CN110423908B - Silver oxide, tin oxide and indium oxide electric contact material capable of rapidly oxidizing silver and preparation method - Google Patents

Silver oxide, tin oxide and indium oxide electric contact material capable of rapidly oxidizing silver and preparation method Download PDF

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CN110423908B
CN110423908B CN201910786745.8A CN201910786745A CN110423908B CN 110423908 B CN110423908 B CN 110423908B CN 201910786745 A CN201910786745 A CN 201910786745A CN 110423908 B CN110423908 B CN 110423908B
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oxide
silver
contact material
agsninx
agsnin
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CN110423908A (en
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穆成法
祁更新
陈家帆
张舟磊
杨辉
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0466Alloys based on noble metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1078Alloys containing non-metals by internal oxidation of material in solid state
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • H01H1/023Composite material having a noble metal as the basic material
    • H01H1/0237Composite material having a noble metal as the basic material and containing oxides
    • H01H1/02372Composite 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/04Co-operating contacts of different material

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Abstract

The invention discloses a silver oxide, tin oxide and indium oxide electric contact material capable of rapidly oxidizing silver and a preparation method thereof, which comprises the following steps: s1, preparing an AgSnIn or AgSnInX spindle by adopting a powder isostatic pressing method; s2, sintering the spindle to obtain a plate; s3, compounding the board and the silver plate to obtain a compounded board; s4, performing heat treatment and cold rolling on the composite plate, and punching the composite plate into a material belt; s5, carrying out internal oxidation on the material belt to obtain the rapid silver oxide tin oxide indium oxide electric contact material which has a uniform tissue structure, the tissue particle size after oxidation is basically consistent, and AgSnO after oxidation2‑In2O3The expansion is almost not expanded, the product appearance is relatively flat, the welding surface is flat, and the welding performance is good; and the oxidation speed is improved by more than 30 percent compared with the traditional internal oxidation speed.

Description

Silver oxide, tin oxide and indium oxide electric contact material capable of rapidly oxidizing silver and preparation method
Technical Field
The invention relates to a preparation method of an electrical contact material, in particular to a high-performance silver tin oxide indium oxide AgSnO capable of being quickly oxidized2-In2O3An electric contact material and a preparation method thereof.
Background
The electric contact material and the components thereof are widely applied to automatic control circuits of automobiles, communication, household appliances, machine tools and the like, and play a key role in automatic adjustment, conversion and safety protection of the circuits. The contact is used as a key part in the electric contact component and directly bears the on-off of load current in a circuit, and the reliability and the service life of the electric contact component are determined by the performance of the contact. Preparation of silver tin oxide indium oxide (AgSnO) by internal oxidation method2-In2O3) The material has better electric life and excellent electric resistanceArc erosion, abrasion resistance and fusion welding resistance, and is widely applied to various electrical appliances.
Relevant research and report at home and abroad in recent years. Such as: 1) the invention has the following patent: a preparation method of a high-oxide-content flaky contact material is disclosed as follows: CN104404419A, by combining the traditional preparation internal oxidation process and high-temperature diffusion annealing, the silver tin oxide electric contact material with the characteristics of high oxide content, high composite silver interface bonding strength and the like is prepared. 2) Wangsong, etc. and its preparation process is AgSnO2(8)-In2O3(4) The influence of the structure and properties of electrical contact materials, rare metals and cemented carbides, vol.43, No.2, apr.2015; introduction to the preparation of AgSnO by powder metallurgy, alloy powder preoxidation and pressure internal oxidation2(8)-In2O3(4) Electric contact material, research of different preparation process to AgSnO2In2O3The microstructure and performance of the electrical contact material. Patent 1) introduces a method and process for increasing the bonding strength of silver tin oxide (high oxidation content) and silver interface, namely: smelting, extruding, silver-coated hot rolling, cold rolling, punching, high-temperature diffusion annealing treatment, internal oxidation treatment and post-treatment processes, but the method for preparing the silver tin oxide indium oxide has longer internal oxidation period, and particularly has lower production efficiency for thicker products; meanwhile, the internal oxidation structure prepared by the method is relatively thick, and cracks are easily generated in the structure. Document 2) emphasis on powder metallurgy of Ag powder and SnO2Powder, In2O3Performing low-energy ball milling on the powder, performing cold isostatic pressing, and sintering and extruding; the alloy powder preoxidation method is Ag-Sn-In atomization pulverization, oxidation, isostatic pressing, sintering, extrusion and the like, and the traditional internal oxidation is combined with a high-pressure Ag-Sn-In alloy vacuum melting furnace, casting, plate pulling, pressure oxidation and the like. The former two main powder metallurgy processes, the latter one is also the traditional internal oxidation process, but the internal oxidation pressure is increased; however, in the internal oxidation process, parameters have influence on the oxidation speed, the increase of the oxygen pressure has little influence on the increase of the oxidation speed, and meanwhile, high pressure needs special equipment and is generally difficult to be used for mass production; the process for preparing silver tin oxide indium oxide has the same structure as that of patent 1). In addition, conventional internal oxidation processes, are described, consisting ofAgSnO is generated after AgSnIn oxidation2-In2O3Make the working surface AgSnO2-In2O3The volume expands, the silver surface area of a welding interface is unchanged, and a final product is caused, the appearance is uneven, the welding surface is concave, and the subsequent welding quality is seriously influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-performance AgSnO capable of being quickly oxidized2-In2O3An electric contact material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
according to a first aspect of the invention, a method for preparing a rapid silver oxide tin oxide indium oxide electrical contact material is provided, which comprises the following steps:
s1, preparing an AgSnIn or AgSnInX spindle by adopting a powder isostatic pressing method, wherein X is any element capable of forming an alloy with Ag and Sn and improving the electrical property of the Ag and Sn;
s2, sintering the AgSnIn or AgSnInX spindle to prepare an AgSnIn or AgSnInX plate;
s3, compounding the AgSnIn or AgSnInX board and a silver board to obtain a compounded board;
s4, performing heat treatment and cold rolling on the composite plate, and punching the plate into a sheet;
and S5, carrying out internal oxidation on the sheet to obtain the rapid silver oxide, tin oxide and indium oxide electric contact material.
Optionally, in S1, the preparing an AgSnIn or AgSnInX spindle by using a powder isostatic pressing method includes:
smelting an Ag ingot, an Sn ingot and an In ingot, or smelting the Ag ingot, the Sn ingot, the In ingot and an X element to obtain an alloy solution;
atomizing the alloy solution to prepare powder to obtain AgSnIn or AgSnInX powder;
and sieving and isostatic pressing the AgSnIn or AgSnInX powder to prepare the AgSnIn or AgSnInX spindle.
Optionally, the smelting, wherein: the Ag content is 83.5-93.5%, the Sn content is 4.5-12%, the In content is 1.5-4%, and the total X content is less than or equal to 1.0%.
Optionally, the sieving and isostatic pressing, wherein: the sieve mesh number is between 100 and 600 meshes, and the isostatic pressure is between 70 and 200 Mpa.
Optionally, in S2, the sintering, wherein: temperature between 650 ℃ and 820 ℃ and H2Or hydrogen-nitrogen mixed gas protection.
Optionally, in S2, the AgSnIn or AgSnInX spindle is sintered and then made into an AgSnIn or AgSnInX plate by an extrusion process.
Optionally, in S3, compounding the AgSnIn or AgSnInX sheet with a silver plate, wherein: the thermal composite deformation is between 40 and 70 percent, the temperature is controlled between 500 and 750 ℃, and N2Or Ar protection.
Optionally, in S4, the composite board is subjected to heat treatment, wherein: the temperature is between 450 and 750 ℃, and N is introduced2Or nitrogen-hydrogen mixed gas protection.
According to a second aspect of the present invention, there is provided a fast silver oxide tin oxide indium oxide electrical contact material prepared by the above method.
The technical route of the method is compared with the conventional internal oxidation method for preparing AgSnO (AgSnO) by using traditional materials2-In2O3The method of (a) is significantly different:
the technical route adopted by the invention is as follows: firstly, preparing an AgSnInX spindle by a powder isostatic pressing method (AgSnInX can be smelted and atomized to prepare powder, then carrying out isostatic pressing on the obtained powder to form the spindle), then sintering and extruding, and then carrying out punching and internal oxidation.
The traditional internal oxidation method is as follows: AgSnIn smelting → ingot casting → surface processing → thermal compounding (silver coating) → rolling → punching → internal oxidation, etc.
As is well known, when the alloy is smelted and cast into a spindle, the compactness of an alloy structure is higher, and oxygen diffusion channels are fewer in the internal oxidation process, so that the oxidation speed is lower; because the traditional smelting and casting method is adopted, the sizes of internal crystal grains of the internal oxidized structure cannot be uniformAnd (3) stabilizing. According to the invention, the AgSnIn or AgSnInX spindle is prepared in the early stage by a powder isostatic pressing method, the compactness is only about 90% of that of a smelting casting spindle, a large number of superfine micropores exist among powder particles, the superfine micropores are partially eliminated by extrusion, and a large number of boundary lines and grain boundaries are formed among particles, so that more channels are provided for oxygen diffusion in the subsequent internal oxidation process, namely, short-circuit oxidation. Meanwhile, the subsequent compounding and cold rolling processes further break the crystal grains to form more 'grain boundaries'; after oxidation the metals (Sn, In, X) evolve into the metal oxide MeO, expanding further In volume, filling the boundaries between the particles. Furthermore, as the AgSnIn or AgSnInX atomized powder particles are specially screened, the structure 'crystal grain' size after oxidation is relatively uniform, and the AgSnO prepared by the traditional internal oxygen method2-In2O3The uniformity and stability of the prepared oxide particles are difficult to control. Meanwhile, because a large number of 'grain boundaries' exist and oxygen diffusion 'channels' exist, the oxidation speed is high according to a common oxidation process, and compared with the traditional internal oxidation speed, the oxidation speed can be improved by more than 30%.
The method of the invention skillfully designs the technical route of the whole method by utilizing the principle of internal organizational structure change among materials, has the advantages of simple process, convenient operation, low cost and no special requirement on equipment, and the prepared electric contact material has uniform and exquisite organizational structure, higher electric service life, can be widely applied to low-voltage electric appliances and has lower temperature rise. Meanwhile, the method can realize rapid oxidation, has high production efficiency, and shortens the internal oxidation time by more than 30 percent compared with the traditional method.
The AgSnO prepared by the method can be quickly oxidized and has high performance2-In2O3The electric contact material has a relatively uniform tissue structure, the sizes of the oxidized tissue particles are basically consistent, and the AgSnO on the oxidized working surface2-In2O3The volume is hardly expanded, the appearance of the product is relatively flat, the welding surface is flat, and the welding performance is good.
Drawings
FIG. 1 shows conventional internal oxidized AgSnO2(9)-In2O3(4) Metallographic structure;
FIG. 2 shows AgSnO prepared according to an embodiment of the invention2(9)-In2O3(4) And (4) metallographic structure.
Detailed Description
The technical solutions of the present invention are further described below, and the following description is only for understanding the technical solutions of the present invention and is not intended to limit the scope of the present invention, which is defined by the claims.
High-performance AgSnO capable of being rapidly oxidized and prepared by embodiment of the invention2-In2O3The electric contact material has uniform tissue distribution, basically consistent tissue particle size after oxidation and AgSnO after oxidation2-In2O3Almost does not expand, the product appearance is relatively flat, the welding surface is flat, and the welding performance is good; and the oxidation speed is improved by more than 30 percent compared with the traditional internal oxidation speed.
In the invention, the designed smelting, atomizing and pulverizing, sieving and isostatic pressing, sintering, extruding, compounding, heat treatment, cold rolling, punching, internal oxidation, cleaning and other steps, the parameters of the specific process operation can be selected, for example, in some preferred embodiments of the invention:
firstly, smelting an Ag ingot, an Sn ingot and an In ingot, or smelting the Ag ingot, the Sn ingot, the In ingot and an X element to obtain an alloy melt. The parameters can adopt: the Ag content is 83.5-93.5%, the Sn content is 4.5-12%, the In content is 1.5-4%, and further, the total content of X is less than or equal to 1.0%. X is any element capable of forming an alloy with Ag and Sn and improving the electrical property of the alloy, for example, X can be one or more of Zn, Bi, Cu, Ni and rare earth elements.
And secondly, atomizing the alloy melt smelted in the first step. The parameters can adopt: the pressure of the atomizing gas is between 1.0Mpa and 10 Mpa.
And thirdly, sieving and isostatic pressing the atomized powder. The parameters can adopt: the mesh number is 100-600 meshes, the isostatic pressure is 70-200 Mpa, and the pressure maintaining time can be 30-120 s.
Fourthly, sintering the obtained spindle, wherein the parameters can adopt: the temperature is between 650 ℃ and 820 ℃; h2Or hydrogen-nitrogen mixed gas protection, and the time can be 2-7 hours.
Fifthly, carrying out hot extrusion on the sintered spindle, wherein the parameters can adopt: the temperature is 600-720 ℃, the protection of charcoal or hydrogen-nitrogen mixed gas can be carried out for 2-4 hours. The thickness and the width of the extruded plate are obtained by calculating the width and the thickness ratio of the AgSnIn or AgSnInX layer required by the final product.
And sixthly, compounding the plate and the silver plate. The parameters can adopt: the thermal composite deformation is 40-70%, the temperature is controlled to be 500-750 ℃, the temperature is protected by N2 or Ar, and the thickness and the width of the material belt are calculated according to the width and the thickness proportion of the AgSnIn or AgSnInX layer and the Ag layer required by the final product.
Certainly, the plate can be cleaned and brushed and then compounded with the silver plate, so that the compounding effect is improved.
And seventhly, performing heat treatment on the composite material belt, wherein the parameters can adopt: the temperature is between 450 and 750 ℃, and N is introduced2Or under the protection of nitrogen-hydrogen mixed gas, and the time can be 6-12 hours.
And eighthly, cold rolling and punching the heat-treated material belt again. The parameters can adopt: the cold rolling single-pass deformation is controlled to be between 5 and 20 percent.
Ninth, the sheet after punching is internally oxidized to obtain fine, uniform and quickly oxidized high-performance AgSnO2-In2O3An electrical contact material. The parameters can adopt: the oxidation temperature is 580-700 ℃; the oxygen pressure is controlled between 0.8MPa and 5 MPa; the oxidation time is obtained by calculating according to the thickness of the punched sheet and combining with the oxidation process parameters.
The detailed technical operation of the present invention is explained by the following examples of specific applications.
Example one
To prepare Ag (92) SnO2-In2O3Example of electrical contact materials
Firstly, smelting and ingoting Ag ingots, Sn ingots, In ingots and additive Ni. Wherein the Ag content was 93.5 wt%, the Sn content was 4.7 wt%, the In content was 2.5 wt%, and the Ni content was 0.3 wt%.
And secondly, atomizing the alloy melt smelted in the first step, wherein the pressure of atomizing gas is 1.0 MPa.
Thirdly, sieving and isostatic pressing the atomized powder, wherein the sieve mesh number is 600 meshes; isostatic pressure 70MPa, dwell time 120 s.
Fourthly, sintering the obtained spindle at 820 ℃; the time is 2 hours; and protecting with mixed hydrogen and nitrogen gas.
Fifthly, hot extruding the sintered spindle at 720 ℃; the time is 2 hours; and (3) protecting by hydrogen-nitrogen mixed gas, wherein the thickness of the extruded plate is 20mm, and the width of the extruded plate is 60 mm.
And sixthly, cleaning and brushing the plate and compounding the plate with the silver plate. The thermal composite deformation is 70%, the temperature is 750 ℃, the protection is realized by N2, the width of the Ag layer is 60mm, and the thickness is 2 mm. The composite effect can be further enhanced by adopting the brushing.
And seventhly, performing heat treatment on the composite material belt, wherein the parameters can adopt: the temperature is 750 ℃, the time is 12 hours, and the nitrogen-hydrogen mixed gas is used for protection.
And eighthly, carrying out cold rolling and punching again on the heat-treated material belt, wherein the single-pass deformation of the cold rolling is controlled to be 20%, and the final thickness of the material belt is 2.0 mm.
Ninthly, internally oxidizing the punched sheet at the oxidation temperature of 700 ℃; controlling the oxygen pressure at 0.8 Mpa; the oxidation time was 55 h.
Step ten, cleaning the sheet after internal oxidation to obtain fine, uniform and quickly-oxidizable high-performance AgSnO2-In2O3An electrical contact material.
The embodiment finally obtains the silver tin oxide indium oxide electric contact material which has fine and uniform crystal grains and can quickly oxidize high performance. Wherein, the oxidation speed is improved by 32 percent compared with the traditional process. The electric service life of the contact is improved by 10 percent compared with the traditional contact, the particles are uniform and fine, the welding surface is flat, and the welding performance is better.
Example two
To prepare Ag (80) SnO2-In2O3Example of electrical contact materials
Firstly, smelting and ingoting Ag ingots, Sn ingots, In ingots and additive Cu elements. Wherein the Ag content is 83.5 wt%, the Sn content is 12 wt%, the In content is 4 wt%, and the additive Cu is 0.5 wt%.
And secondly, atomizing the alloy melt smelted in the first step, wherein the pressure of atomizing gas is 10 Mpa.
Thirdly, sieving and isostatic pressing the atomized powder, and sieving the powder by a sieve with the mesh number of 100; isostatic pressure 200MPa, dwell time 30 s.
Fourthly, sintering the obtained spindle at the temperature of 650 ℃; the time is 7 hours; h2 gas shield.
Fifthly, carrying out hot extrusion on the sintered spindle at the temperature of 600 ℃; the time is 4 hours; charcoal protection, in which the extruded sheet is 15mm thick and 60mm wide.
And sixthly, cleaning and brushing the plate and compounding the plate with the silver plate. The thermal composite deformation is 40%, the temperature is 500 ℃, the Ar protection is carried out, the width of the Ag layer is 60mm, and the thickness is 1 mm.
And seventhly, performing heat treatment on the composite material belt, wherein the parameters can adopt: the temperature is 450 ℃, the time is 6 hours, and the N2 is protected by gas.
And eighthly, carrying out cold rolling and punching again on the heat-treated material belt, wherein the single-pass deformation of the cold rolling is controlled to be 5%, and the final thickness of the material belt is 1.5 mm.
Ninthly, internally oxidizing the punched sheet at the temperature of 630 ℃; controlling the oxygen pressure at 5 Mpa; the oxidation time is 40 h.
Step ten, cleaning the sheet after internal oxidation to obtain fine, uniform and quickly-oxidizable high-performance AgSnO2-In2O3An electrical contact material.
The embodiment finally obtains the silver tin oxide indium oxide electric contact material which is fine, uniform and can quickly oxidize high performance. Wherein, the oxidation speed is improved by 35 percent compared with the traditional process. The welding surface is smooth, the welding performance is good, the electric service life of the contact is prolonged by 15 percent compared with the traditional contact, and the particles are uniform and fine.
EXAMPLE III
To prepare Ag (90) SnO2-In2O3Example of electrical contact materials
Firstly, smelting and ingoting Ag ingots, Sn ingots, In ingots and additives of Ni and Cu. Wherein the Ag content is 93 wt%, the Sn content is 4.5 wt%, the In content is 1.5 wt%, the additive Ni is 0.5 wt%, and the Cu content is 0.5 wt%.
And secondly, atomizing the alloy melt smelted in the first step, wherein the pressure of atomizing gas is 5 Mpa.
Thirdly, sieving and isostatic pressing the atomized powder, and sieving the powder with a 200-mesh sieve; isostatic pressure 100MPa, dwell time 70 s.
Fourthly, sintering the obtained spindle at the temperature of 750 ℃; the time is 5 hours; h2 gas shield.
Fifthly, hot extruding the sintered spindle at 680 ℃; the time is 3 hours; charcoal protection, in which the extruded sheet is 10mm thick and 70mm wide.
And sixthly, cleaning and brushing the plate and compounding the plate with the silver plate. The thermal composite deformation is 60%, the temperature is 600 ℃, the Ar protection is carried out, the width of the Ag layer is 70mm, and the thickness is 1.5 mm.
And seventhly, performing heat treatment on the composite material belt, wherein the parameters can adopt: the temperature is 630 ℃, the time is 8 hours, and the N2 is protected by gas.
And eighthly, cold rolling and punching the heat-treated material belt again, wherein the single-pass deformation of the cold rolling is controlled to be 15%, and the final thickness of the material belt is 2.5 mm.
Ninthly, internally oxidizing the punched sheet at the temperature of 580 ℃; controlling the oxygen pressure at 2 Mpa; the oxidation time was 95 h.
Step ten, cleaning the sheet after internal oxidation to obtain fine, uniform and quickly-oxidizable high-performance AgSnO2-In2O3An electrical contact material.
The embodiment finally obtains the silver tin oxide indium oxide electric contact material which is fine, uniform and can quickly oxidize high performance. Wherein, the oxidation speed is improved by 31 percent compared with the traditional process. The welding surface is smooth, the welding performance is good, the electric service life of the contact is prolonged by 20 percent compared with the traditional contact, and the particles are uniform and fine.
Example four
To prepare Ag (90) SnO2-In2O3Example of electrical contact materials
Firstly, smelting and ingoting Ag ingots, Sn ingots, In ingots and additive Zn elements. Wherein the Ag content was 93 wt%, the Sn content was 4.5 wt%, and the In content was 2.5 wt%.
And secondly, atomizing the alloy melt smelted in the first step, wherein the pressure of atomizing gas is 10 Mpa.
Thirdly, sieving and isostatic pressing the atomized powder, and sieving the powder by a sieve with the mesh number of 100; isostatic pressure 100MPa, dwell time 70 s.
Fourthly, sintering the obtained spindle at 800 ℃; the time is 5 hours; h2 gas shield.
Fifthly, hot extruding the sintered spindle at 700 ℃; the time is 3 hours; charcoal protection, in which the extruded sheet is 10mm thick and 70mm wide.
And sixthly, cleaning and brushing the plate and compounding the plate with the silver plate. The thermal composite deformation is 60%, the temperature is 620 ℃, the Ar protection is carried out, the width of the Ag layer is 70mm, and the thickness is 1.5 mm.
And seventhly, performing heat treatment on the composite material belt, wherein the parameters can adopt: the temperature is 630 ℃, the time is 6 hours, and the N2 is protected by gas.
And eighthly, cold rolling and punching the heat-treated material belt again, wherein the single-pass deformation of the cold rolling is controlled to be 15%, and the final thickness of the material belt is 2.5 mm.
Ninthly, internally oxidizing the punched sheet at 670 ℃; controlling the oxygen pressure at 2 Mpa; the oxidation time was 35 h.
Step ten, cleaning the sheet after internal oxidation to obtain fine, uniform and quickly-oxidizable high-performance AgSnO2-In2O3An electrical contact material.
The embodiment finally obtains the silver tin oxide indium oxide electric contact material which is fine, uniform and can quickly oxidize high performance. Wherein, the oxidation speed is improved by 50 percent compared with the traditional process. The welding surface is smooth, the welding performance is good, the electric service life of the contact is improved by 40 percent compared with the traditional contact, and the particles are uniform and fine.
As shown in figure 1, is conventional internal oxidation AgSnO2(9)-In2O3(4) The metallographic structure had coarse and uneven grains. The internal oxidation parameters are 680 ℃, 1.5MPa, 1.8mm thickness and the complete oxidation time is 75 h.
As shown in FIG. 2, AgSnO was prepared for the preparation of the examples of the present invention2(9)-In2O3(4) The metallographic structure is fine and uniform in particles; internal oxidation parameters of 680 ℃, 1.5Mpa, 1.8mm thickness and complete oxidation time of 50 h.
The above is an example of adding the element X, and the addition of the element X can improve the product performance, so the above are all preferred embodiments of the present invention, and of course, the rapid silver oxide, tin oxide, indium oxide electrical contact material can also be obtained without adding the element X, and all the steps and operations and principles are the same as those of the above example, which is easily understood by those skilled in the art, and are not described herein again.
In conclusion, the embodiment of the invention has the advantages of simple process, convenient operation, low cost, no special requirement on equipment, uniform and fine prepared electrical contact material and tissue structure, long electrical service life, wide application in low-voltage electrical appliances and low temperature rise. Meanwhile, the method can realize rapid oxidation, has high production efficiency, and shortens the internal oxidation time by more than 30 percent compared with the traditional method.
The above description is only a few preferred embodiments of the present invention, and does not limit the technical scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A preparation method of a rapid silver oxide tin oxide indium oxide electric contact material is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing an AgSnIn or AgSnInX spindle by adopting a powder isostatic pressing method, wherein X is any element capable of forming an alloy with Ag and Sn and improving the electrical property of the Ag and Sn;
s2, sintering the AgSnIn or AgSnInX spindle to prepare an AgSnIn or AgSnInX plate;
s3, compounding the AgSnIn or AgSnInX board and a silver board to obtain a compounded board;
s4, performing heat treatment and cold rolling on the composite plate, and punching the plate into a sheet;
s5, carrying out internal oxidation on the sheet to obtain the rapid silver oxide, tin oxide and indium oxide electric contact material;
in S1, the AgSnIn or AgSnInX spindle prepared by the powder isostatic pressing method comprises the following steps:
smelting an Ag ingot, an Sn ingot and an In ingot, or smelting the Ag ingot, the Sn ingot, the In ingot and an X element to obtain an alloy solution;
atomizing the alloy solution to prepare powder to obtain AgSnIn or AgSnInX powder;
sieving and isostatic pressing the AgSnIn or AgSnInX powder to prepare an AgSnIn or AgSnInX spindle;
the smelting is carried out, wherein: the Ag content is 83.5-93.5%, the Sn content is 4.5-12%, the In content is 1.5-4%, wherein the total content of X is less than or equal to 1.0%; the content here is wt%;
the atomizing pulverization, wherein: the pressure of the atomizing gas is between 1.0MPa and 10 MPa;
said sieving and isostatic pressing, wherein: the mesh number of the sieve is between 100 and 600 meshes, and the isostatic pressure is between 70 and 200 MPa.
2. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 1, wherein the method comprises the following steps: s2, the sintering, wherein: temperature between 650 ℃ and 820 ℃ and H2Or hydrogen-nitrogen mixed gas protection.
3. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 1, wherein the method comprises the following steps: and S2, sintering the AgSnIn or AgSnInX spindle, and then preparing the AgSnIn or AgSnInX plate by adopting an extrusion process.
4. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 3, wherein the method comprises the following steps: the extrusion, wherein: the temperature is 600-720 ℃, and the charcoal or the hydrogen-nitrogen mixed gas is used for protection.
5. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 1, wherein the method comprises the following steps: in S3, compounding the AgSnIn or AgSnInX sheet with a silver plate, wherein: the thermal composite deformation is between 40 and 70 percent, the temperature is controlled between 500 and 750 ℃, and N2Or Ar protection.
6. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 1, wherein the method comprises the following steps: and S4, performing heat treatment on the composite plate, wherein: the temperature is between 450 and 750 ℃, and N is introduced2Or nitrogen-hydrogen mixed gas protection.
7. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 1, wherein the method comprises the following steps: and S4, cold rolling, wherein the single-pass deformation amount of the cold rolling is controlled to be between 5 and 20 percent.
8. The method for preparing the rapid silver oxide tin oxide indium oxide electrical contact material according to claim 1, wherein the method comprises the following steps: in S5, internally oxidizing the sheet, wherein: the oxidation temperature is 580-700 ℃, and the oxygen pressure is controlled between 0.8MPa and 5 MPa.
9. A tin oxide indium oxide electric contact material capable of rapidly oxidizing silver is characterized in that: prepared by the process according to any one of claims 1 to 8.
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