CN110064762A - A kind of silver-tungsten carbide contact material and preparation method thereof - Google Patents
A kind of silver-tungsten carbide contact material and preparation method thereof Download PDFInfo
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- CN110064762A CN110064762A CN201910424585.2A CN201910424585A CN110064762A CN 110064762 A CN110064762 A CN 110064762A CN 201910424585 A CN201910424585 A CN 201910424585A CN 110064762 A CN110064762 A CN 110064762A
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of preparation methods of silver-tungsten carbide contact material, the following steps are included: S1, silver nitrate solution, polyethylene glycol, sodium hydroxide solution and glucose solution be uniformly mixed, reduction reaction is carried out under sonic oscillation and stirring condition, silver is precipitated and to be wrapped in tungsten carbide powder external, forms silver package carbonization tungsten composite powder；S2, green compact is pressed into after mixing the silver package tungsten carbide powder and silver powder；S3, green compact made of S2 and silver bullion are placed in sintering, infiltration in the sintering furnace of ammonia dissolving atmosphere protection, obtain silver-tungsten carbide contact material.The invention also discloses the silver-tungsten carbide contact materials being prepared using above-mentioned preparation method.The silver-tungsten carbide contact material that the present invention is prepared is high compactness infiltration type silver tungsten carbide material, and tungsten carbide mass ratio is in 40%-90%.
Description
Technical field
The invention belongs to the technical field of contact material more particularly to a kind of silver-tungsten carbide contact material and its preparation sides
Method.
Background technique
Requirement with power grid distribution end to electrical reliability is higher and higher, and appliance manufacturers just constantly release more high breaking
The LV power distribution product of index.Part electronics plastic casing breaker can reach capacity the index of disjunction 150kA.Electric appliance disjunction
The promotion of index means that the thermal break-through power of electric arc when disjunction is extremely powerful, and contact material causes easily by arc erosion at this time
Electric appliance is not turned on, and is broken down.
Comprehensively consider materials conductive, anticorrosive etc. performance, it is the most general in high breaking type low-voltage circuit breaker at this stage
It is silver-colored tungsten carbide (AgWC) material all over the material used.On the one hand, the tungsten carbide particle containing micron order dispersion in such material
As reinforced phase, material arc ablation resistance ability can greatly be promoted；On the other hand, such material uses powder metallurgic method,
The production of liquid-phase sintering (infiltration) technique can ensure that silver forms good wet with tungsten carbide particle, to avoid material in high temperature
It splashes under arcing.
For the arc resistant ability for promoting silver-colored tungsten carbide material, it usually needs reduce the tungsten carbide size in material, simultaneously
Promote the content of tungsten carbide.The silver-colored tungsten carbide material used on the special equipments such as large-scale smelting furnace, or even needing will carbonization
The mass percent of tungsten is promoted to 60% or even higher, at the same the particle mean size of tungsten carbide to drop to 1 micron hereinafter, this
Very high requirement just is proposed to the manufacture craft of material.
When tungsten carbide content is excessively high in silver-colored tungsten carbide powder, while tungsten carbide size is too small, there are huge in mixed powder
It is adjacent with particle inevitably to encounter a large amount of tungsten carbide particle in powder forming process for big tungsten carbide particle surface
Situation.And due to its ultrahigh hardness, when tungsten carbide particle contacts compression with particle surface, hardly it is plastically deformed, because
Intermeshing can not be formed between this particle, cause easily cracked or even green compact in green compact that can not form.
Therefore, the silver-colored tungsten carbide material for making high tungsten carbide content is industry problem all the time.This problem is also in phase
When limiting the further promotion of electric appliance interrupting performance in big degree.
Conventional cladding process not can avoid tungsten carbide particle reunion in chemical reaction process, and the silver for reacting generation will not
Parcel form tungsten carbide particle, but the aggregate of several tungsten carbide particles is wrapped up, therefore exists in coated powder a large amount of
Tungsten carbide particle and particle directly contact, powder formability is poor.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of silver-tungsten carbide contact material and its preparation side
Method.The compactness of silver-tungsten carbide contact material can be effectively improved.
The present invention is achieved by the following technical solutions:
A kind of preparation method of silver-tungsten carbide contact material, includes the following steps:
S1, silver nitrate solution, polyethylene glycol, sodium hydroxide solution and glucose solution are uniformly mixed, in sonic oscillation
With carry out reduction reaction under stirring condition, silver is precipitated and is wrapped in tungsten carbide powder external, form silver package tungsten carbide composite powder
Body；The dosage of the silver nitrate solution is from the dosage conversion of silver, the dosage m of the silverAgIt is calculated using following formula:
Wherein mWCIt is tungsten carbide gross mass used, ρAgIt is silver-colored
Density, ρWCIt is the density of tungsten carbide, d is the average grain diameter of tungsten carbide powder, and the unit of d is um, and x is that silver package tungsten carbide is compound
The thickness of silver layer in powder；
S2, green compact is pressed into after mixing the silver package tungsten carbide powder and silver powder；
S3, green compact made of S2 and silver bullion are placed in sintering, infiltration in the sintering furnace of ammonia dissolving atmosphere protection, obtain silver-colored carbon
Change tungsten contact material.
Further, in the S1, silver package carbonization tungsten composite powder in silver layer with a thickness of 10~200nm.
Further, in the S1, further includes: tungsten carbide powder and silver nitrate solution are added in reaction vessel, then to
It is added polyethylene glycol in reaction vessel, sonic oscillation and stirring are uniformly mixed it, sonic oscillation and stirring are then kept, to anti-
It answers and sodium hydroxide solution is added in container, until solution ph reaches 8~9, continuing sonic oscillation and stirring later makes its mixing
Uniformly, ultrasonic agitation is then kept, glucose solution is gradually added into reaction vessel, the warm 0.5~2L/min of speed is added,
After silver ion in the solution is precipitated completely, continue sonic oscillation and stirring, carry out reduction reaction, the silver of precipitation is wrapped in carbonization
Silver package carbonization tungsten composite powder is formed on tungsten powder body, the reactant solution in reaction vessel is filtered, and isolates silver package carbon
Change tungsten composite powder, and is cleaned and dried.
Further, the solid-to-liquid ratio of the tungsten carbide powder and silver nitrate solution is 5-70g/L.
Further, in the S1, the molecular weight of polyethylene glycol is 500~20000, and additional amount is tungsten carbide powder weight
7~12%.By addition polyethylene glycol as stabilizer, polyethylene glycol is covered on tungsten carbide particle table in ultrasonic procedure
Face increases particle surface potential energy, it is suppressed that tungsten carbide particle is reunited.
Further, in the S1, the concentration of the glucose solution is 30~300g/L.It is molten using low concentration glucose
Liquid is as reducing agent, it is suppressed that silver-colored too fast precipitation, while cooperating the growth inhibition effect of polyethylene glycol, effectively control silver-colored shell
The thickness of layer.
Further, in the S1, the average grain diameter of the tungsten carbide powder is 0.5~8 μm.
Further, in the S2, the porosity of green compact is 5~55%.
The present invention also proposes that a kind of mass percent of tungsten carbide is 40~90% silver-tungsten carbide contact material.
The present invention is obtained by covering the fine silver shell that a layer thickness is 10~200nm in tungsten carbide powder extra-granular
The tungsten carbide of monodisperse core-shell structure-argentum composite powder body, i.e. silver packet carbonization tungsten composite powder, with fine silver in tungsten carbide-tungsten carbide
Physical isolation is established between particle.Since silver has very good ductility, in powder compression forming process, phase
It can be intermeshed by being covered on the fine silver shell of outer layer between adjacent tungsten carbide particle, mechanical bond be formed, to be substantially improved
The processability of powder has ensured the molding of high tungsten carbide content silver tungsten carbide mixed powder, has realized high tungsten carbide content
The production of high compactness silver tungsten carbide material.By above-mentioned technique, the formation of individual particle dispersion composite granule is ensured, has substantially mentioned
Powder formability is risen.
Detailed description of the invention
The present invention will be further explained below with reference to the attached drawings:
Fig. 1 is silver-tungsten carbide contact material tissue SEM photograph in the embodiment of the present invention 1；
The tissue SEM obtained when Fig. 2 is in the embodiment of the present invention 1 to common silver-tungsten carbide contact material performance detection shines
Piece；
Fig. 3 is the metallograph of silver-tungsten carbide contact material in the embodiment of the present invention 1；
Fig. 4 is the metallograph of silver-tungsten carbide contact material in the embodiment of the present invention 2.
Specific embodiment
Next combined with specific embodiments below invention is further explained, but does not limit the invention to these tools
Body embodiment.One skilled in the art would recognize that present invention encompasses may include in Claims scope
All alternatives, improvement project and equivalent scheme.
Embodiment 1
A kind of preparation method of silver-tungsten carbide contact material, includes the following steps:
A, silver nitrate solid 3.25kg is dissolved in 2500L deionized water, configures silver nitrate solution；
B, 33.2kg tungsten carbide powder and silver nitrate solution are added in reaction vessel, then the poly- second of 3kg is added into container
Two pure and mild appropriate amount of deionized water, ultrasound and stirring 2 hours；
C, ultrasound and stirring are kept, sodium hydroxide solution is gradually added into container, until solution ph reaches 8-9, is protected
Hold ultrasound and stirring 0.5 hour；
D, ultrasound and stirring are kept, the glucose solution that concentration is 100g/L is gradually added into container, speed is added
1.5L/min keeps ultrasound and stirring 0.5 hour until silver is precipitated completely in solution；
E, solution is filtered, obtained composite granule is cleaned twice with deionized water, and drying is stand-by；
F, the composite granule that step e is obtained is put into the mixed powder machine of V-type with silver powder and is mixed 10~12 hours, obtain argentiferous
5% AgWC powder；
G, using powder molding equipment, AgWC powder obtained in step f is pressed into green compact；
H, green compact obtained in step g and silver bullion are placed in ammonia dissolving atmosphere protection sintering furnace, 1000 DEG C of sintering, infiltrations
It 2 hours, comes out of the stove after cooling, silver-tungsten carbide contact material is obtained after cleaning.
It is understood that step h is the prior art, the setting of sintering temperature and infiltration time are not limited to the example,
Details are not described herein.
The silver-tungsten carbide contact material obtained using the preparation method of the silver-tungsten carbide contact material in the present embodiment 1,
Metallograph is as shown in figure 3, it organizes SEM photograph as shown in Figure 1.Commercially available silver-colored tungsten carbide material is carried out in the present embodiment 1
Performance test, obtained tissue SEM photograph are as shown in Figure 2.The silver it is found that in the present embodiment 1 is compared from attached drawing 1 and attached drawing 2
There is no micropore in tungsten carbide contact material tissue, silver is well combined with tungsten carbide, and compactness is very high.
Embodiment 2
A kind of preparation method of silver-tungsten carbide contact material, includes the following steps:
A, silver nitrate solid 6.5kg is dissolved in 4000L deionized water, configures silver nitrate solution；
B, 66.79kg tungsten carbide powder and silver nitrate solution are added in reaction vessel, then the poly- second of 5kg is added into container
Two pure and mild appropriate amount of deionized water, ultrasound and stirring 2 hours；
C, ultrasound and stirring are kept, sodium hydroxide solution is gradually added into container, until solution ph reaches 8-9, is protected
Hold ultrasound and stirring 0.5 hour；
D, ultrasound and stirring are kept, the glucose solution that concentration is 100g/L is gradually added into container, speed 3L/ is added
Min keeps ultrasound and stirring 0.5 hour after silver is all precipitated in solution；
E, solution is filtered, obtained composite granule is cleaned twice with deionized water, and drying is stand-by；
F, composite granule obtained in step e is put into the mixed powder machine of V-type with silver powder and is mixed 10~12 hours, obtain argentiferous
The AgWC powder of amount 5%；
G, using powder molding equipment, the AgWC powder that step f is obtained is pressed into green compact；
H, green compact and silver bullion that step g is obtained are placed in the sintering furnace of ammonia dissolving atmosphere protection, 1000 DEG C of sintering, infiltrations
It 2 hours, comes out of the stove after cooling, obtains silver-tungsten carbide contact material.
It is understood that step h is the prior art, the setting of sintering temperature and infiltration time are not limited to the example,
Details are not described herein.
The silver-tungsten carbide contact material obtained using the preparation method of the silver-tungsten carbide contact material in the present embodiment 2,
Metallograph is as shown in Figure 4.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications also regard
For protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silver-tungsten carbide contact material, which comprises the steps of:
S1, silver nitrate solution, polyethylene glycol, sodium hydroxide solution and glucose solution are uniformly mixed, in sonic oscillation and are stirred
Reduction reaction is carried out under the conditions of mixing, silver is precipitated and is wrapped in tungsten carbide powder external, form silver package carbonization tungsten composite powder；Institute
The dosage of silver nitrate solution is stated from the dosage conversion of silver, the dosage m of the silverAgIt is calculated using following formula:
Wherein mWCIt is tungsten carbide gross mass used, ρAgIt is the density of silver,
ρWCIt is the density of tungsten carbide, d is the average grain diameter of tungsten carbide powder, and the unit of d is um, and x is silver package carbonization tungsten composite powder
The thickness of middle silver layer；
S2, green compact is pressed into after mixing the silver package tungsten carbide powder and silver powder；
S3, green compact made of S2 and silver bullion are placed in sintering, infiltration in the sintering furnace of ammonia dissolving atmosphere protection, obtain silver-colored tungsten carbide
Contact material.
2. the preparation method of silver-tungsten carbide contact material according to claim 1, which is characterized in that in the S1, silver packet
Wrap up in carbonization tungsten composite powder in silver layer with a thickness of 10~200nm.
3. the preparation method of silver-tungsten carbide contact material according to claim 1, which is characterized in that in the S1, also wrap
It includes: tungsten carbide powder and silver nitrate solution being added in reaction vessel, then polyethylene glycol is added into reaction vessel, sonic oscillation
It is uniformly mixed it with stirring, sonic oscillation and stirring is then kept, sodium hydroxide solution is added into reaction vessel, until molten
Liquid pH value reaches 8~9, and continuing sonic oscillation and stirring later is uniformly mixed it, ultrasonic agitation is then kept, to reaction vessel
In be gradually added into glucose solution, the warm 0.5~2L/min of speed is added, after silver ion in the solution is precipitated completely, continuation
Sonic oscillation and stirring carry out reduction reaction, and the silver of precipitation, which is wrapped on tungsten carbide powder, forms silver package tungsten carbide composite powder
Body filters the reactant solution in reaction vessel, isolates silver package carbonization tungsten composite powder, and be cleaned and dried.
4. the preparation method of silver-tungsten carbide contact material according to claim 3, which is characterized in that the tungsten carbide powder
Solid-to-liquid ratio with silver nitrate solution is 5-70g/L.
5. the preparation method of silver-tungsten carbide contact material according to claim 3, which is characterized in that in the S1, poly- second
The molecular weight of glycol is 500~20000, and additional amount is the 7~12% of tungsten carbide powder weight.
6. the preparation method of silver-tungsten carbide contact material according to claim 3, which is characterized in that described in the S1
The concentration of glucose solution is 30~300g/L.
7. the preparation method of silver-tungsten carbide contact material according to claim 3, which is characterized in that described in the S1
The average grain diameter of tungsten carbide powder is 0.5~8 μm.
8. the preparation method of silver-tungsten carbide contact material according to claim 1, which is characterized in that in the S2, green compact
Porosity be 5~55%.
9. a kind of silver-tungsten carbide contact material, which is characterized in that by silver carbonization tungsten contact according to any one of claims 1 to 8
The preparation method of material is prepared.
10. silver-tungsten carbide contact material according to claim 9, which is characterized in that the mass percent of the tungsten carbide
It is 40~90%.
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| CN201910424585.2A CN110064762B (en) | 2019-05-21 | 2019-05-21 | Silver tungsten carbide contact material and preparation method thereof |
| DE102020113766.4A DE102020113766A1 (en) | 2019-05-21 | 2020-05-20 | Silver tungsten carbide contact material and manufacturing process therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111618297A (en) * | 2020-04-21 | 2020-09-04 | 陕西斯瑞新材料股份有限公司 | Preparation method of rapid sintering forming silver-based contact |
| CN112170862A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver-tungsten contact material |
| CN115478188A (en) * | 2022-08-24 | 2022-12-16 | 苏州银孚新材料有限公司 | Preparation method of silver tungsten carbide electrical contact material |
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| GB1411500A (en) * | 1972-09-12 | 1975-10-29 | Siemens Ag | Preparation of a catalytic material |
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| CN101717928A (en) * | 2008-10-09 | 2010-06-02 | 北京有色金属研究总院 | Method for preparing compound powder used for abrasion-resistant self-lubricating coating |
| CN101817079A (en) * | 2009-10-31 | 2010-09-01 | 福达合金材料股份有限公司 | Method for preparing framework coating powder of silver-tungsten carbide contact material |
| CN103447526A (en) * | 2013-09-11 | 2013-12-18 | 中南大学 | Preparation method of nanometer WC-Co composite powder |
| CN103824710A (en) * | 2014-03-10 | 2014-05-28 | 温州中希电工合金有限公司 | Method for preparing silver-tungsten carbide contact material from silver-coated tungsten carbide powder and silver-tungsten carbide contact material |
| CN104493170A (en) * | 2014-12-30 | 2015-04-08 | 桂林电器科学研究院有限公司 | Preparation method of flakey or rivet-shaped silver and tungsten electrical contact material |
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| CN111618297A (en) * | 2020-04-21 | 2020-09-04 | 陕西斯瑞新材料股份有限公司 | Preparation method of rapid sintering forming silver-based contact |
| CN112170862A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver-tungsten contact material |
| CN115478188A (en) * | 2022-08-24 | 2022-12-16 | 苏州银孚新材料有限公司 | Preparation method of silver tungsten carbide electrical contact material |
| CN115478188B (en) * | 2022-08-24 | 2023-04-18 | 苏州银孚新材料有限公司 | Preparation method of silver tungsten carbide electrical contact material |
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| CN110064762B (en) | 2021-12-14 |
| DE102020113766A1 (en) | 2020-11-26 |
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