CN101510479B - Method for preparing siller tin oxide electric contact material - Google Patents
Method for preparing siller tin oxide electric contact material Download PDFInfo
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- CN101510479B CN101510479B CN2009100644879A CN200910064487A CN101510479B CN 101510479 B CN101510479 B CN 101510479B CN 2009100644879 A CN2009100644879 A CN 2009100644879A CN 200910064487 A CN200910064487 A CN 200910064487A CN 101510479 B CN101510479 B CN 101510479B
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- tin oxide
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Abstract
The invention discloses a preparation method of a silver tin oxide electrical contact material, which comprises the following steps: SnO2 is put into 1 percent to 20 percent SnCl2 for ultrasonic oscillation treatment for 1min to 100min; the powder after treatment is subjected to silver wrapping treatment in a diamminesilver solution and then milled and mixed with Ag powder according to ratio (tinoxide with the content of 6 wt percent to 15 wt percent and silver with the content of 85 wt percent to 94 wt percent); then the mixed power is heated to 200 DEG C to 600 DEG C, kept at the temperature for 1h to 4h and then subjected to isopressing formation; an obtained ingot is sintered for 1h to 5h at the temperature of 700 DEG C to 900 DEG C and extruded into a wire material at the extrusion ratio of 100 to 400 times at the temperature of 700 DEG C to 900 DEG C. The silver tin oxide material prepared by the method has low resistivity and good electrical using property and processing performance, long service life, simple production technique, low energy consumption and low product cost, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of electrical material and preparation field technology thereof, particularly relate to a kind of preparation method of siller tin oxide electric contact material.
Background technology
Electrical contact is the contact element of appliance switch, instrument and meter, is the critical material of electrical equipment such as contactor, relay, plays a part connection, disjunction and transmission current.Its main materials used is silver-based materials such as fine silver, thin brilliant silver, silver-colored cerium, silver-colored nickel, silver-colored nickel graphite, Agcdo, Ag-ZnO, silver-colored tungsten.In numerous Ag-based electrical contact materials, combination properties such as the processing characteristics of Ag-CdO, contact resistance, anti electric arc corrosion are better, use comparatively extensive in existing market.But because the Ag-CdO material produces the cadmium poison inevitably in production, use, cause environmental pollution, and along with low-voltage electrical apparatus requires high reliability and long-life day by day miniaturization the time, shortcoming such as the Ag-CdO material also exposes its melt resistance can be poor, the arc resistant scaling loss is serious.Ag-SnO
2Electrical contact material is a kind of non-toxic material that fast development is in recent years got up, and it has Heat stability is good, anti-arc erosion and resistance fusion welding can be good, and the scope of application can reach 10～1000A, is comparatively desirable electrical contact material.But because Ag and SnO
2The interface in conjunction with poor, the contact resistance of silver tin oxide material is big, influenced its electric serviceability, and plasticity is low, shortcomings such as processing difficulties have also limited Ag-SnO
2The application of material.
Development siller tin oxide contact adopts two kinds of methods both at home and abroad: " internal oxidation " and " powder metallurgic method ".The main internal oxidation that adopts of Japan, this method needs to add indium in the process of producing the siller tin oxide contact, so that Sn is oxidized to SnO
2, the method production cost height, technology are complicated.Germany adopts powder metallurgic method to produce the siller tin oxide contact, and properties of product are stable, obtained practical application.
Present domestic patent of also applying for some siller tin oxide aspects prepares silver tin oxide material as the surface modifying method of employings such as CN02146696.3 patent and CN03100430.X patent, can partly solve the problem of processing characteristics, but have SnO
2In surface treatment process,, cause electric serviceability to be affected by the problem of metal ion pollution, and complex process, the cost height.The processing characteristics and the electrical property of the tin oxide or indium oxide electrical contact of Chinese patent CN02132791.2 employing internal oxidation preparation are better, cause it with high costs but add indium.
Summary of the invention
Technical problem to be solved by this invention is the deficiency at above existing silver tin oxide material preparation technology, and a kind of preparation method of siller tin oxide electric contact material is provided.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme to realize:
The preparation method of a kind of siller tin oxide electric contact material of the present invention, the raw material of its siller tin oxide electric contact material is made up of silver powder and tin ash powder, and its preparation method is:
(1) SnO
2Powder carries out pre-treatment.Its method is: with SnO
2Powder is put into the SnCl of 1%～20%wt
2In the solution, SnO wherein
2With the mass ratio of solution be 1: 10～1: 50; Supersonic oscillations 1～100min washs then, dries.Described SnCl
2Solution, preferred concentration is 2～6%, preferred concentration is 4%.Described supersonic oscillations mode, preferable condition are 40kHz, vibration 5～40min, and preferred duration of oscillation is 10min.
(2) powder that (1) oven dry is obtained is put into the AgNO that contains 1.75～17.5g/L in 1: 10～1: 20 ratio of mass ratio
324%～26%NH with 5～100ml/L
3H
2In the silver ammino solution of O, add 37%～40% formalin with the isopyknic 1～100ml/L of silver ammino solution again, the 40kHz supersonic oscillations are handled 10min, and preparation silver coats the tin ash powder, and washing, oven dry; Described AgNO
3Solution, preferred concentration is 10g/L～17.5g/L, preferred concentration is 16g/L; Described formalin, preferred concentration is 15～60ml/L, 37%～40% formalin, preferred concentration is 50ml/L 37%～40% formalin.
(3) powder that (2) oven dry is obtained and silver powder are according to SnO
26～15wt%: Ag 85～94wt% puts into ball grinder and carries out ball milling mixing 1～10 hour, and powder is heated to 400 ℃～600 ℃ after will mixing, and is incubated 1～4 hour;
(4) powder that (3) are obtained was at the forming under the pressure of 100～400MPa, 700 ℃～900 ℃ sintering 1～5 hour;
(5) ingot blank that (4) are obtained carries out hot extrusion under 700 ℃～900 ℃, and extrusion ratio is 100～400, obtains the silver tin oxide silk material.
The preparation method of the siller tin oxide electric contact material of this patent avoids the pollution of powder simultaneously, thereby has guaranteed the electric serviceability of material because drawing abillity in conjunction with problem, can be improved in the interface of having adopted surface modification technology solution siller tin oxide.It is simple that this method has production technology, and cost is low, the characteristics that production efficiency is high.
The electrical contact material of the present invention's preparation has following performance: density is 9.9～10.5g/cm3, hardness HV75～120, tensile strength 250～350MPa, elongation 10%～40%, resistivity 2.05～2.25 μ Ω cm.The contact material of producing with this method satisfies the every performance index in the GB/T20235-2006 siller tin oxide electric contact material technical conditions, and the materials processing performance is good, processing does not have the cracking situation during rivet, is significantly improved with the cracking ratio of prior art 10%～30%.
By adopting these technical schemes, the preparation method of siller tin oxide electric contact material of the present invention compares with other siller tin oxide preparation technology, and its beneficial effect is:
(1) pre-treatment, silver coat in the processing procedure, do not contact with other metal ion outside Ag, the Sn, make SnO
2Powder can be not contaminated, thereby guarantee that material has low resistivity and good electric serviceability.
(2) Zhi Bei silver tin oxide material good processability can be prepared into the electrical contact material of a material and different shape, finished material rate height, and the processing rivet does not have cracking.
(3) production technology is simple, and heat treatment period is short, and energy consumption is little, and product cost is low, is fit to suitability for industrialized production.
Embodiment
Embodiment 1
Take by weighing 300g tin oxide, containing SmCl
2Handle 10min with the 40kHz supersonic oscillations in 5% the 3000g solution, add after the washing and drying and contain AgNO
317.5g/L, 24%～26%NH
3H
3The solution 4000g of O 50ml/L adds solution that equal-volume contains 37%～40%HCOH 18ml/L again and carries out silver and coat and handle 40kHz ultrasonic Treatment 30min.To coat the back powder and put into ball grinder with deionized water wash, oven dry back and 2700g silver powder and carry out ball milling and mix, the mixed powder time is 1 hour.Mixed powder is heated to 500 ℃ under vacuum, is incubated 3 hours.The gum cover of then powder being packed into, isostatic compaction under 200MPa 800 ℃ of sintering 2 hours, is heated to ingot blank 850 ℃ again, adopts 200 times of extrusion ratios, is squeezed into a material.Silk material after the extruding is cold drawing to final size, and is processed into rivet.The electrical contact material of the present invention's preparation has following performance: density is 9.9～10.5g/cm3, hardness HV75～120, tensile strength 250～350MPa, elongation 15%～40%, resistivity 2.05～2.25 μ Ω cm, and the materials processing performance is good, does not have the cracking situation during processing rivet.
Embodiment 2
Take by weighing 150g tin oxide, containing SmCl
2Handle 10min with the 40kHz supersonic oscillations among 3% the solution 2000g, add after the washing and drying and contain AgNO
315g/L, 24%～26%NH
3H
3The solution 2000g of O 50ml/L adds the equal-volume solution that contains 37%～40%HCOH 18ml/L again and carries out silver coating processing, 40kHz ultrasonic Treatment 30min.Mix with 1725g silver powder ball milling after will coating back powder washing and drying, mixing the powder time is 4 hours.Mixed powder is carried out reprocessing, promptly under vacuum, be heated to 600 ℃, be incubated 1 hour.With the gum cover of packing into of the powder after the reprocessing, isostatic compaction under 200MPa 860 ℃ of sintering 4 hours, is squeezed into a material under 800 ℃ of 225 times of extrusion ratios.
Embodiment 3
Take by weighing 120g tin oxide, containing SnCl
2Handle 10min with the 40kHz supersonic oscillations among 10% the solution 2000g, add after the washing and drying and contain AgNO317.5g/L, 24%～26%NH
3H
3Among the solution 1250g of O 35ml/L, the solution that adds isopyknic 10ml/L 37%～40%HCOH again carries out silver and coats processing.Carry out ball milling with 880g silver powder after the powder washing after will coating and mix, mixing the powder time is 5 hours.Mixed powder is carried out reprocessing, promptly under vacuum, be heated to 590 ℃, be incubated 1 hour.With the gum cover of packing into of the powder after the reprocessing, isostatic compaction under 200MPa 860 ℃ of sintering 5 hours, is squeezed into a material under 800 ℃ of 225 times of extrusion ratios.
Claims (8)
1. the preparation method of a siller tin oxide electric contact material is characterized in that technical process is:
(1) SnO
2Powder carries out pre-treatment, and its method is: with SnO
2Powder is put into 1%～20% SnCl
2In the solution, SnO
2With the mass ratio of solution be 1: 10～1: 50, supersonic oscillations 1～100min washs then, dries;
(2) powder that (1) oven dry is obtained is put into the AgNO that contains 1.75～17.5g/L in 1: 10～1: 20 ratio of mass ratio
324%～26%NH with 5～100ml/L
3H
2In the silver ammino solution of O, add 37%～40% formalin with the isopyknic 1～100ml/L of silver ammino solution again, the 40kHz supersonic oscillations are handled 10min, and preparation silver coats the tin ash powder, and washing, oven dry;
(3) powder that (2) oven dry is obtained and silver powder are according to SnO
2: 6～15wt%; Ag:85～94wt% puts into ball grinder and carries out ball milling mixing 1～10 hour, and powder is heated to 400 ℃～600 ℃ after will mixing, and is incubated 1～4 hour;
(4) powder that (3) are obtained was at the forming under the pressure of 100～400MPa, 700 ℃～900 ℃ sintering 1～5 hour;
(5) ingot blank that (4) are obtained carries out hot extrusion under 700 ℃～900 ℃, and extrusion ratio is 100～400, obtains the silver tin oxide silk material.
2. according to the preparation method of the described siller tin oxide electric contact material of claim 1, it is characterized in that: described SnCl
2Solution concentration is 2～6%.
3. according to the preparation method of the described siller tin oxide electric contact material of claim 1, it is characterized in that: the supersonic oscillations frequency in the described step (1) is 40kHz, vibration 5～40min.
4. according to the preparation method of the described siller tin oxide electric contact material of claim 1, it is characterized in that: described SnCl
2Solution concentration is 4%; Supersonic oscillations frequency in the step (1) is 40kHz, vibration 10min.
5. according to the preparation method of the described siller tin oxide electric contact material of claim 1, it is characterized in that: described AgNO
3Solution concentration is 10g/L～17.5g/L.
6. according to the preparation method of the described siller tin oxide electric contact material of claim 1, it is characterized in that: described formalin is that concentration is the formalin of 15～60ml/L 37%～40%.
7. according to the preparation method of the described siller tin oxide electric contact material of claim 5, it is characterized in that: described AgNO
3Solution concentration is 16g/L.
8. according to the preparation method of the described siller tin oxide electric contact material of claim 6, it is characterized in that: described formalin is that concentration is the formalin of 50ml/L 37%～40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009100644879A CN101510479B (en) | 2009-03-18 | 2009-03-18 | Method for preparing siller tin oxide electric contact material |
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|---|---|---|---|
| CN2009100644879A CN101510479B (en) | 2009-03-18 | 2009-03-18 | Method for preparing siller tin oxide electric contact material |
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| CN101510479A CN101510479A (en) | 2009-08-19 |
| CN101510479B true CN101510479B (en) | 2010-08-25 |
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| CN101656160B (en) * | 2009-09-11 | 2012-10-31 | 昆明理工大学 | Preparing method of silver-base metal acid-salt electrical-contact composite material |
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| CN102151830B (en) * | 2011-03-08 | 2012-08-29 | 郴州雄风稀贵金属材料股份有限公司 | Preparation method of silver-rare earth refractory metal oxide electrical contact material |
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| CN105886813A (en) * | 2016-04-23 | 2016-08-24 | 东莞市华诺合金有限公司 | Silver tin oxide-wolfram electrical contact material and preparation method thereof |
| CN106220153B (en) * | 2016-06-30 | 2019-01-18 | 佛山市惠丰合金有限公司 | A kind of preparation method of electrical contact material |
| CN106098421A (en) * | 2016-08-05 | 2016-11-09 | 雷春生 | A kind of compound electric apparatus contact material of strong electric property and preparation method thereof |
| CN108010772B (en) * | 2017-12-08 | 2019-05-24 | 福达合金材料股份有限公司 | A kind of method that microwave heating prepares tin-oxygen-silver electric contact material |
| CN110802224A (en) * | 2018-08-06 | 2020-02-18 | 三菱电机株式会社 | Preparation method of silver-nickel-tin oxide composite powder and silver-nickel-tin oxide electrical contact material |
| CN110643847B (en) * | 2019-10-18 | 2021-08-27 | 宁波汉博贵金属合金有限公司 | Preparation method of silver tin oxide electric contact material |
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