CN109593981B - Preparation method of silver tin oxide contact material for improving sintering property of ingot blank - Google Patents
Preparation method of silver tin oxide contact material for improving sintering property of ingot blank Download PDFInfo
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- CN109593981B CN109593981B CN201811590827.7A CN201811590827A CN109593981B CN 109593981 B CN109593981 B CN 109593981B CN 201811590827 A CN201811590827 A CN 201811590827A CN 109593981 B CN109593981 B CN 109593981B
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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
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/056—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using gas
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
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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
Abstract
The invention discloses a preparation method of a silver tin oxide contact material for improving the sintering property of an ingot blank, which comprises the following steps: 1) calculating and weighing silver, tin and additives with the same application amount according to the material ratio of the silver tin oxide contact to be prepared, melting and atomizing to prepare powder to obtain silver-tin alloy powder; 2) oxidizing the silver-tin alloy powder to obtain silver-tin oxide composite powder; 3) carrying out wet grinding on the silver tin oxide composite powder under the protective atmosphere condition to obtain ball-milled silver tin oxide composite powder; 4) molding the ball-milled silver tin oxide composite powder to obtain a silver tin oxide blank; 5) sintering the obtained silver tin oxide blank under the conditions that the oxygen partial pressure is more than or equal to 0.8Mpa and the temperature is 900-960 ℃ to obtain a silver tin oxide ingot blank; 6) and carrying out hot extrusion on the obtained silver tin oxide ingot blank to obtain a silver tin oxide wire or strip. The silver tin oxide contact material prepared by the method has uniform tissue and good processing performance.
Description
Technical Field
The invention relates to a preparation method of a silver tin oxide contact, in particular to a preparation method of a silver tin oxide contact material for improving the sintering property of an ingot blank.
Background
The electric contact is a core component of various high and low switches, electric appliances, instruments and meters and components, and is widely applied to high-capacity alternating current and direct current contactors, alternating current and direct current power relays, automobile electric appliances and medium and small-capacity low-voltage circuit breakers in the industrial fields of aerospace, aviation, automobiles and the like and the civil industry. Electrical contacts are of a wide variety and are commonly used in silver-based alloys and copper-based alloys. Among silver-based alloys, silver cadmium oxide contact materials have good arc wear resistance, fusion welding resistance, electrical conductivity, and thermal conductivity, and are called "universal contact materials" because of low contact resistance and high stability. However, the silver cadmium oxide material has the harm of cadmium toxicity in the production, use and recovery processes, so the development and development of novel environment-friendly materials with good electrical contact performance become the hot topic in the field.
Silver tin oxide (AgSnO)2) The contact material has good fusion welding resistance and arc ablation resistance, is nontoxic and environment-friendly, and is the most promising contact material for replacing silver cadmium oxide. The methods for preparing silver tin oxide contact materials are roughly classified into powder metallurgy (e.g., patent publications CN101202169A and CN 101649399A), internal oxidation (e.g., patent publications CN1042010208A and CN 103700544A), chemical coprecipitation (e.g., patent publication CN 102528055A), and atomization. Among them, the powder metallurgy method and the internal oxidation method are the mainstream preparation methods of the silver tin oxide contact material. However, these methods have drawbacks: powder metallurgy processThe prepared material has low density, large contact resistance and high temperature; the surface and the internal structure of the material prepared by the internal oxidation method are not uniform, the oxide particles are seriously aggregated, and a lean oxidation layer is arranged in the middle; the chemical coprecipitation method has the problems of complex process, chemical pollution generated in the preparation process and the like. The atomization method process combines the advantages of a powder metallurgy method and an internal oxidation method, is suitable for mass production, has good application prospect, but improves the production efficiency of the silver tin oxide and brings some defects, such as difficult powder oxidation and sintering, poor processing performance and the like.
The traditional process flow of the atomization method is roughly as follows: smelting, atomizing to prepare powder, oxidizing alloy powder, isostatic pressing, sintering, hot extrusion, drawing and finally preparing the finished product. Wherein SnO is generated in the oxidation stage of alloy powder2Has a thermodynamic stability higher than that of Ag2Because of O, Sn is oxidized preferentially to Ag. SnO2Segregation occurs on the surface of powder particles, and the contact and diffusion of Ag among the powder are hindered in the subsequent sintering process, so that the problems of difficult sintering of a blank, poor processing performance and the like are caused.
By searching the prior art, the invention patent with the publication number of CN101707153A discloses a preparation method of a fine-particle tin oxide reinforced silver-based electrical contact material. The method comprises the steps of firstly, sieving AgSn alloy powder and an additive, then placing the AgSn alloy powder and the additive into a high-energy ball mill, carrying out ball milling in an oxygen-gas atmosphere, enabling the pre-oxidation and ball milling dispersion processes of the AgSn alloy powder to be carried out synchronously, then carrying out annealing treatment and isostatic pressing forming on the powder after ball milling, sintering an obtained blank in the oxygen atmosphere, and finally carrying out hot pressing, re-sintering and hot extrusion on the sintered blank to obtain the strip or wire. The invention points out that the mechanical alloying is combined with a high-pressure normal-temperature pre-oxidation method, so that the surface of fresh AgSn alloy powder is continuously exposed in the mechanical alloying process, thereby promoting the AgSn alloy powder to be continuously combined with oxygen and accelerating the oxidation process under huge high-energy impact; and oxidation of the obtained SnO2The particles are dispersed in the Ag matrix. However, it is well known to those skilled in the art that high energy ball milling under oxygen pressure tends to agglomerate the AgSn alloy powder with additives, thereby affecting the materialUniformity of texture.
The invention patent with the publication number of CN101202169A discloses a method for manufacturing a novel silver tin oxide wire material electric contact material. The method comprises the steps of melting raw materials of silver, tin and additives in a certain proportion in a medium-frequency smelting furnace, carrying out high-pressure alloy atomization through a high-pressure water atomization device, drying and oxidizing and tempering atomized alloy powder, forming an isostatic pressing ingot blank through isostatic pressing, sintering the ingot blank in a heating furnace, conveying the sintered ingot blank to an extruder to extrude wires, and processing the extruded wires into finished products through a hot drawing mode. As mentioned above, SnO is generated in the oxidation stage of alloy powder2Has a thermodynamic stability higher than that of Ag2O, Sn is oxidized preferentially to Ag, SnO2The surface of the powder particles is subjected to segregation, and the contact and diffusion of Ag among the powder particles are hindered in the subsequent sintering process, so that the problems of difficult sintering of a blank, poor processing performance and the like exist.
Disclosure of Invention
The invention aims to provide a preparation method of a silver tin oxide contact material for improving the sinterability of an ingot blank. The method wetly grinds the oxidized silver tin oxide composite powder under the atmosphere protection condition and then forms the silver tin oxide composite powder, and the obtained blank is sintered under the conditions of specific oxygen pressure and ultrahigh temperature, so that the sinterability of the obtained ingot blank is effectively improved, and the silver tin oxide contact material with uniform tissue and good processing performance is obtained.
To solve the above technical problems, the present invention provides
The preparation method of the silver tin oxide contact material for improving the sintering property of the ingot blank comprises the following steps:
1) calculating the required silver, tin and additive amount according to the material ratio of the silver tin oxide contact to be prepared, weighing the silver, tin and additive with corresponding amount, melting and atomizing to prepare powder to obtain silver-tin alloy powder;
2) oxidizing the silver-tin alloy powder to obtain silver-tin oxide composite powder;
3) placing the silver tin oxide composite powder in a ball mill, carrying out wet milling under the condition of protective atmosphere, and drying the obtained powder after the wet milling is finished to obtain the ball-milled silver tin oxide composite powder;
4) molding the ball-milled silver tin oxide composite powder to obtain a silver tin oxide blank;
5) sintering the obtained silver tin oxide blank under the conditions that the oxygen partial pressure is more than or equal to 0.8Mpa and the temperature is 900-960 ℃ to obtain a silver tin oxide ingot blank;
6) and carrying out hot extrusion on the obtained silver tin oxide ingot blank to obtain a silver tin oxide wire or a silver tin oxide strip.
In the step 1) of the preparation method, in the obtained silver-tin alloy powder, the additive accounts for 0-5% by mass, the tin accounts for 1-20% by mass, and the balance is silver. Preferably, the additive accounts for 0.1-2%, the tin accounts for 1-20%, and the balance is silver. The additive may be selected In the same manner as In the prior art, and may be one or a combination of two or more selected from Cu, Bi, In, Ni, Zn, Sb and Te. In the step, the raw materials of silver, tin and additives can be in the form of pure metal ingots or pure metal powder, for example, Ag can be pure Ag blocks or pure Ag powder.
In the step 2) of the preparation method, the operation during oxidation is the same as that in the prior art, and specifically, the silver-tin alloy powder is placed in a high-pressure oxidation furnace and oxidized for 4-8 hours under the conditions that the oxygen partial pressure is 0.5-2 MPa and the temperature is 600-800 ℃. And crushing the material obtained after oxidation to obtain the silver-tin oxide composite powder.
In step 3) of the above production method, it is usually required to wet-grind the resulting powder to a particle size of 5 μm or less, preferably to wet-grind the resulting powder to a particle size of 2 μm or less, and more preferably to wet-grind the resulting powder to a particle size of 1 μm or less. The ball milling medium, the ball material mass ratio, the ball milling time and the like in the wet milling are the same as those in the prior art, and preferably, the ball material mass ratio is 3-10: 1, a ball milling medium is absolute ethyl alcohol, and the mass ratio of the medium to the material is 0.5-2: 1, the ball milling speed is 250-500 rmp, and the ball milling time is 6-15 h. The protective atmosphere is usually N2Or an inert gas (e.g., Ar, etc.). Drying the powder obtained after wet grinding is usually carried out at the temperature of 80-100 ℃, and the time is usually 6-10 h.
In the step 4) of the preparation method, the silver-tin oxide composite powder after ball milling is molded by adopting the prior conventional technology to obtain a silver-tin oxide blank, the silver-tin oxide composite powder after ball milling is generally molded on an isostatic press, the isostatic pressure is controlled to be 50-200 MPa, the pressure maintaining time is 10-200 s,
in the step 5) of the preparation method, the sintering time is usually controlled to be 4-10 h. In order to further improve the processing performance of the obtained ingot blank, the sintering is preferably carried out under the conditions that the oxygen partial pressure is 1-2 Mpa and the temperature is 950-960 ℃, and the sintering time is preferably controlled to be 6-8 h.
In the step 6) of the preparation method, the operation of hot extrusion is the same as that of the prior art, specifically, the temperature of hot extrusion is 830-900 ℃, and the extrusion ratio is 190-270. After obtaining the silver tin oxide wire or the silver tin oxide strip, the required silver tin oxide contact is manufactured according to the conventional process. For example, the wire or the strip is subjected to drawing (or rolling and compounding) for multiple times, annealing processing is carried out to the required size, and then the wire or the strip is processed (or punched by a punch) by a riveting machine to form the rivet-type (or sheet-type) contact.
Compared with the prior art, the invention is characterized in that:
1. placing the formed silver tin oxide blank under the conditions that the oxygen partial pressure is more than or equal to 0.8Mpa and the temperature is 900-960 ℃, particularly sintering under the conditions that the oxygen partial pressure is 1-2 Mpa and the temperature is 950-960 ℃, and utilizing the characteristic that the melting point of silver rises along with the increase of pressure, the melting point of silver in the technical scheme of the invention is more than 962 ℃ (the melting point of silver is 962 ℃ under the standard atmospheric pressure), so that the ingot blank does not melt in the ultra-high temperature sintering process (under the standard atmospheric pressure, when the sintering temperature of the silver tin oxide ingot blank reaches 960 ℃, the melting phenomenon can occur, even when the sintering temperature of the silver tin oxide ingot blank is more than 950 ℃); on the other hand, the mutual sintering diffusion effect among the silver tin oxide particles can be enhanced by sintering under the condition of ultrahigh temperature and high pressure, and the formation of sintering necks among the particles is promoted (according to the traditional sintering theory, the closer the sintering temperature is to the melting point of a substance, the more excellent sintering performance is obtained by sintering the substance), so that the processing performance of the material is improved, and further, the silver tin oxide ingot blank with high ductility is obtained.
2. Oxidizing the atomized silver-tin alloy powder, then placing the oxidized silver-tin alloy powder into a ball mill to carry out high-energy wet grinding under the atmosphere protection condition, and crushing SnO in the oxidation process2Hard shells formed by segregation are generated on the surfaces of the powder particles, so that metal bases in the powder particles are continuously exposed, the sintering promotion effect is achieved, and the processing performance of the ingot blank is further improved; on the other hand, the particle size is refined and crushed, the agglomeration phenomenon can not be generated, the problem of surface oxidation of powder particles can not be caused, a large number of microcracks can be generated in the wet grinding process of the particles, and a diffusion channel of oxygen is added for the subsequent oxidation process, so that the diffusion rate of oxygen atoms of the particles to the interior of the powder particles in the subsequent high-pressure rapid oxidation process is greater than the diffusion rate of tin atoms from the interior of the particles to the boundary, the enrichment of tin oxide on the particle surface is reduced, and the uniformity of material organization is improved.
3. The method is simple and easy to control, and is suitable for industrial production.
Drawings
FIG. 1 is a picture of a silver tin oxide ingot blank object obtained by sintering in step 5) in example 1 of the present invention;
FIG. 2 is a fracture morphology chart and a metallographic structure of a silver tin oxide ingot blank sintered in step 5) in example 1 of the present invention, wherein (a) is the fracture morphology chart, and (b) is the metallographic structure;
FIG. 3 is a picture of a silver tin oxide ingot blank object obtained by sintering in step 5) in comparative example 1 of the present invention;
FIG. 4 is a picture of a silver tin oxide ingot blank object obtained by sintering in step 5) in comparative example 2 of the present invention;
FIG. 5 is a fracture morphology chart and a metallographic structure of the silver tin oxide ingot blank sintered in step 5) in comparative example 2 of the present invention, wherein (a) is the fracture morphology chart, and (b) is the metallographic structure;
FIG. 6 is a fracture morphology chart and a metallographic structure of silver tin oxide ingots obtained by sintering in step 5) in examples 2 and 3, wherein (a) is the fracture morphology chart of example 2, and (b) is the fracture morphology chart of example 3.
Detailed Description
The present invention will be better understood from the following detailed description of specific examples, which should not be construed as limiting the scope of the present invention.
Example 1
1) Weighing the components according to the following mass percentage, placing the components in a medium-frequency induction smelting furnace to be smelted into uniform alloy melt, then atomizing the alloy melt by high-pressure water atomization equipment, drying the obtained powder slurry, and sieving the powder slurry by a 200-mesh sieve to obtain silver-tin alloy powder;
Sn：9.5％；
addition of: 0.1 percent of Bi;
the balance of Ag;
2) placing silver-tin alloy powder in a high-pressure oxidation furnace, oxidizing for 6h under the conditions that the oxygen partial pressure is 1MPa and the temperature is 700 ℃, taking out, crushing, and sieving by a 100-mesh sieve to obtain silver-tin oxide composite powder;
3) placing the silver tin oxide composite powder in a high-energy ball mill, carrying out wet grinding treatment under the protection of an atmosphere (Ar) until the particle size of the obtained powder is 1-2 mu m, and drying the powder subjected to wet grinding in an oven at the temperature of 80 ℃ for 10h to obtain the ball-milled silver tin oxide composite powder; during wet grinding, the ball material mass ratio is 8: 1, the ball milling medium is absolute ethyl alcohol, and the mass ratio of the medium to the material is 0.8: 1, ball milling rotation speed is 500rmp, and ball milling time is 15 h;
4) placing the ball-milled silver tin oxide composite powder on an isostatic press for molding, controlling the isostatic pressure to be 50MPa, and keeping the pressure for 200s to obtain a silver tin oxide green body;
5) placing the silver tin oxide blank into a high-pressure oxidation furnace, and sintering for 6h under the conditions that the oxygen partial pressure is 0.8MPa and the temperature is 960 ℃, so as to obtain a silver tin oxide ingot blank, wherein the material object is shown in figure 1, and as can be seen from the figure, the surface of the silver tin oxide ingot blank obtained by sintering already has metallic luster, which indicates that the sintering densification effect of the blank is good; the fracture morphology and the metallographic structure of the obtained silver tin oxide ingot blank are respectively shown in FIGS. 2(a) and 2 (b);
6) the silver tin oxide ingot blank is processed into a wire by hot extrusion, and the wire is processed into a rivet type contact by a riveting machine after being drawn and annealed for a plurality of times to a required size.
Comparative example 1
Example 1 was repeated except that:
5) and (3) placing the silver tin oxide blank into a high-pressure oxidation furnace, and heating to 960 ℃ under the condition of standard atmospheric pressure for sintering for 6 hours. As a result: the silver base in the obtained ingot had melted (since the melting point of silver at 1 atm was 961 ℃, the sintered ingot would certainly melt at 960 ℃, and thus an acceptable silver tin oxide ingot could not be obtained), and the obtained ingot was as shown in fig. 3. That is, in this example, a satisfactory silver tin oxide ingot for the subsequent step was not obtained.
Comparative example 2
Example 1 was repeated except that:
5) and (3) placing the silver tin oxide blank into a high-pressure oxidation furnace, and heating to 930 ℃ under the standard atmospheric pressure condition for sintering for 6 h. As a result: an ingot of silver tin oxide was obtained, shown in fig. 4, but the surface of the obtained ingot was still dark gray, indicating that the sintering densification of the ingot at 930 ℃ was very undesirable. The fracture morphology and the metallographic structure of the obtained silver tin oxide ingot are shown in fig. 5(a) and 5(b), respectively.
As can be seen from a comparison of FIGS. 5 and 2, the ingot of silver tin oxide obtained in step 5) of comparative example 2 has almost no sintering of the powders together, the fracture is brittle and separates along the boundaries of the powder grains, the fracture surface retains the characteristics of the original powder grains, and a large amount of SnO is distributed on the grain surface2The grain, the composition analysis of the inside of the large grain (or grain) shows that the tin content in the inside is extremely low, and most of the tin is enriched to the surface of the powder grain. Example 1 the powder in the ingot of silver tin oxide obtained in step 5) has been completely sintered together, a compact structure is formed, fracture of the ingot is characterized by plastic fracture with a large number of pits, and the original powder particles are hardly distinguished on the fracture surface. SnO2The particles are distributed not only on the grain boundary but also in the interior of the crystal grains in a large amount, which remarkably improves the distribution state of the second phase particles and is beneficial to the improvement of the processing property, the plasticity and the electrical property of the material.
Example 2
1) Weighing the components according to the following mass percentage, placing the components in a medium-frequency induction smelting furnace to be smelted into uniform alloy melt, then atomizing the alloy melt by high-pressure water atomization equipment, drying the obtained powder slurry, and sieving the powder slurry by a 200-mesh sieve to obtain silver-tin alloy powder;
Sn：8％；
addition of: in 1%, Cu 1% and Ni 1%;
the balance of Ag;
2) placing silver-tin alloy powder in a high-pressure oxidation furnace, oxidizing for 4h under the conditions that the oxygen partial pressure is 2MPa and the temperature is 800 ℃, taking out, crushing, and sieving by a 100-mesh sieve to obtain silver-tin oxide composite powder;
3) placing the silver tin oxide composite powder in a high-energy ball mill, carrying out wet grinding treatment under the protection of an atmosphere (Ar) until the particle size of the obtained powder is 2-4 mu m, and placing the powder after the wet grinding in an oven to dry for 6h at the temperature of 100 ℃ to obtain the silver tin oxide composite powder after ball grinding; during wet grinding, the ball material mass ratio is 3: 1, the ball milling medium is absolute ethyl alcohol, and the mass ratio of the medium to the material is 1: 1, ball milling rotation speed is 250rmp, and ball milling time is 10 h;
4) placing the ball-milled silver tin oxide composite powder on an isostatic press for molding, controlling the isostatic pressure to be 100MPa, and keeping the pressure for 10s to obtain a silver tin oxide green body;
5) placing the silver tin oxide blank in a high-pressure oxidation furnace, and sintering for 6h under the conditions that the oxygen partial pressure is 2MPa and the temperature is 960 ℃ to obtain a silver tin oxide ingot blank; the fracture morphology is shown in FIG. 6 (a);
6) the silver tin oxide ingot blank is processed into a plate by hot extrusion, and the plate is processed into a sheet contact by a punch after being rolled and annealed for a plurality of times to the required size.
Example 3
1) Weighing the components according to the following mass percentage, placing the components in a medium-frequency induction smelting furnace to be smelted into uniform alloy melt, then atomizing the alloy melt by high-pressure water atomization equipment, drying the obtained powder slurry, and sieving the powder slurry by a 200-mesh sieve to obtain silver-tin alloy powder;
Sn：10％；
addition of: zn 2%;
the balance of Ag;
2) placing silver-tin alloy powder in a high-pressure oxidation furnace, oxidizing for 8 hours under the conditions that the oxygen partial pressure is 0.5MPa and the temperature is 800 ℃, taking out, crushing, and sieving by a 100-mesh sieve to obtain silver-tin oxide composite powder;
3) placing the silver tin oxide composite powder in a high-energy ball mill, carrying out wet grinding treatment under the protection of an atmosphere (Ar) until the particle size of the obtained powder is 3-5 mu m, and placing the powder after the wet grinding in an oven to dry for 9h at the temperature of 90 ℃ to obtain the silver tin oxide composite powder after ball grinding; during wet grinding, the ball material mass ratio is 5: 1, the ball milling medium is absolute ethyl alcohol, and the mass ratio of the medium to the material is 10: 1, ball milling rotation speed is 400rmp, and ball milling time is 10 h;
4) placing the ball-milled silver tin oxide composite powder on an isostatic press for molding, controlling the isostatic pressure to be 80MPa, and keeping the pressure for 100s to obtain a silver tin oxide green body;
5) placing the silver tin oxide blank in a high-pressure oxidation furnace, and sintering for 4h under the conditions that the oxygen partial pressure is 1MPa and the temperature is 960 ℃ to obtain a silver tin oxide ingot blank; the fracture morphology is shown in FIG. 6 (b);
6) the silver tin oxide ingot blank is processed into a wire by hot extrusion, and the wire is processed into a rivet type contact by a riveting machine after being drawn and annealed for a plurality of times to a required size.
Example 4
1) Weighing the components according to the following mass percentage, placing the components in a medium-frequency induction smelting furnace to be smelted into uniform alloy melt, then atomizing the alloy melt by high-pressure water atomization equipment, drying the obtained powder slurry, and sieving the powder slurry by a 200-mesh sieve to obtain silver-tin alloy powder;
Sn：20％；
addition of: sb 3% and Te 2%;
the balance of Ag;
step 2), 3), 4) are the same as in example 3;
5) placing the silver tin oxide blank in a high-pressure oxidation furnace, and sintering for 10h under the conditions that the oxygen partial pressure is 1MPa and the temperature is 900 ℃ to obtain a silver tin oxide ingot blank;
6) the silver tin oxide ingot blank is processed into a wire by hot extrusion, and the wire is processed into a rivet type contact by a riveting machine after being drawn and annealed for a plurality of times to a required size.
Example 5
1) Weighing the components according to the following mass percentage, placing the components in a medium-frequency induction smelting furnace to be smelted into uniform alloy melt, then atomizing the alloy melt by high-pressure water atomization equipment, drying the obtained powder slurry, and sieving the powder slurry by a 200-mesh sieve to obtain silver-tin alloy powder;
Sn：12％；
addition of: 0 percent;
the balance of Ag;
step 2), 3), 4) are the same as in example 3;
5) placing the silver tin oxide blank in a high-pressure oxidation furnace, and sintering for 6h under the conditions that the oxygen partial pressure is 1MPa and the temperature is 950 ℃ to obtain a silver tin oxide ingot blank;
6) the silver tin oxide ingot blank is processed into a wire by hot extrusion, and the wire is processed into a rivet type contact by a riveting machine after being drawn and annealed for a plurality of times to a required size.
The bending strength and other properties of the silver tin oxide ingot produced in step 5) of examples 1 to 5 and the silver tin oxide ingot produced in comparative example 2 were measured, and the results are shown in table 1 below:
table 1:
Claims (7)
1. a preparation method of a silver tin oxide contact material for improving the sinterability of an ingot blank comprises the following steps:
1) calculating the required silver, tin and additive amount according to the material ratio of the silver tin oxide contact to be prepared, weighing the silver, tin and additive with corresponding amount, melting and atomizing to prepare powder to obtain silver-tin alloy powder;
2) oxidizing the silver-tin alloy powder to obtain silver-tin oxide composite powder;
3) placing the silver tin oxide composite powder in a ball mill, carrying out wet milling under the condition of protective atmosphere, and drying the obtained powder after the wet milling is finished to obtain the ball-milled silver tin oxide composite powder;
4) molding the ball-milled silver tin oxide composite powder to obtain a silver tin oxide blank;
5) sintering the obtained silver tin oxide blank under the conditions that the oxygen partial pressure is 0.8-2 MPa and the temperature is 950-960 ℃ to obtain a silver tin oxide ingot blank;
6) and carrying out hot extrusion on the obtained silver tin oxide ingot blank to obtain a silver tin oxide wire or a silver tin oxide strip.
2. The method of claim 1, wherein: in the step 1), in the obtained silver-tin alloy powder, the additive accounts for 0-5% by mass, the tin accounts for 1-20% by mass, and the balance is silver.
3. The method of claim 1, wherein: in the step 1), the additive is one or a combination of more than two selected from Cu, Bi, In, Ni, Zn, Sb and Te.
4. The method of claim 1, wherein: in the step 3), wet grinding is carried out until the grain diameter of the obtained powder is less than or equal to 5 mu m.
5. The production method according to any one of claims 1 to 4, characterized in that: in the step 5), the sintering time is 4-10 h.
6. The method of claim 5, wherein: in the step 5), sintering is carried out under the condition that the oxygen partial pressure is 1-2 MPa.
7. The method of claim 6, wherein: in the step 5), the sintering time is 6-8 h.
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| CN115570139B (en) * | 2022-10-12 | 2023-08-15 | 浙江福达合金材料科技有限公司 | Preparation method of silver tin oxide electric contact material |
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| JPH07173555A (en) * | 1993-12-17 | 1995-07-11 | Higashifuji Seisakusho:Kk | Silver-tin oxide sintered electrical contact material excellent in melt sticking and wear resistance |
| CN1443864A (en) * | 2003-04-17 | 2003-09-24 | 章景兴 | Silver tin-oxide zinc-oxide alloy electric contact and its production process |
| JP5484210B2 (en) * | 2010-06-15 | 2014-05-07 | 田中貴金属工業株式会社 | Ag-oxide based electrical contact material and automotive relay using the same |
| CN103639232B (en) * | 2013-12-06 | 2016-04-27 | 桂林电器科学研究院有限公司 | A kind of preparation method of AgSnO2 wire |
| CN104498762B (en) * | 2014-12-30 | 2016-08-10 | 桂林电器科学研究院有限公司 | A kind of processing method of the siller tin oxide electric contact material containing additive |
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