CN101086923A - A making method of silver/graphite electrical contact - Google Patents

A making method of silver/graphite electrical contact Download PDF

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Publication number
CN101086923A
CN101086923A CN 200710072077 CN200710072077A CN101086923A CN 101086923 A CN101086923 A CN 101086923A CN 200710072077 CN200710072077 CN 200710072077 CN 200710072077 A CN200710072077 A CN 200710072077A CN 101086923 A CN101086923 A CN 101086923A
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China
Prior art keywords
silver
graphite
powder
expanded graphite
preparation
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Pending
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CN 200710072077
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Chinese (zh)
Inventor
魏彤
范壮军
解大收
张瑞
姚静
鄢少锋
段斐
李佳晶
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Harbin Engineering University
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Harbin Engineering University
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Priority to CN 200710072077 priority Critical patent/CN101086923A/en
Publication of CN101086923A publication Critical patent/CN101086923A/en
Pending legal-status Critical Current

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Abstract

The invention provides a method of producing high performance Argentine/ graphite electronic contactor material, it includes following steps: 1) expanded graphite and Argentine are combined to produce raw material powder, the weight ratio of expanded graphite is 3-10%, the weight ratio of Argentine is 90%-97%; 2) Argentine/ graphite raw material powder obtained in step 1) is sintered, and pressed to molding. The craftwork of the invention is easy, it convenient to operate, requirement of equipment is low, cost of production is low; the performance of product produced is well, nanophase graphite piece is even in material, resistivity is low, density is high, it possesses perfect performance of anti-arc corrosion.

Description

A kind of preparation method of electric silver/graphite contact
(1) technical field
The present invention relates to a kind of electric silver/graphite contact preparation method, belong to electrical contact material and make the field.
(2) background technology
Silver/graphite (Ag/C) electrical contact material is widely used on the various protection electrical equipment owing to have good resistance fusion welding and conductivity, low and stable contact resistance and excellent low temperature rise characteristic.In this material, thereby matrix silver provides good conductivity and don't has formed stable oxide and can not cause the rapid rising of contact resistance in use, the main effect of graphite is to stop the bonding and melting welding of contact, and does not form any insulant and make contact resistance become big.But graphite has the tendency and the aerial poor heat stability of stable arc, thereby arc resistant corrosive power difference is the greatest drawback of this material.
Adopt micron-sized synthetic graphite and silver powder to carry out powder mixing machine and powder metallurgy is the preparation technology commonly used of present Ag/C electrical contact, this is simple for process, flow process is few, low for equipment requirements, material recovery rate height, production cost are low, but gained finished product tissue odds is even, relatively poor, the arc erosion rate height of compactness.Therefore researchers make great efforts from the arc resistant corrosive power of raw material or preparation technology's raising electric silver/graphite contact always.Wang Ya equality [CN 03133585.3] adopts one dimension carbon nano-tube or carbon nano-fiber to replace the electric silver/graphite contact material of synthetic graphite preparation can significantly reduce the electroerosion rate of material when guaranteeing high conductivity, high-termal conductivity and improves the anti-wear performance of material.Germany Degussa company has developed the extrusion process of preparation electric silver/graphite contact, density height, ductility is good and the arc resistant corrosive power significantly improves electric silver/graphite contact material have been made, but above-mentioned two kinds of methods or cost of material are relatively more expensive, perhaps product yield is low, causes final production cost to improve.
(3) summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, easy operating, low for equipment requirements, production cost is low prepares the method for electric silver/graphite contact material with nanometer technology; With the good product performance of this method preparation, nano graphite flakes is evenly distributed in material, and resistivity is low, density is high, have good anti electric arc corrosion performance.
The preparation method of electric silver/graphite contact of the present invention comprises the steps:
1) according to the expanded graphite weight ratio be 3~10%, silver-colored weight ratio is that 90%~97% ratio is mixed and made into composite raw powder with expanded graphite and silver;
2) composite raw powder is just molded, sintering in sintering furnace, the multiple at last molded finished product that makes.
The present invention also has some technical characterictics like this:
1, the expanding volume of described expanded graphite is 10mL/g~600mL/g, is preferably 200mL/g~600mL/g;
2, the expanded graphite weight ratio is preferably 3~6% in the described silver/graphite composite raw powder, and silver-colored weight ratio is preferably 94%~97%;
3, described just molded be with composite raw powder pre-profiling under 20t pressure, described sintering be under nitrogen atmosphere protection in sintering furnace 600 ℃~850 ℃ sintering, be preferably 600 ℃~700 ℃, described multiple molded be the multiple molded finished product that makes under 50~60t pressure;
4, described compound be that high-energy ball milling machinery mixes: get expanded graphite and silver powder, in planetary high-energy ball mill, carry out ball milling and mix, rotating speed 100~250r/min,, ball powder ratio 10: 1~30: 1,5~40 hours ball milling time;
5, described ball powder ratio be preferably 10: 1~15: 1, the ball milling time is preferably: 10~20 hours;
6, the described compound chemistry coating mixing that is silver powder on the expanded graphite surface comprises the steps:
A) will mix with the expanded graphite powder with ammoniacal liquor complexing to the liquor argenti nitratis ophthalmicus that pH is 10~11, concentration is 0.5~5mol/L, fully stir;
B) step a) is made mixture carries out ultrasonic dispersion in the ultrasonic wave separating apparatus, the time is 0~20h, is preferably 3~10h;
C) be that 10%~40% hydrazine hydrate solution dropping or the form of spraying with liquid phase add in the made mixture of step b) while stirring with concentration, the silver of separating out is coated between expanded graphite powder particles surface or the graphite flake layer, forms silver/expanded graphite coated composite powder;
D) water-washing step c) made coated composite powder is extremely neutral, and in 100 ℃~200 ℃ dryings;
7, described liquor argenti nitratis ophthalmicus concentration is preferably 0.5~1mol/L, and hydrazine hydrate solution concentration is preferably 10%~20%.Compare with traditional handicraft, the present invention has following advantage:
Traditional handicraft adopts micron-sized synthetic graphite and silver powder to carry out powder mixing machine usually, carries out powder metallurgy then and prepares the Ag/C electrical contact, and gained finished product tissue odds is even, relatively poor, the arc erosion rate height of compactness.The present invention adopts a kind of expanded graphite with nanometer or micron pore size and fluffy sandwich construction and silver powder evenly compound by physics or chemical method, and the preparation electric silver/graphite contact is realized the equably dispersion of nano graphite flakes in silver matrix.This method technology is simple, easy operating, low for equipment requirements, production cost is low; With the good product performance of this method preparation, nano graphite flakes evenly distributes in material, and resistivity is low, the density height, has good anti electric arc corrosion performance.
(4) specific embodiment
The specific embodiment of the invention is as follows:
Embodiment 1:
With expanded graphite (expanding volume: 200mL/g; purity 99.5%) mix in planetary high-energy ball mill with silver powder (average grain diameter 70nm); revolution 100rpm; ball powder ratio 10: 1; the ball milling time is 40 hours; the pre-profiling under 20t pressure with mixed expanded graphite of ball milling and silver powder raw material, under nitrogen atmosphere protection in sintering furnace 600 ℃ of sintering, the multiple molded finished product (weight content of expanded graphite is 10%) that makes under 50t pressure at last.Its physical and mechanical properties sees Table 1.
Embodiment 2:
Expanded graphite (expanding volume: 300mL/g, purity 99.9%) is mixed in planetary high-energy ball mill with silver powder (average grain diameter 70nm), revolution 250rpm, ball powder ratio 30: 1, the ball milling time is 5 hours.The pre-profiling under 20t pressure with mixed expanded graphite of ball milling and silver powder raw material, under nitrogen atmosphere protection in sintering furnace 600 ℃ of sintering, the multiple molded finished product (weight content of expanded graphite is 5%) that makes under 50t pressure at last.Its physical and mechanical properties sees Table 1.
Embodiment 3:
With expanded graphite (expanding volume: 400mL/g, purity 99.9%) with mix with ammoniacal liquor complexing to the liquor argenti nitratis ophthalmicus that pH is 10, concentration is 0.5mol/L, fully stir.Drip 10% hydrazine hydrate solution then while stirring, obtain silver/expanded graphite coated composite powder.Wash prepared coated composite powder to neutral, and in 100 ℃ of dryings.With dried silver/expanded graphite coated composite powder pre-profiling under 20t pressure, under nitrogen atmosphere protection in sintering furnace 850 ℃ of sintering, the multiple molded finished product (weight content of expanded graphite is 3%) that makes under 60t pressure at last.Its physical and mechanical properties sees Table 1.
Embodiment 4:
With expanded graphite (expanding volume: 400mL/g, purity 99.9%) with mix with ammoniacal liquor complexing to the liquor argenti nitratis ophthalmicus that pH is 11, concentration is 5mol/L, fully stir.In ultrasonic dispersing machine, carry out ultrasonic dispersion 20 hours.Spraying while stirring adds 20% hydrazine hydrate solution then, obtains silver/expanded graphite coated composite powder.Wash prepared coated composite powder to neutral, and in 200 ℃ of dryings.With dried silver/expanded graphite coated composite powder pre-profiling under 20t pressure, under nitrogen atmosphere protection in sintering furnace 750 ℃ of sintering, the multiple molded finished product (weight content of expanded graphite is 5%) that makes under 55t pressure at last, its physical and mechanical properties sees Table 1.
Embodiment 5:
With expanded graphite (expanding volume: 600mL/g,, purity 99.9%) with mix with ammoniacal liquor complexing to the liquor argenti nitratis ophthalmicus that pH is 10, concentration is 2.5mol/L, fully stir.In ultrasonic dispersing machine, carry out ultrasonic dispersion 10 hours.Spraying while stirring adds 20% hydrazine hydrate solution then, obtains silver/expanded graphite coated composite powder.Wash prepared coated composite powder to neutral, and in 150 ℃ of dryings.With dried silver/expanded graphite coated composite powder pre-profiling under 20t pressure, under nitrogen atmosphere protection in sintering furnace 650 ℃ of sintering, the multiple molded finished product (weight content of expanded graphite is 5%) that makes under 55t pressure at last.Its physical and mechanical properties sees Table 1.
Embodiment 6:
With expanded graphite (expanding volume: 300mL/g, purity 99.9%) with mix with ammoniacal liquor complexing to the liquor argenti nitratis ophthalmicus that pH is 10, concentration is 0.5mol/L, fully stir.In ultrasonic dispersing machine, carry out ultrasonic dispersion 5 hours.Spraying while stirring adds 30% hydrazine hydrate solution then, obtains silver/expanded graphite coated composite powder.Wash prepared coated composite powder to neutral, and in 150 ℃ of dryings.With dried silver/expanded graphite coated composite powder pre-profiling under 20t pressure, under nitrogen atmosphere protection in sintering furnace 650 ℃ of sintering, the multiple molded finished product (weight content of expanded graphite is 4%) that makes under 55t pressure at last.
The multiple molded mechanical performance that makes finished product of table 1
Embodiment Expanded graphite weight contains wt% Conductivity m/ Ω mm 2 Density g/cm 3 Hardness Mpa Compactness %
Embodiment 1 10 34.5 8.70 513 98.5
Embodiment 2 5 35.6 8.72 574 99.0
Embodiment 3 3 38.4 8.75 605 99.5
Embodiment 4 5 37.9 8.81 629 99.3
Embodiment 5 5 39.5 8.82 638 99.9
Embodiment 6 4 38.6 8.80 633 99.7

Claims (8)

1, a kind of preparation method of electric silver/graphite contact is characterized in that:
1) according to the expanded graphite weight ratio be 3~10%, silver-colored weight ratio is that 90%~97% ratio is mixed and made into composite raw powder with expanded graphite and silver;
2) composite raw powder is just molded, sintering in sintering furnace, the multiple at last molded finished product that makes.
2, the preparation method of a kind of electric silver/graphite contact according to claim 1 is characterized in that the expanding volume of described expanded graphite is 10mL/g~600mL/g, is preferably 200mL/g~600mL/g.
3, the preparation method of a kind of electric silver/graphite contact according to claim 1 is characterized in that the expanded graphite weight ratio is preferably 3~6% in the described silver/graphite composite raw powder, and silver-colored weight ratio is preferably 94%~97%.
4, the preparation method of electric silver/graphite contact according to claim 1; it is characterized in that described just molded be with composite raw powder pre-profiling under 20t pressure; described sintering be under nitrogen atmosphere protection in sintering furnace 600 ℃~850 ℃ sintering; be preferably 600 ℃~700 ℃, described multiple molded be the multiple molded finished product that makes under 50~60t pressure.
5, the preparation method of a kind of electric silver/graphite contact according to claim 1, it is characterized in that described compound be that high-energy ball milling machinery mixes: get expanded graphite and silver powder, carrying out ball milling in planetary high-energy ball mill mixes, rotating speed 100~250r/min, ball powder ratio 10: 1~30: 1,5~40 hours ball milling time.
6, the preparation method of a kind of electric silver/graphite contact according to claim 5, it is characterized in that described ball powder ratio be preferably 10: 1~15: 1, the ball milling time is preferably: 10~20 hours.
7, the preparation method of a kind of electric silver/graphite contact according to claim 1, it is compound to it is characterized in that the described compound chemistry that is silver powder on the expanded graphite surface coats, and comprises the steps:
A) will mix with the expanded graphite powder with ammoniacal liquor complexing to the liquor argenti nitratis ophthalmicus that pH is 10~11, concentration is 0.5~5mol/L, fully stir;
B) step a) is made mixture carries out ultrasonic dispersion in the ultrasonic wave separating apparatus, the time is 0~20h, is preferably 3~10h;
C) be that 10%~40% hydrazine hydrate solution dropping or the form of spraying with liquid phase add in the made mixture of step b) while stirring with concentration, the silver of separating out is coated between expanded graphite powder particles surface or the graphite flake layer, forms silver/expanded graphite coated composite powder;
D) water-washing step c) made coated composite powder is washed to neutrality, and in 100 ℃~200 ℃ dryings.
8, the preparation method of a kind of electric silver/graphite contact according to claim 7 is characterized in that described liquor argenti nitratis ophthalmicus concentration is preferably 0.5~1mol/L, and hydrazine hydrate solution concentration is preferably 10%~20%.
CN 200710072077 2007-04-20 2007-04-20 A making method of silver/graphite electrical contact Pending CN101086923A (en)

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Application Number Priority Date Filing Date Title
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101196506B (en) * 2007-12-29 2011-11-02 哈尔滨工业大学 Device for testing electrical erosion property of electrical contact material
CN102294485A (en) * 2011-08-25 2011-12-28 哈尔滨东大高新材料股份有限公司 composite electric contact material and preparation method thereof
CN102496517A (en) * 2011-12-02 2012-06-13 深圳市奇辉电气有限公司 Novel load switch arcing contact and fixed contact thereof
CN103421970A (en) * 2012-03-30 2013-12-04 施耐德电器工业公司 Preparation method for silver-based electrical contact material
CN104741616A (en) * 2013-12-31 2015-07-01 施耐德电器工业公司 Electric contact material and preparation method thereof
CN105551861A (en) * 2016-02-26 2016-05-04 周懿涵 Preparation method of graphene-reinforced silver-based electric contact material
CN105965022A (en) * 2015-12-29 2016-09-28 桂林电器科学研究院有限公司 Processing method for slice-shaped silver graphite electrical contact material
CN107755686A (en) * 2017-10-12 2018-03-06 上海交通大学 A kind of nanometer silver carbon composite and preparation method thereof
CN113345725A (en) * 2021-06-01 2021-09-03 宁波毅立电子有限公司 Composite contact material and manufacturing method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101196506B (en) * 2007-12-29 2011-11-02 哈尔滨工业大学 Device for testing electrical erosion property of electrical contact material
CN102294485A (en) * 2011-08-25 2011-12-28 哈尔滨东大高新材料股份有限公司 composite electric contact material and preparation method thereof
CN102294485B (en) * 2011-08-25 2013-01-30 哈尔滨东大高新材料股份有限公司 Composite electric contact material and preparation method thereof
CN102496517A (en) * 2011-12-02 2012-06-13 深圳市奇辉电气有限公司 Novel load switch arcing contact and fixed contact thereof
CN103421970A (en) * 2012-03-30 2013-12-04 施耐德电器工业公司 Preparation method for silver-based electrical contact material
CN104741616A (en) * 2013-12-31 2015-07-01 施耐德电器工业公司 Electric contact material and preparation method thereof
CN105965022A (en) * 2015-12-29 2016-09-28 桂林电器科学研究院有限公司 Processing method for slice-shaped silver graphite electrical contact material
CN105965022B (en) * 2015-12-29 2018-04-10 桂林电器科学研究院有限公司 A kind of processing method of sheet silver-graphite electrical contact material
CN105551861A (en) * 2016-02-26 2016-05-04 周懿涵 Preparation method of graphene-reinforced silver-based electric contact material
CN105551861B (en) * 2016-02-26 2018-06-05 周懿涵 A kind of preparation method of graphene enhancing Ag-based electrical contact material
CN107755686A (en) * 2017-10-12 2018-03-06 上海交通大学 A kind of nanometer silver carbon composite and preparation method thereof
CN113345725A (en) * 2021-06-01 2021-09-03 宁波毅立电子有限公司 Composite contact material and manufacturing method thereof

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Open date: 20071212