CN102312119B - Preparation method for silver tin oxide electrical contact material - Google Patents
Preparation method for silver tin oxide electrical contact material Download PDFInfo
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- CN102312119B CN102312119B CN 201010218545 CN201010218545A CN102312119B CN 102312119 B CN102312119 B CN 102312119B CN 201010218545 CN201010218545 CN 201010218545 CN 201010218545 A CN201010218545 A CN 201010218545A CN 102312119 B CN102312119 B CN 102312119B
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Abstract
The invention discloses a preparation method for a silver tin oxide electrical contact material, which comprises the following steps: by taking a silver ingot, a tin ingot, an indium ingot and an additive ingot as raw materials, atomizing the raw materials to prepare a silver tin alloy powder; ingoting, sintering, extruding and drawing/rolling the silver tin alloy powder to prepare a wire material or a sheet plate or a belt material; and finally, carrying out internal oxidation to prepare the silver tin oxide electrical contact material. The preparation method for the silver tin oxide electrical contact material has the characteristics of uniform and stable contact material components, no conventional internally oxidized central lean oxidation zone, high density, high hardness and the like. The preparation method for the silver tin oxide electrical contact material has a simple process and is suitable for mass production. A prepared silver tin oxide product can be widely used for relays and contactors.
Description
Technical field
The present invention relates to a kind of preparation method of tin-oxygen-silver electric contact material, be mainly used in the production that low-voltage apparatus is used contact material.
Background technology
AgSnO
2Contact material has more and more replaced the AgCdO contact application in electrical equipment, and has tentatively finished AgSnO at west european developed country owing to its good resistance fusion welding energy and high electric life performance and environmental-protecting performance
2Replace AgCdO work.Domestic and international AgSnO
2The contact main production is divided into three kinds of technologies: powder mixing method, internal oxidation, chemical method.Wherein powder mixing method is Ag powder, SnO
2And additive powder powder fully mixes, and material extruding then, mold pressing are prepared into AgSnO
2Contact material; Internal oxidation is by being divided into preoxidation and product internal oxidation, and wherein preoxidation mainly refers to prepare the AgSn alloy powder, is prepared into AgSnO by the powder oxidation then
2Material is prepared into highdensity AgSnO by extruding or press moulding mode at last
2Contact material, this method, for example Chinese disclosure of the Invention number is a kind of preparation of silver-tin oxide material of CN1425790A; Internal oxidation refers to be prepared into alloy wire or sheet material after the AgSn fusing, is prepared into AgSnO by internal oxidation process then
2Contact material; Chemical method mainly refers to prepare AgSnO by hydrometallurgical processes
2Contact material, the most representative is exactly that silver nitrate solution adds the stannic oxide powder, and reduction silver realizes that chemistry coats AgSnO in the solution then
2Contact method, this method are called chemical coating method again;
By contrasting general AgSnO now
2Contact preparation method can be summed up as two kinds, and a kind of is preparation AgSnO
2Powder then by the whole bag of tricks, improves AgSnO
2Density, thereby preparation AgSnO
2Contact material, the AgSnO of this method preparation
2There are two problems in material, and the one, the materials processing poor-performing, the 2nd, contact material density is on the low side than the alloy inner oxidation method; Another method is prepared AgSn alloy wire or sheet material by alloy melting exactly, prepares AgSnO by internal oxidation then
2Also there are two problems in contact material, these class methods, and the one, material internalization process product center can occur and organize poor Sn phenomenon, and the 2nd, oxidising process is comparatively very long in the material, and especially in the thick product specification of strip-form contacts, interior oxidization time is veryer long.
Along with AgSnO
2Contact material increases at the consumption of low-voltage apparatus, just must seek a kind of materials processing better performances, composition homogeneous microstructure, the obvious production technique that shortens of interior oxidization time.
Summary of the invention
The present invention is directed to all drawbacks that existing technology exists, and combine the advantage of powder preparing-raising density and alloy melting-Nei oxidation two class technologies, the preparation method of the tin-oxygen-silver electric contact material of proposed a kind of density of material height, composition is uniform and stable, metallographic structure is even, the center does not have poor Sn layer, good, the interior oxidation rate of processing characteristics is fast.
For achieving the above object, technical scheme of the present invention is may further comprise the steps
(1) alloy melting, with silver-colored tin in proportion proportioning form alloy melt by intermediate frequency (IF) smelting;
(2) powder by atomization is made silver-colored stannum alloy powder with alloy melt through the atomizing of high-pressure atomization equipment;
(3) isostatic pressing ingot is processed into the embryo ingot with silver-colored stannum alloy powder by the isostatic pressing ingot;
(4) sintering carries out sintering with the embryo ingot in non-oxidative medium, sintering temperature is 300 ℃-900 ℃ and obtains silver-colored stannum alloy powder sintered ingot;
(5) through extruding, silver-colored stannum alloy powder sintered ingot is crushed to extruding silk material or extrusion plate, to push the silk material then and make the silver-colored stannum alloy powder silk material of specification by cold drawing, or with extrusion plate by the rolling silver-colored stannum alloy powder sheet material of making specification; The dimensions of silver stannum alloy powder silk material and silver-colored stannum alloy powder sheet material can be set according to user's actual needs.
(6) interior oxidation makes tin-oxygen-silver electric contact material with silver-colored stannum alloy powder silk material or silver-colored stannum alloy powder sheet material internal oxidation.
Further arranging is also can include other metallic additionses in the described step (1), and each component is by massfraction, wherein
Sn 6％-20％ In 0％-4％，
Cu 0.2％-1％ Ni 0.2％-1％
A1 0.2％-1％B i 0.2％-1％
All the other are Ag.
Further arrange is that smelting temperature is 900 ℃-1300 ℃ in the described step (1).
Further arranging is that described step (2) powder by atomization is water atomization powder process or aerosolization powder process, and wherein aerosolization pressure is at 5MPa-20MPa, and water atomization pressure is at 20MPa-100MPa.
Further arrange is that the control of described step (3) hydrostatic pressure is at 50MPa-250MPa.Non-oxidative medium is vacuum or hydrogen, argon gas or nitrogen atmosphere in the described step (4).
The processing condition control that further setting is extrusion operation in the described step (5) exists: 400 ℃-900 ℃ of extrusion temperatures, extrusion ratio 〉=80.
Further arrange is that the control of internal oxidation process condition exists in the described step (6): pure oxygen pressure 0.1-1.5MPa, temperature 400-750 ℃.
AgSn silk material or sheet material that it is the alloy powder preparation that the present invention prepares its interior fast principle of the more conventional AgSnIn alloy inner oxidation of oxidation rate of tin-oxygen-silver electric contact material can't be realized 100% relative density, silk material or the sheet material organization internal gap of the preparation of AgSn alloy powder have fully guaranteed the oxygen concn of material internal, thereby have improved interior oxidation rate; The present invention prepares AgSnO
2The uniform principle of contact material composition is to adopt the powder by atomization mode to prepare the AgSn alloy powder, the component segregation phenomenon of having avoided alloy melt to occur at melting, process of setting fully, thus guaranteed that whole contact composition is uniform and stable; The present invention prepares AgSnO
2The principle that the contact material center does not have poor Sn layer is because adopt AgSn silk material or the sheet material of the preparation of AgSn alloy powder, obstruction between powder and the powder and gap effect have stoped interior oxidising process Sn element owing to the AgSn alloy concentrations changes the segregation that produces, thereby have guaranteed center and outside consistence of composition; The present invention prepares AgSnO
2Contact material is because employing at first prepares AgSn alloy powder silk material or sheet material, so processing characteristics is than the AgSnO of preoxidation and mixed powder preparation
2Be significantly improved.
Referring to accompanying drawing 2, wherein 2a is the AgSnO of prepared of the present invention
2Metallograph, 2b are the AgSnO of conventional alloy inner oxidation method preparation
2Metallograph, 2c is the AgSnO of conventional mechanical powder mixing method preparation
2Metallograph;
Referring to the polytechnic physicals contrast table of table 1,
From metallographic structure, and the density of material, hardness, resistivity processing characteristics comprehensively contrasts, and technology of the present invention is AgSnO
2Best a kind of of over-all properties among the electric contact material preparation technology.
The AgSnO of table 1 prepared of the present invention
2(12) AgSnO of material and existing prepared
2(12) performance comparison
With the AgSnO of preparing product thickness at 4mm
2In
2O
3The strip-form contacts material is example, and oxidization time only needs 70 hours in the technology of the present invention, and the interior oxidization time of conventional alloy inner oxidation method minimum be 120 hours.
Below in conjunction with specification drawings and specific embodiments the present invention is done further introduction.
Description of drawings
Fig. 1 process flow sheet of the present invention;
The AgSnO of Fig. 2 the present invention preparation
2AgSnO with existing comparatively maturation process preparation
2The metallographic comparison diagram;
Embodiment
Below in conjunction with accompanying drawing 1; and carry out concrete description by the present invention of embodiment; only be used for the present invention is further specified; can not be interpreted as the restriction to protection domain of the present invention, the technician in this field can make some nonessential improvement and adjustment to the present invention according to the content of foregoing invention.
Embodiment 1
With AgSnO
2(8) In2O3 (4) material preparation is example
1, the 17.6kg silver ingot is placed in the heating in medium frequency stove, be heated to 1100 ℃-1200 ℃, melt fully to Ag, be cooled to 1000 ℃ then, add the tin slab of 1.26kg and the indium ingot of 0.662kg, after the fusing, refining 10 minutes;
2, under 8 ± 1MPa air pressure, aerosolization powder process;
3, AgSnIn alloy powder ingot processed under the 150MPa hydrostatic pressure;
4, AgSnIn alloy powder ingot sintering 4 hours in hydrogen furnace, 680 ℃ of temperature;
5, AgSnIn alloy powder ingot pushes at the 1100t extrusion machine, is prepared into the AgSnIn alloy powder sheet material of 40X4mm cross section specification;
6, AgSnIn alloy powder sheet material adopts the multiple silver process of hot rolling to be prepared into the AgSnIn/Ag sheet material that has silver layer;
7, AgSnIn/Ag sheet material is through cold rolling, punching out, the side's of preparation sheet type product;
8, the AgSnIn/Ag strip-form contacts is oxidized to AgSnO at 700 ℃, 0.6MPa oxygen in depressing
2In
2O
3The contact; This step is carried out in interior oxidized still.
The AgSnO of this examples preparation
2(8) In
2O
3(4) the strip-form contacts physicals is as follows: density 9.78g/cm
3(relative density 99.5%), resistivity 2.45 μ Ω .cm, hardness (HV0.3) 105 (annealed state), oxide particle evenly tiny, do not have thick crystal boundary, a poor Sn layer in no center;
Embodiment 2
With AgSnO
2(14) In
2O
3(1) material preparation is example
1, the 17kg silver ingot is placed in the heating in medium frequency stove, be heated to 1100 ℃-1200 ℃, melt fully to Ag, be cooled to 1000 ℃ then, add the tin slab of 2.207kg and the indium ingot of 0.0.179kg, after the fusing, refining 10 minutes;
2, under 40 ± 2MPa atomized water pressure, powder by atomization;
3, AgSnIn alloy powder ingot processed under the 150MPa hydrostatic pressure;
4, AgSnIn alloy powder ingot sintering 4 hours in hydrogen furnace, 680 ℃ of temperature;
5, AgSnIn alloy powder ingot pushes at the 1100t extrusion machine, is prepared into the AgSnIn alloy powder sheet material of 30X5mm cross section specification;
6, AgSnIn alloy powder sheet material adopts the multiple silver process of hot rolling to be prepared into the AgSnIn/Ag sheet material that has silver layer;
7, AgSnIn/Ag sheet material is through cold rolling, punching out, the side's of preparation sheet type product;
8, the AgSnIn/Ag strip-form contacts is oxidized to AgSnO at 700 ℃, 0.6MPa oxygen in depressing
2(14) In
2O
3(1) contact;
The AgSnO of this examples preparation
2(14) In
2O
3(1) the strip-form contacts physicals is as follows: density 9.65g/cm
3(relative density 99.4%), resistivity 2.74 μ Ω .cm, hardness (HV0.3) 124 (annealed state), oxide particle evenly tiny, do not have thick crystal boundary, a poor Sn layer in no center; And have only at Indium sesquioxide content under 1% the condition, this material can be fully by interior oxidation.
Embodiment 3
With AgSnO
2(12) Bi
2O
3(0.5) material preparation is example
1, the 17.5kg silver ingot is placed in the heating in medium frequency stove, be heated to 1100 ℃-1200 ℃, melt fully to Ag, be cooled to 1000 ℃ then, add the tin slab of 1.89kg and the bismuth ingot of 0.090kg, after the fusing, refining 10 minutes;
2, under 40 ± 2MPa atomized water pressure, powder by atomization;
3, AgSn alloy powder ingot processed under the 150MPa hydrostatic pressure;
4, AgSn alloy powder ingot sintering 4 hours in hydrogen furnace, 680 ℃ of temperature;
5, AgSn alloy powder ingot pushes at the 1100t extrusion machine, is prepared into the AgSn alloy bean vermicelli material of Φ 6.0 cross section specifications;
6, after AgSn alloy bean vermicelli material material is drawn to Φ 2.0, carry out interior oxidation in the oxidized still in inserting, internal oxidation process is: 750 ℃ of temperature, 0.6MPa oxygen are oxidized to AgSnO in depressing
2+ T contact;
The AgSnO of this examples preparation
2(12) Bi
2O
3Contact silk material physicals is as follows: density 9.91g/cm
3(relative density 99.5%), resistivity 2.23 μ Ω .cm, hardness (HV0.3) 93 (annealed state), oxide particle be tiny, tensile strength 310MPa (annealed state), unit elongation 19% (annealed state) evenly;
Claims (5)
1. the preparation method of a tin-oxygen-silver electric contact material is characterized in that may further comprise the steps successively:
(1) alloy melting, with silver-colored tin in proportion proportioning form alloy melt by intermediate frequency (IF) smelting; Also include other metallic additionses, each component is by massfraction, wherein
Sn 6％-20％ In 0％-4％，
Cu 0.2％-1％ Ni 0.2％-1％
Al 0.2％-1％ Bi 0.2％-1％
All the other are Ag;
(2) powder by atomization is made silver-colored stannum alloy powder with alloy melt through the atomizing of high-pressure atomization equipment;
(3) isostatic pressing ingot is processed into the embryo ingot with silver-colored stannum alloy powder by the isostatic pressing ingot; Hydrostatic pressure control is at 50MPa-250MPa;
(4) sintering carries out sintering with the embryo ingot in non-oxidative medium, sintering temperature is 300 ℃-900 ℃ and obtains silver-colored stannum alloy powder sintered ingot;
(5) extruding, rolling, silver-colored stannum alloy powder sintered ingot is crushed to extruding silk material or extrusion plate, to push the silk material then and make the silver-colored stannum alloy powder silk material of specification by cold drawing, or with extrusion plate by the rolling silver-colored stannum alloy powder sheet material of making specification, the processing condition control of extrusion operation exists: 400 ℃-900 ℃ of extrusion temperatures, extrusion ratio 〉=80;
(6) interior oxidation makes tin-oxygen-silver electric contact material with silver-colored stannum alloy powder silk material or silver-colored stannum alloy powder sheet material internal oxidation.
2. the preparation method of a kind of tin-oxygen-silver electric contact material according to claim 1 is characterized in that: smelting temperature is 900 ℃-1300 ℃ in the described step (1).
3. the preparation method of a kind of tin-oxygen-silver electric contact material according to claim 2, it is characterized in that: described step (2) powder by atomization is water atomization powder process or aerosolization powder process, wherein aerosolization pressure is at 5MPa-20MPa, and water atomization pressure is at 20MPa-100MPa.
4. the preparation method of a kind of tin-oxygen-silver electric contact material according to claim 3 is characterized in that: non-oxidative medium is vacuum or hydrogen, argon gas or nitrogen atmosphere in the described step (4).
5. the preparation method of a kind of tin-oxygen-silver electric contact material according to claim 4 is characterized in that: the control of internal oxidation process condition exists in the described step (6): pure oxygen pressure 0.1-1.5MPa, temperature 400-750 ℃.
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| CN 201010218545 CN102312119B (en) | 2010-06-29 | 2010-06-29 | Preparation method for silver tin oxide electrical contact material |
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|---|---|---|---|
| CN 201010218545 CN102312119B (en) | 2010-06-29 | 2010-06-29 | Preparation method for silver tin oxide electrical contact material |
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| CN102312119B true CN102312119B (en) | 2013-07-10 |
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| CN102820153A (en) * | 2012-08-21 | 2012-12-12 | 福达合金材料股份有限公司 | Preparation method of refined AgSnO2In2O3 (silver tin oxide - indium oxide) crystal grain |
| CN102925738B (en) * | 2012-11-07 | 2015-01-07 | 福达合金材料股份有限公司 | Method for preparing silver tin oxide material |
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| CN111321315B (en) * | 2020-03-07 | 2021-05-04 | 福达合金材料股份有限公司 | Isolating material for internal oxidation of electric contact material and preparation method thereof |
| CN112475295B (en) * | 2020-09-30 | 2022-11-15 | 浙江福达合金材料科技有限公司 | Silver ferric oxide electric contact material with oxide particles dispersed and distributed and preparation method thereof |
| CN114360948B (en) * | 2022-01-10 | 2024-08-02 | 温州宏丰特种材料有限公司 | Silver tin oxide indium oxide electric contact composite material and preparation method thereof |
| CN115637349A (en) * | 2022-09-17 | 2023-01-24 | 浙江福达合金材料科技有限公司 | Silver tin oxide electric contact material and preparation method thereof |
| 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 |
| CN115725871A (en) * | 2022-11-08 | 2023-03-03 | 浙江福达合金材料科技有限公司 | Preparation method of silver tin oxide electrical contact material |
| CN115870498B (en) * | 2022-12-06 | 2024-08-06 | 浙江福达合金材料科技有限公司 | Preparation method for improving bonding strength of flaky silver tin oxide electrical contact material |
| CN115740465B (en) * | 2022-12-13 | 2023-08-18 | 温州中希电工合金有限公司 | Silver tin oxide contact material and preparation method thereof |
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| JPH07166267A (en) * | 1993-12-15 | 1995-06-27 | Mitsubishi Materials Corp | Ag-oxide electrical contact material excellent in arc resistance |
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| CN1477219A (en) * | 2002-08-21 | 2004-02-25 | 中国科学院金属研究所 | Preparation method of siluer metal oxide electric contact material |
| CN101202169A (en) * | 2007-10-23 | 2008-06-18 | 福达合金材料股份有限公司 | Method of preparing novel silver tin oxide silk electrical contact material |
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