CN103700544A - Preparing method of AgSnO electric contact materials with uniform tissues - Google Patents

Preparing method of AgSnO electric contact materials with uniform tissues Download PDF

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CN103700544A
CN103700544A CN201310698853.2A CN201310698853A CN103700544A CN 103700544 A CN103700544 A CN 103700544A CN 201310698853 A CN201310698853 A CN 201310698853A CN 103700544 A CN103700544 A CN 103700544A
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electric contact
oxygen
tin
preparation
percent
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CN103700544B (en
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李�杰
颜小芳
柏小平
翁桅
杨坤
刘立强
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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Abstract

The invention relates to a preparing method of AgSnO electric contact materials with uniform tissues. The method comprises the steps of smelting, surface treatment, extrusion, drawing, pushing and cutting, ingot pressing, inner oxidation, re-pressing, surface treatment, extrusion and drawing, wherein additives are any two kinds of materials or more than two kinds of materials from Cu, Ga, Ce, Zr and CO. The materials comprise the following ingredients in percentage by weight: 86 to 92 percent of Ag, 5 to 8 percent of Sn, 2 to 3 percent of In, 0 to 2 percent of Cu, 0 to 1 percent of Ga, 0 to 0.2 percent of Ce, 0 to 0.3 percent of Zr and 0 to 0.5 percent of Co. The key steps of the process include the ingot pressing after the wire material pushing and cutting,the inner oxidization, the re-pressing and the surface treatment. The wire materials prepared by the method have the advantages that the metallographic structure is uniform, and the oxide aggregation and silver aggregation phenomena do not occur. Meanwhile, the hardness of the wire materials is low, the elongation percentage is high, after the materials are made into rivets, electric performance tests are carried out, the material transfer resistance performance is good, and the AgSnO electric contact materials prepared by the method are suitable for being applied to various different vehicle-mounted relays.

Description

A kind of preparation method of tin-oxygen-silver electric contact material of even tissue
Technical field
The present invention relates to electrical material, specifically refer to a kind of preparation method of tin-oxygen-silver electric contact material of even tissue.
Background technology
AUTOMOTIVE RELAY is the important control element in automotive electrical system, is widely used in systems such as controlling automobile start, preheating, air-conditioning, light and electronic automobile meter and failure diagnosis.And electrical contact material is one of core component of relay, its quality is for guaranteeing that vehicle-mounted relay reliability of operation, stability have decisive meaning.
At present, the contact material that is applied to AUTOMOTIVE RELAY be take siller tin oxide as main, has the problems such as oxide buildup, silver gathering due to contact material, causes material to have the problems such as electrical endurance is short, material transfer phenomenon is serious.
By pertinent literature, retrieve, the method for preparing siller tin oxide electric contact material has powder mixing method, chemical method, preoxidation, internal oxidation, and most technology mainly concentrate on first three methods.The patent documentation of preparing silver tin oxide material retrieving is as follows:
(1) patent CN102509654A, a kind of preparation method for silver stannic oxide wire;
(2) patent CN1417817, Nano silver-tin oxide electric contact and preparation method thereof;
(3) patent CN1054505, silver-tin contact material and manufacture method thereof;
(4) patent CN102154572A, a kind of gradient internal oxidation is prepared process and the material thereof of silver-tin oxide or indium oxide contact material.
The combination that patent (1) adopts atomization process and blending processes of powders, mainly improves the problems such as in prior art, the intensity of material is low, compactness is poor, processing difficulties; Patent (2) is the combination of sol-gel process and powder mixing method, mainly solves the problems such as in powder metallurgical technique, in difficult drawing moulding, use, contact resistance is large, temperature rise is high; The processing step of patent (3) comprises melting, is squeezed into rectangular bar, covers silver, rolling, punching, interior oxidation, reprocessing, is mainly used in the preparation of sheet material stannic oxide materials; What patent (4) adopted is melting, extruding, drawing, then oxidation in silk material gradient, thrusts the method for briquetting, extruding, drawing, and the core of technique is oxidation in gradient, the separating out of material surface fine silver layer in oxidizing process in solving.
Above-mentioned these patent documentations all do not provide the oxide buildup solving in vehicle-mounted relay contact material, solution and the enlightenment of silver-colored rendezvous problem.
Summary of the invention
The object of the invention is in order to overcome the problems such as the oxide buildup existing in contact material in prior art, silver-colored gathering, and a kind of preparation method of tin-oxygen-silver electric contact material of even tissue is provided, thereby improve its anti-material transfer performance.
For achieving the above object, technical scheme of the present invention is to comprise the following steps:
(1) silver ingot, tin slab, indium ingot are put into mid-frequency melting furnace melting, add additive in process, then ingot casting is through surface treatment;
(2) ingot casting after step (1) processing is thermally processed into a material;
(3) the silk material after step (2) hot working is cold worked into small dimension silk material;
(4) the small dimension silk material of step (3) is cut off, briquetting becomes spindle;
(5) spindle after step (4) processing is inserted in aerobic environment, be oxidized, then pressure, surface treatment again;
(6) spindle after step (5) processing is thermally processed into a material.
Further arranging is that the described additive of described step (1) is at least two kinds in Cu, Ga, Ce, Zr, Co, by weight percentage, and Ag 86-92%, Sn 5-8%, In 2-3%, Cu0-2%, Ga 0-1%, Ce 0-0.2%, Zr 0-0.3%, Co 0-0.5%.
Further setting is that the extruding heating-up temperature of described step (2) is 660-770 ℃, temperature retention time 3-6h, silk material diameter 4-7mm.
Further setting is that the cold working of described step (3) is a silk material drawing mode.
Further setting is that the fracture of wire length of described step (4) is 20-30mm, spindle diameter 80-85mm, pressure 8-12MPa.
Further setting is that the oxidizing temperature of described step (5) is 750-850 ℃, oxidization time is 10-15h, and described aerobic environment oxygen is pressed in the oxygen atmosphere for 2MPa-5MPa, the multiple sub-diameter 80-85mm of briquetting, pressure 50-60MPa, then removes spindle surface layer thickness 2-4mm with lathe.
Further setting is that the extruding heating-up temperature of described step (6) is 800-900 ℃, temperature retention time 5-10h, silk material diameter 3-5mm.
Further setting is that the thermal processing method of described step (6) is the wantonly 2 kinds of combinations in high-frequency heating, heating in medium frequency, resistance heating.
The present invention in preparing siller tin oxide electric contact material, core procedure for a silk material thrusts, briquetting, interior oxidation, press again, surface treatment, be different from that conventional internal oxidation process step thrusts, interior oxidation, briquetting.After oxidation there is the phenomenons such as continuous oxidation film, silver gathering in spindle top layer, processed superficial layer is removed, and spindle interior tissue is even by turning.The method solved the difficult problems such as a large amount of silver gatherings that exist in silver tin oxide material, oxide buildup, improved the anti-material transfer performance of silver tin oxide material in vehicle-mounted relay is applied, electrical endurance etc.This technological process is simple, be easy to produce, and contact material prepared by this technique is more suitable for being applied on various vehicle-mounted relay.
Below in conjunction with specification drawings and specific embodiments, the present invention is described further.
Accompanying drawing explanation
Fig. 1 process chart of the present invention;
The horizontal metallographic structure figure of silk material prepared by the existing conventional internal oxidation process of Fig. 2;
The sample metallographic structure transverse view of Fig. 3 embodiment of the present invention one;
The sample metallographic structure transverse view of Fig. 4 embodiment of the present invention two;
Photo after silk material electrical performance test prepared by the existing conventional internal oxidation process of Fig. 5;
Photo after the material electrical performance test of Fig. 6 embodiment of the present invention one;
Photo after the material electrical performance test of Fig. 7 embodiment of the present invention two.
Embodiment
Below by embodiment, the present invention is specifically described; only be used to further illustrate the present invention; can not be interpreted as limiting the scope 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 mono-:
(1) Ag ingot, Sn ingot, additive (In, Ga, Ce) are carried out to melting, composition proportion be Ag86Sn8In3Cu2Ga1(by weight percentage) pour into billet, then with lathe, remove surface scale 4mm;
(2) extruding, 660 ℃ of heating-up temperatures, are incubated 6h, obtain the silk material of Φ 4mm;
(3) pull to Φ 2.5mm;
(4) thrust also briquetting, wherein fracture of wire length is 30mm, spindle diameter 80mm, pressure 8MPa;
(5) oxidizing temperature is 750 ℃, and oxygen is pressed 5MPa, and oxidization time is 5h, spindle diameter 85mm after multiple pressure, and multiple pressure pressure 50MPa, spindle surface car removes 4mm;
(6) extruding heating-up temperature is 900 ℃, and temperature retention time 5h, obtains Φ 7mm silk material, and then hot pull is to silk material finished product Φ 1.5mm;
(7) above-mentioned specification silk material system is broken into rivet, and carry out electrical performance test, experimental condition is direct current, motor load, voltage 14V, electric current 28A, the disconnected 4.8s of logical 0.2s, test number (TN) 100,000 times.
Material physical property contrast is as shown in the table
Classification Hardness (HV) Tensile strength (MPa) Elongation (%)
Oxidation in conventional 120-122 420 13
The present invention 94-96 310 26
As shown in Figure 3, the metallographic structure of the present embodiment is even in metallographic structure, does not occur that a large amount of silver is assembled, oxide buildup phenomenon.
Fig. 6 is the photo after embodiment of the present invention material electrical performance test, and material transfer is less.
 
embodiment bis-:
(1) Ag ingot, Sn ingot, additive (In, Zr, Co) are carried out to melting, composition proportion be Ag92Sn5In2Ce0.3Zr0.3Co0.2(by weight percentage) pour into billet, then with lathe, remove surface scale 3mm;
(2) extruding, 770 ℃ of heating-up temperatures, are incubated 3h, obtain the silk material of Φ 3mm;
(3) pull to Φ 2.5mm;
(4) thrust also briquetting, wherein fracture of wire length is 20mm, spindle diameter 85mm, pressure 12MPa;
(5) oxidizing temperature is 850 ℃, and oxygen is pressed 2MPa, and oxidization time is 10h, spindle diameter 85mm after multiple pressure, and multiple pressure pressure 60MPa, then spindle surface car removes 2mm;
(6) extruding heating-up temperature is 800 ℃, insulation 8h, and then 900 ℃ of temperature retention time 2h, push rear silk material specification Φ 5mm, and then hot pull is to silk material finished product Φ 1.5mm;
(7) above-mentioned specification silk material system is broken into rivet, and carry out electrical performance test, experimental condition is direct current, motor load, voltage 14V, electric current 28A, the disconnected 4.8s of logical 0.2s, test number (TN) 100,000 times.
Material physical property contrast is as shown in the table
Classification Hardness (HV) Tensile strength (MPa) Elongation (%)
Interior oxidation 120-122 420 13
The present invention 92-94 300 30
As shown in Figure 4, the metallographic structure of the present embodiment is even in metallographic structure, does not occur oxide buildup, silver-colored clustering phenomena.
Fig. 7 is the photo of embodiment of the present invention material after electrical performance test, and material transfer is less.

Claims (8)

1. a preparation method for the tin-oxygen-silver electric contact material of even tissue, is characterized in that comprising the following steps:
(1) silver ingot, tin slab, indium ingot are put into mid-frequency melting furnace melting, add additive in process, then ingot casting is through surface treatment;
(2) ingot casting after step (1) processing is thermally processed into a material;
(3) the silk material after step (2) hot working is cold worked into small dimension silk material;
(4) the small dimension silk material of step (3) is cut off, briquetting becomes spindle;
(5) spindle after step (4) processing is inserted in aerobic environment, be oxidized, then pressure, surface treatment again;
(6) spindle after step (5) processing is thermally processed into a material.
2. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, it is characterized in that the described additive of described step (1) is at least two kinds in Cu, Ga, Ce, Zr, Co, by weight percentage, Ag 86-92%, Sn 5-8%, In 2-3%, Cu0-2%, Ga 0-1%, Ce 0-0.2%, Zr 0-0.3%, Co 0-0.5%.
3. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, the extruding heating-up temperature that it is characterized in that described step (2) is 660-770 ℃, temperature retention time 3-6h, silk material diameter 4-7mm.
4. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, the cold working that it is characterized in that described step (3) is silk material drawing mode.
5. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, the fracture of wire length that it is characterized in that described step (4) is 20-30mm, spindle diameter 80-85mm, pressure 8-12MPa.
6. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, the oxidizing temperature that it is characterized in that described step (5) is 750-850 ℃, oxidization time is 10-15h, described aerobic environment oxygen is pressed in the oxygen atmosphere for 2MPa-5MPa, the multiple sub-diameter 80-85mm of briquetting, pressure 50-60MPa, then removes spindle surface layer thickness 2-4mm with lathe.
7. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, the extruding heating-up temperature that it is characterized in that described step (6) is 800-900 ℃, temperature retention time 5-10h, silk material diameter 3-5mm.
8. according to the preparation method of the tin-oxygen-silver electric contact material of a kind of even tissue of claim 1, the thermal processing method that it is characterized in that described step (6) is any two combinations in high-frequency heating, heating in medium frequency, resistance heating.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551838A (en) * 2015-12-29 2016-05-04 桂林电器科学研究院有限公司 Processing method for silver-tin oxide-indium oxide flake electrical contact containing additive
CN107598176A (en) * 2017-08-02 2018-01-19 福达合金材料股份有限公司 A kind of preparation technology of siluer metal oxide contact material
CN108220650A (en) * 2017-12-27 2018-06-29 昆明贵金属研究所 A kind of multicomponent oxide enhancing silver-based electric contact material and preparation method thereof
CN111215839A (en) * 2018-11-23 2020-06-02 宁波江丰电子材料股份有限公司 Forming method of coating material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1823176A (en) * 2003-07-18 2006-08-23 住友电气工业株式会社 Electric contact and electrical equipment including the same
CN101944441A (en) * 2010-08-31 2011-01-12 扬州乐银合金科技有限公司 Silver zinc oxide electric contact material and preparation method thereof
CN102796914A (en) * 2012-08-21 2012-11-28 福达合金材料股份有限公司 Preparation method of refined silver tin oxide crystal grain
US20130266791A1 (en) * 2010-12-30 2013-10-10 Wenzhou Hongfeng Electrical Alloy Co., Ltd. Method of preparing Ag- based oxide contact materials with directionally arranged reinforcing particles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1823176A (en) * 2003-07-18 2006-08-23 住友电气工业株式会社 Electric contact and electrical equipment including the same
CN101944441A (en) * 2010-08-31 2011-01-12 扬州乐银合金科技有限公司 Silver zinc oxide electric contact material and preparation method thereof
US20130266791A1 (en) * 2010-12-30 2013-10-10 Wenzhou Hongfeng Electrical Alloy Co., Ltd. Method of preparing Ag- based oxide contact materials with directionally arranged reinforcing particles
CN102796914A (en) * 2012-08-21 2012-11-28 福达合金材料股份有限公司 Preparation method of refined silver tin oxide crystal grain

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551838A (en) * 2015-12-29 2016-05-04 桂林电器科学研究院有限公司 Processing method for silver-tin oxide-indium oxide flake electrical contact containing additive
CN107598176A (en) * 2017-08-02 2018-01-19 福达合金材料股份有限公司 A kind of preparation technology of siluer metal oxide contact material
CN107598176B (en) * 2017-08-02 2020-06-05 福达合金材料股份有限公司 Preparation process of silver metal oxide electrical contact material
CN108220650A (en) * 2017-12-27 2018-06-29 昆明贵金属研究所 A kind of multicomponent oxide enhancing silver-based electric contact material and preparation method thereof
CN111215839A (en) * 2018-11-23 2020-06-02 宁波江丰电子材料股份有限公司 Forming method of coating material

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Patentee before: FUDA ALLOY MATERIALS Co.,Ltd.