally oxidizing and sintering the silver-coated ingot blank obtained by coating silver in an oxygen atmosphere, wherein the oxygen partial pressure is 2.0MPa, the sintering temperature is 680 ℃, and the sintering time is 4 h.
Hot repressing: and carrying out hot repressing treatment on the sintered silver-coated ingot blank, wherein the hot repressing temperature is 900 ℃, and the pressure maintaining time is 60 s.
(3) Preparing a molding material from the silver-coated ingot blank;
and performing reverse hot extrusion on the silver-coated ingot blank subjected to the hot re-extrusion treatment to obtain a silver tin oxide/silver strip, wherein the heating temperature is 900 ℃ during the reverse hot extrusion. Cutting off the head and the tail of the silver tin oxide/silver strip obtained by reverse hot extrusion, rolling the silver tin oxide/silver strip on a cold rolling mill to a required thickness, and annealing at 800 ℃ for 1h at least once in the process. And punching the strip rolled to the required thickness by adopting a stamping die to obtain the silver tin oxide/silver electric contact profile.
Comparative example 1
This comparative example is essentially the same as example 1 except that:
referring to the hot-rolling silver-coating process disclosed in patent document No. CN 103643074A:
and (2) after the preparation of the silver tin oxide ingot blank in the step (1) is finished, sintering and extruding to obtain a silver tin oxide strip, heating the silver tin oxide strip and the pure Ag strip to 700 ℃ by using a heating device, and then rolling the two strips to be thick at a rolling speed of 5m/min by using a hot rolling mill to obtain the silver-coated strip. And rolling the obtained silver-coated strip on a cold rolling mill to the required thickness, and annealing at least once in the process, wherein the annealing temperature is 600 ℃ and the time is 6 hours. And punching the strip rolled to the required thickness by adopting a stamping die to obtain the silver tin oxide/silver electric contact profile.
Comparative example 2
This comparative example is essentially the same as example 1 except that:
refer to the reduction silver coating process disclosed in patent document with publication number CN 111468719A:
and (2) after the preparation of the silver tin oxide ingot blank in the step (1) is finished, placing the prepared silver tin oxide ingot blank in a hydrogen atmosphere for reduction treatment, wherein the reduction temperature is 720 ℃, and the reduction time is 4 h. Then, the hot repressing treatment is carried out, the hot repressing temperature is 750 ℃, and the pressure maintaining time is 20 s. And finally heating the silver-tin oxide composite strip at 700 ℃ for 4h under the protection of nitrogen, and then extruding the silver-tin oxide composite strip by adopting backward extrusion equipment. And (3) cutting off the head and the tail of the silver tin oxide composite strip obtained by reverse hot extrusion, rolling the silver tin oxide composite strip on a cold rolling mill to a required thickness, and annealing at least once midway at the annealing temperature of 600 ℃ for 6 hours. And punching the strip rolled to the required thickness by adopting a stamping die to obtain the silver tin oxide/silver electric contact profile.
[ PROPERTIES DETECTION ]
Conductivity:for the profiles prepared in examples and comparative examples, 10 arbitrary points on the profiles were taken as detection points, the conductivities of the 10 detection points were respectively detected, and the average value of the 10 conductivities was found, thereby finding the standard deviation between the 10 conductivities and the average value.
Bonding strength between the silver tin oxide green sheet and the silver coating layer:the profiles prepared in examples and comparative examples were cut off from the interface using a Zwick/Roell electronic universal material tester by a shearing method, and the shearing force was measured, and the greater the force required to break the interface, the better the interface bonding. The shear strength was calculated by dividing the shear force by the bonding area.
The results of the measurements are shown in Table 1 below.
Table 1.
As shown in table 1, it can be seen from example 1 and comparative example 1 that, in the present application, the bonding strength between the silver tin oxide ingot and the silver coating layer can be effectively improved by a series of means of reduction, sand blasting, silver coating and oxidation sintering, compared with the hot-rolling silver coating means in the prior art. As can be seen from the example 1 and the comparative example 2, the difference of the conductivity between the detection points on the section bar prepared in the application is small, which shows that the section bar prepared in the embodiment has the advantages of uniform thickness of the silver layer on the surface and good uniformity of the conductivity. In contrast, in comparative example 2, the silver layer obtained by reduction had high bonding strength with the silver tin oxide ingot, but the silver layer had non-uniform thickness, resulting in non-uniform conductivity.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of a silver tin oxide electric contact material comprises the following steps:
(1) mixing silver and tin oxide, and then pressing and sintering to prepare a silver tin oxide ingot blank;
(2) coating a silver layer on the surface of the silver tin oxide ingot blank to prepare a silver-coated ingot blank;
(3) preparing the silver-coated ingot blank into a molding material;
the method is characterized in that: the step (2) comprises the following steps:
reduction: placing the silver tin oxide ingot blank in a hydrogen atmosphere for reduction treatment;
sand blasting: carrying out sand blasting treatment on the surface of the silver tin oxide ingot blank subjected to reduction treatment;
coating silver: coating a silver layer on the surface of the silver tin oxide ingot blank subjected to sand blasting treatment;
oxidizing and sintering: and (3) placing the silver tin oxide ingot blank coated with the silver layer on the outer layer in an oxygen-containing atmosphere for internal oxidation and sintering treatment.
2. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: in the step (1), silver, tin oxide and additives are mixed, and then are pressed into ingots and sintered to prepare silver tin oxide ingot blanks; the additive comprises one or more of transition metal oxide and rare earth oxide.
3. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: in the reduction step, the reduction temperature is 680-820 ℃, and the reduction time is 10-30 min.
4. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: in the sand blasting step, aluminum oxide abrasive is adopted for dry sand blasting, the particle size of the aluminum oxide abrasive is 20-150 mu m, and the sand blasting pressure is 0.4-1.5 MPa.
5. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: in the silver coating step, an isostatic pressing treatment process is adopted to coat a silver layer on the surface of the silver tin oxide ingot blank.
6. The method for preparing a silver tin oxide electrical contact material according to claim 5, wherein: in the silver coating step, the isostatic pressure is 50-300 MPa.
7. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: in the step of oxidizing and sintering, the oxygen partial pressure of the oxygen-containing atmosphere is 0.02-2.0 MPa, the sintering temperature is 680-820 ℃, and the sintering time is 2-4 h.
8. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: the step (2) further comprises the following steps: and after the step of oxidizing sintering, carrying out hot repressing treatment on the obtained oxidized sintered ingot blank to obtain the silver-coated ingot blank.
9. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: and (3) performing reverse hot extrusion on the silver-coated ingot blank to obtain a strip material, and then manufacturing the strip material into the section.
10. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein: and carrying out the reduction step after carrying out turning treatment on the silver tin oxide ingot blank.
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| CN112126810A (en) * | 2020-09-03 | 2020-12-25 | 大都克电接触科技（中国）有限公司 | Preparation method of silver tungsten carbide graphite electrical contact material |
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| US4452652A (en) * | 1982-07-08 | 1984-06-05 | Akira Shibata | Electrical contact materials and their production method |
| US5846288A (en) * | 1995-11-27 | 1998-12-08 | Chemet Corporation | Electrically conductive material and method for making |
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