CN108010772B - A kind of method that microwave heating prepares tin-oxygen-silver electric contact material - Google Patents

A kind of method that microwave heating prepares tin-oxygen-silver electric contact material Download PDF

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Publication number
CN108010772B
CN108010772B CN201711289931.8A CN201711289931A CN108010772B CN 108010772 B CN108010772 B CN 108010772B CN 201711289931 A CN201711289931 A CN 201711289931A CN 108010772 B CN108010772 B CN 108010772B
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microwave heating
oxygen
silver
electric contact
contact material
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CN108010772A (en
Inventor
李�杰
颜小芳
张秀芳
杨昌麟
王珩
柏小平
翁桅
林万焕
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Zhejiang Fuda Alloy Materials Technology Co Ltd
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Fuda Alloy Materials Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/048Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes

Abstract

The present invention discloses a kind of method that microwave heating prepares tin-oxygen-silver electric contact material.Step includes water atomization, microwave heating drying and oxidation, hot isostatic pressing, sintering, hot-working, the additive is In, Cu, Zr, Co, Bi, Ni, two or more in rare earth, by weight percentage, Ag 80-94%, Sn5-19%, In 0-6%, Cu0-3%, Zr 0-2%, Co 0-2%, Bi 0-3%, Ni 0-2%, rare earth 0-3%.The preparation method is using microwave heating drying, oxidation AgSn powder, the resistance heating drying, the resistance heating oxidation that are different from conventional technique.Silver is prepared by microwave heating and aoxidizes silk material, and the problems such as solving drying and uneven in oxidation process, oxide particle size fluctuation is big, heating time length, low efficiency, big power consumption, there is remarkable effect to raising production efficiency, shortening production friendship phase.

Description

A kind of method that microwave heating prepares tin-oxygen-silver electric contact material
Technical field
The present invention relates to a kind of methods that electrical material, in particular to microwave heating prepare tin-oxygen-silver electric contact material.
Background technique
Microwave heating is exactly to utilize the features such as the wavelength of microwave is short, frequency is high, Quantum Properties are obvious, realizes and carries out to object Heating.Microwave technology can not only effectively improve reaction conversion ratio, selectivity, but also many advantages, such as embody energy conservation and environmental protection, extensively It is general to be applied to the fields such as radar, navigation, multiplex communication, remote sensing and TV, food.
Currently, the method for preparing tin-oxygen-silver electric contact material has powder mixing method, chemical method, preoxidation, internal oxidation, Middle preoxidation has the characteristics that oxide particle is evenly distributed, process is short, processing technology is simple and is widely used.
Preparing the general heating means of tin-oxygen-silver electric contact material is the environment by circumference, with the radiation of heat Or heat the surface of object first, then pass through the inside of heat transfer conductive object.This Kind method heating time length, low efficiency.
It is retrieved by pertinent literature, the pre-oxidation process retrieved prepares the following institute of patent document of silver tin oxide material Show:
(1) patent CN1425790, a kind of preparation method of silver tin oxide material;
(2) patent CN102925738A, a kind of preparation method of silver tin oxide material;
(3) patent CN102312119A, a kind of preparation method of tin-oxygen-silver electric contact material.
AgSn powder in patent (1) uses oxidation furnace to aoxidize (oxidation furnace is resistance-heated furnace);Water atomization in patent (2) It is passed through oxygen simultaneously in the process to be aoxidized, then be dried using resistance furnace;Internal oxidition is in interior oxidation furnace in patent (3) Carry out (internal oxidition furnace is resistance-heated furnace).Above-mentioned patent is using conventional electric resistance mode or using logical during water atomization Enter dioxygen oxidation and prepare tin-oxygen-silver electric contact material, there are heating time is long, energy consumption is high, powder oxidation is uneven in oxidation process It is even, cause oxide particle size to there are problems that notable difference.
Summary of the invention
The purpose of the present invention is for the water atomization powder in the presence of existing tin-oxygen-silver electric contact material preparation process Drying, the problems such as oxidation is uneven in oxidation process, heating time length, low efficiency, big power consumption, and a kind of microwave heating is provided The method for preparing tin-oxygen-silver electric contact material makes powder drying, oxidation uniformity are good, improve production to imitate by this method Rate, the consistency for shortening the production friendship phase, improving oxide particle size.
To achieve the above object, the technical scheme is that the following steps are included:
(1) silver ingot, tin slab, additive are put into mid-frequency melting furnace melting, water mist is melted into AgSn alloy powder;
(2) AgSn alloy powder obtained by step (1) dried by microwave heating equipment, aoxidized;
(3) ingot blank is made in the powder hot isostatic pressing after step (2) oxidation;
(4) spindle of step (3) is sintered in having oxygen atmosphere;
(5) step (4) sintered spindle is thermally processed into silk material.
Further setting be the step (1) additive be In, Cu, Zr, Co, Bi, Ni, any three kinds in rare earth Or three kinds of combination of the above.
Further setting is the component of silver ingot, tin slab, additive, by weight percentage, Ag 80-94%, Sn 5-19%, In 0-6%, Cu 0-3%, Zr 0-2%, Co 0-2%, Bi 0-3%, Ni 0-2%, rare earth 0-3%.
Further setting is that the drying in the step (2) is carried out in microwave heating equipment, with 5 DEG C~40 DEG C/min Heating rate reaches 200-350 DEG C of drying AgSn alloy powder, and powder tiles thickness in 1-5mm;Then in microwave heating equipment Upper progress powder oxidation exists, and reaches 400-800 DEG C with 10 DEG C~50 DEG C/min of heating rate and is aoxidized, when amounting to heat preservation Between 5-60min.
It is 400-800 DEG C, pressure 100-200MPa that further setting, which is the temperature of hot isostatic pressing in the step (3), ingot The diameter of base is 50-110mm.
Further setting is that the sintering of the step (4) uses resistance stove heating, 750-900 DEG C of temperature, keeps the temperature 5- 60min, oxygen press 0.1-1MPa.
It is resistance heating or mid-frequency induction heating, temperature 750- that further setting, which is the thermal processing method of the step (5), 900 DEG C, 1-5h is kept the temperature, extruding silk material specification is Ф 3mm- Ф 8mm.
It is an advantage of the invention that in preparing siller tin oxide electric contact material, using microwave heating drying, oxidation powder, oxygen Temperature uniformity is good during change, it is more uniform to aoxidize.The process flow is simple, is readily produced.
Meanwhile the present invention by heated object internal dipole molecule high-frequency reciprocating move, generate " interior frictional heat " and make by Heated material temperature increases, and is not necessary to any heat transfer process, has reached elimination Ag and SnO2Deng internal stress, optimization oxide The wetability for being arranged of preferred orient, improving tin oxide and silver matrix and interface binding power of grain reduce relay electrical performance test Oxide particle in the process splash, greatly promote slider material resistance to scaling loss performance purpose.
The silk material metallographic structure of this method preparation is uniform, and the discreteness of mechanical and physical performance is small, adds to improve rivet The stability of stability and relay electric life during work.
The present invention is described further with specific embodiment with reference to the accompanying drawings of the specification.
Detailed description of the invention
Process flow chart Fig. 1 of the invention.
Specific embodiment
The present invention is specifically described below by embodiment, is served only for that invention is further explained, no It can be interpreted as limiting the scope of the present invention, the technician in the field can be according to the content of foregoing invention to the present invention Make some nonessential modifications and adaptations.
(1) silver ingot, tin slab, additive are put into mid-frequency melting furnace melting, water mist is melted into AgSn powder, with weight percent Meter, Ag 80%, Sn19%, In 0%, Cu0.2%, Zr 0.2%, Co 0.1%, Bi 0.2%, Ni 0.1%, rare earth 0.2%;
(2) 200 DEG C of drying AgSn powders are reached with 5 DEG C/min of heating rate, powder tiles with a thickness of 5mm, then with 10 DEG C/min of heating rate reaches 400 DEG C, soaking time 60min;
(3) ingot blank is made in the powder hot isostatic pressing after aoxidizing, and the temperature of hot isostatic pressing is 400 DEG C, pressure 200MPa, ingot The diameter of base is 110mm;
(4) spindle after equal static pressure is sintered, 750 DEG C of temperature in oxygen atmosphere, keeps the temperature 60min, oxygen presses 1MPa.
(5) sintered spindle 900 DEG C of temperature, is kept the temperature into 1h in resistance heating or mid-frequency induction heating, squeezes silk material rule Lattice are Ф 8mm.
(6) the silk material performance that the performance of silk material in embodiment one is prepared with common process is compared, specific data As shown in the table.As can be seen from the data in the table, the performance discreteness of the present embodiment is substantially better than the silver-colored oxygen of common process production Change tin silk material.
Silk material performance compares
(7) silk material system in embodiment one is broken into rivet, is assembled into relay and carries out electrical endurance test, and and common process The electrical property of the silk material of preparation compares, and specific data are as shown in the table.
Relay test condition
Relay test result
Embodiment two:
(1) silver ingot, tin slab, additive are put into mid-frequency melting furnace melting, water mist is melted into AgSn powder, with weight percent Meter, Ag 94%, 3Sn5%, In 0.8%, Cu0.2%;
(2) 350 DEG C of drying AgSn powders are reached with 40 DEG C/min of heating rate, powder tiles thickness 0.5mm, then Reach 800 DEG C with 50 DEG C/min of heating rate, soaking time 5min;
(3) the powder isostatic pressing after aoxidizing obtains ingot blank, waits static pressure at ingot blank, and the temperature of hot isostatic pressing is 800 DEG C, pressure 100MPa, the diameter of ingot blank are 50mm.
(4) spindle after equal static pressure is sintered, 900 DEG C of temperature in oxygen atmosphere, keeps the temperature 5min, oxygen pressure 0.1MPa。
(5) sintered spindle is heated, 750 DEG C of temperature in resistance furnace, keeps the temperature 5h, extruding silk material specification is Ф 3mm.
(6) the silk material performance that the performance of silk material in embodiment two is prepared with common process is compared, specific data As shown in the table.As can be seen from the data in the table, the performance discreteness of the present embodiment is substantially better than the silver-colored oxygen of common process production Change tin silk material.
(7) silk material system in embodiment one is broken into rivet, is assembled into relay and carries out electrical endurance test, and and common process The electrical property of the silk material of preparation compares, and specific data are as shown in the table.
Relay test condition
Relay test result

Claims (6)

1. a kind of method that microwave heating prepares tin-oxygen-silver electric contact material, it is characterised in that the following steps are included:
(1) silver ingot, tin slab, additive are put into mid-frequency melting furnace melting, water mist is melted into AgSn alloy powder;
(2) AgSn alloy powder obtained by step (1) is dried and is aoxidized by microwave heating equipment;The step (2) In drying carried out in microwave heating equipment, 200-350 DEG C of drying AgSn conjunction is reached with 5 DEG C~40 DEG C/min of heating rate Bronze body, AgSn alloy powder tile thickness in 1-5mm;Then the oxidation of AgSn alloy powder is carried out on microwave heating equipment, Reach 400-800 DEG C with 10 DEG C~50 DEG C/min of heating rate to be aoxidized, amounts to soaking time 5-60min;
(3) ingot blank is made in the AgSn alloy powder hot isostatic pressing after step (2) oxidation;
(4) ingot blank of step (3) is sintered in having oxygen atmosphere;
(5) step (4) sintered ingot blank is thermally processed into silk material.
2. the method that microwave heating according to claim 1 prepares tin-oxygen-silver electric contact material, it is characterised in that: described The additive of step (1) is In, Cu, Zr, Co, Bi, Ni, any three kinds of combination of the above in rare earth.
3. the method that microwave heating according to claim 1 prepares tin-oxygen-silver electric contact material, it is characterised in that: silver The component of ingot, tin slab, additive, by weight percentage, Ag 80-94%, Sn 5-19%, In 0-6%, Cu 0-3%, Zr 0-2%, Co 0-2%, Bi 0-3%, Ni 0-2%, rare earth 0-3%.
4. the method that microwave heating according to claim 1 or 2 or 3 prepares tin-oxygen-silver electric contact material, feature exist In: the temperature of hot isostatic pressing is 400-800 DEG C, pressure 100-200MPa in the step (3), and the diameter of ingot blank is 50- 110mm。
5. the method that microwave heating according to claim 1 prepares tin-oxygen-silver electric contact material, it is characterised in that: described The sintering of step (4) uses resistance stove heating, 750-900 DEG C of temperature, keeps the temperature 5-60min, oxygen presses 0.1-1MPa.
6. the method that microwave heating according to claim 1 prepares tin-oxygen-silver electric contact material, it is characterised in that: described The thermal processing method of step (5) is resistance heating or mid-frequency induction heating, 750-900 DEG C of temperature, keeps the temperature 1-5h, squeezes silk material rule Lattice are Ф 3mm- Ф 8mm.
CN201711289931.8A 2017-12-08 2017-12-08 A kind of method that microwave heating prepares tin-oxygen-silver electric contact material Active CN108010772B (en)

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CN109500392B (en) * 2019-01-05 2021-03-16 桂林电器科学研究院有限公司 Preparation method of silver zinc oxide contact material for improving sintering property of ingot blank
CN109500391A (en) * 2019-01-05 2019-03-22 桂林电器科学研究院有限公司 A kind of preparation method of high ductility silver zinc oxide contact material
CN111197925B (en) * 2020-01-13 2021-04-30 郑州机械研究所有限公司 Brazing flux drying method and system
CN114457249B (en) * 2021-12-30 2022-12-09 无锡日月合金材料有限公司 Silver-indium tin oxide based sintered material for electric contact and preparation method thereof
CN115386757A (en) * 2022-07-07 2022-11-25 靖江市海源有色金属材料有限公司 Method for manufacturing silver tin oxide contact material
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

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US4904317A (en) * 1988-05-16 1990-02-27 Technitrol, Inc. Erosion resistant Ag-SnO2 electrical contact material
JPH10287938A (en) * 1997-04-15 1998-10-27 Mitsubishi Materials Corp Electrical contact material made of heat treated silver alloy having excellent deposition resistance and consumption resistance
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
CN101510479B (en) * 2009-03-18 2010-08-25 中国船舶重工集团公司第七二五研究所 Method for preparing siller tin oxide electric contact material
CN102382997B (en) * 2011-10-24 2013-02-27 中南大学 Method for preparing WC-Co cemented carbide through microwave sintering

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