CN108010772A - 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
CN108010772A
CN108010772A CN201711289931.8A CN201711289931A CN108010772A CN 108010772 A CN108010772 A CN 108010772A CN 201711289931 A CN201711289931 A CN 201711289931A CN 108010772 A CN108010772 A CN 108010772A
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China
Prior art keywords
oxygen
microwave heating
electric contact
silver
contact material
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CN201711289931.8A
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CN108010772B (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, high temperature insostatic pressing (HIP), sintering, hot-working, the additive is two or more in In, Cu, Zr, Co, Bi, Ni, 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 powders, resistance heating drying, the resistance heating oxidation being different from conventional technique.Heated by microwave and prepare silver-colored oxidation silk material, solve the problems such as drying is uneven with oxidizing process, oxide particle size fluctuation is big, heating time is long, efficiency is low, power consumption is big, to improving production efficiency, the shortening production friendship phase has remarkable effect.

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 method that electrical material, in particular to microwave heating prepare tin-oxygen-silver electric contact material.
Background technology
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 object is carried out 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.
At present, preparing the method for tin-oxygen-silver electric contact material has powder mixing method, chemical method, preoxidation, internal oxidation, its Middle preoxidation has the characteristics that oxide particle is evenly distributed, flow is short, processing technology is simple and widely uses.
It is the environment by circumference to prepare the general heating means of tin-oxygen-silver electric contact material, with the radiation of heat Or the surface of object is first heated by way of hot-air convection, then pass through the inside of heat transfer conductive object.This Kind method heating time is long, efficiency is low.
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 powders in patent (1) use oxidation furnace to aoxidize (oxidation furnace is resistance-heated furnace);Water atomization in patent (2) During be passed through oxygen at the same time and aoxidized, then dried using resistance furnace;Internal oxidition is in interior oxidation furnace in patent (3) Carry out (internal oxidition stove is resistance-heated furnace).Above-mentioned patent is led to using conventional electric resistance mode or using during water atomization Enter dioxygen oxidation and prepare tin-oxygen-silver electric contact material, there are heating time is long, energy consumption is big, powder oxidation is uneven in oxidizing process Even, causing oxide particle size, there are the problem of notable difference.
The content 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 The problems such as uneven, heating time is long, efficiency is low, power consumption is big is aoxidized in drying, oxidizing process, and a kind of microwave heating is provided The method for preparing tin-oxygen-silver electric contact material, is dried, oxidation uniformity is good, improves production effect by this method powder Rate, the uniformity for shortening the production friendship phase, improving oxide particle size.
To achieve the above object, the technical scheme is that comprising the following steps:
(1) silver ingot, tin slab, additive are put into mid-frequency melting furnace melting, water mist chemical conversion AgSn alloy powders;
(2) AgSn alloy powders obtained by step (1) dried by microwave heating equipment, aoxidized;
(3) ingot blank is made in the powder high temperature insostatic pressing (HIP) after step (2) is aoxidized;
(4) spindle of step (3) is sintered in having oxygen atmosphere;
(5) spindle after step (4) is sintered is thermally processed into silk material.
Further set is the step (1) described additive for any three kinds in In, Cu, Zr, Co, Bi, Ni, 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 Programming 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 programming rate and is aoxidized, when amounting to insulation Between 5-60min.
Further setting is that the temperature of high temperature insostatic pressing (HIP) in the step (3) is 400-800 DEG C, pressure 100-200MPa, ingot A diameter of 50-110mm of base.
Further setting is that the sintering of the step (4) uses resistance stove heat, and 750-900 DEG C of temperature, keeps the temperature 5- 60min, oxygen pressure 0.1-1MPa.
It is that the thermal processing method of the step (5) is resistance heating or Frequency Induction Heating further to set, temperature 750- 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 siller tin oxide electric contact material is prepared, using microwave heating, drying, oxidation powder, oxygen During change temperature uniformity it is good, oxidation be more uniformly distributed.The technological process is simple, is readily produced.
Meanwhile the present invention by heated object internal dipole molecule high-frequency reciprocating move, produce " interior frictional heat " and make by Heated material temperature raises, 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 During oxide particle splash, greatly promote slider material resistance to scaling loss performance purpose.
Silk material metallographic structure prepared by this method is uniform, and the discreteness of mechanical and physical performance is small, adds so as to improve rivet The stability of stability and relay electric life during work.
The present invention is described further with reference to specification drawings and specific embodiments.
Brief description of the drawings
The process flow chart of Fig. 1 present invention.
Embodiment
The present invention is specifically described below by embodiment, is served only for that the present invention is further described, no It is understood that for 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 chemical conversion AgSn powders, with percentage by weight 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 programming rate, powder tiling thickness is 5mm, then with 10 DEG C/min programming rate reach 400 DEG C, soaking time 60min;
(3) ingot blank is made in the powder high temperature insostatic pressing (HIP) after aoxidizing, and the temperature of high temperature insostatic pressing (HIP) is 400 DEG C, pressure 200MPa, ingot blank A diameter of 110mm;
(4) spindle after isostatic pressed is sintered in oxygen atmosphere, 750 DEG C of temperature, keeps the temperature 60min, oxygen pressure 1MPa.
(5) spindle after sintering is kept the temperature into 1h in resistance heating or Frequency Induction Heating, 900 DEG C of temperature, extruding silk material is advised 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 It is 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 prepared with common process The electrical property of silk material compare, specific data are as shown in the table.
Relay test condition
Relay test result
Embodiment two:
(1) silver ingot, tin slab, additive being put into mid-frequency melting furnace melting, water mist is melted into AgSn powders, by weight percentage, Ag 94%, 3Sn5%, In 0.8%, Cu0.2%;
(2) 350 DEG C of drying AgSn powders, powder tiling thickness 0.5mm, then with 50 are reached with 40 DEG C/min of programming rate DEG C/min programming rate reach 800 DEG C, soaking time 5min;
(3) the powder isostatic pressing after aoxidizing obtains ingot blank, and isostatic pressed is into ingot blank, and the temperature of high temperature insostatic pressing (HIP) is 800 DEG C, pressure 100MPa, a diameter of 50mm of ingot blank.
(4) spindle after isostatic pressed is sintered in oxygen atmosphere, 900 DEG C of temperature, keeps the temperature 5min, oxygen pressure 0.1MPa。
(5) spindle after sintering is heated in resistance furnace, 750 DEG C of temperature, 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 It is 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 prepared with common process The electrical property of silk material compare, specific data are as shown in the table.
Relay test condition
Relay test result

Claims (7)

1. a kind of method that microwave heating prepares tin-oxygen-silver electric contact material, it is characterised in that comprise the following steps:
(1) silver ingot, tin slab, additive are put into mid-frequency melting furnace melting, water mist chemical conversion AgSn alloy powders;
(2) AgSn alloy powders obtained by step (1) dried by microwave heating equipment, aoxidized;
(3) ingot blank is made in the powder high temperature insostatic pressing (HIP) after step (2) is aoxidized;
(4) spindle of step (3) is sintered in having oxygen atmosphere;
(5) spindle after step (4) is sintered 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:It is described Step (1) described additive is In, Cu, any three kinds or more combination in Zr, Co, Bi, Ni, 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 Ingot, tin slab, the component of additive, by weight percentage, Ag 80-94%, Sn 5-19%, In 0-6%, Cu 0-3%, Zr 0- 2%th, Co 0-2%, Bi 0-3%, Ni 0-2%, rare earth 0-3%.
4. the method that the microwave heating according to claim 1 or 2 or 3 prepares tin-oxygen-silver electric contact material, its feature exist In:Drying in the step (2) is carried out in microwave heating equipment, and the programming rate with 5 DEG C~40 DEG C/min reaches 200- 350 DEG C of drying AgSn alloy powders, powder tile thickness in 1-5mm;Then powder oxidation is carried out on microwave heating equipment, with 10 DEG C~50 DEG C/min of programming rate reaches 400-800 DEG C and is aoxidized, and amounts to soaking time 5-60min.
5. the method that the microwave heating according to claim 1 or 2 or 3 prepares tin-oxygen-silver electric contact material, its feature exist In:The temperature of high temperature insostatic pressing (HIP) is 400-800 DEG C, pressure 100-200MPa in the step (3), a diameter of 50- of ingot blank 110mm。
6. the method that microwave heating according to claim 1 prepares tin-oxygen-silver electric contact material, it is characterised in that:It is described The sintering of step (4) uses resistance stove heat, and 750-900 DEG C of temperature, keeps the temperature 5-60min, oxygen pressure 0.1-1MPa.
7. the method that microwave heating according to claim 1 prepares tin-oxygen-silver electric contact material, it is characterised in that:It is described The thermal processing method of step (5) is resistance heating or Frequency Induction Heating, and 750-900 DEG C of temperature, keeps the temperature 1-5h, extruding 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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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109500392A (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 for the silver zinc oxide contact material improving ingot blank agglutinating property
CN111197925A (en) * 2020-01-13 2020-05-26 郑州机械研究所有限公司 Brazing flux drying method and system
CN114457249A (en) * 2021-12-30 2022-05-10 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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101510479A (en) * 2009-03-18 2009-08-19 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
CN102382997A (en) * 2011-10-24 2012-03-21 中南大学 Method for preparing WC-Co cemented carbide through microwave sintering

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101510479A (en) * 2009-03-18 2009-08-19 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
CN102382997A (en) * 2011-10-24 2012-03-21 中南大学 Method for preparing WC-Co cemented carbide through microwave sintering

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109500392A (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 for the silver zinc oxide contact material improving ingot blank agglutinating property
CN111197925A (en) * 2020-01-13 2020-05-26 郑州机械研究所有限公司 Brazing flux drying method and system
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
CN114457249A (en) * 2021-12-30 2022-05-10 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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