CN110064762B - Silver tungsten carbide contact material and preparation method thereof - Google Patents
Silver tungsten carbide contact material and preparation method thereof Download PDFInfo
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- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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- 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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- 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
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- 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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- 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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Abstract
The invention discloses a preparation method of a silver tungsten carbide contact material, which comprises the following steps: s1, uniformly mixing a silver nitrate solution, polyethylene glycol, a sodium hydroxide solution and a glucose solution, carrying out reduction reaction under the conditions of ultrasonic oscillation and stirring, and separating out silver and wrapping the silver outside tungsten carbide powder to form silver-wrapped tungsten carbide composite powder; s2, mixing the silver-coated tungsten carbide powder and the silver powder and pressing the mixture into a pressed compact; and S3, placing the pressed compact and the silver block prepared in the step S2 in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration to obtain the silver tungsten carbide contact material. The invention also discloses the silver tungsten carbide contact material prepared by the preparation method. The silver tungsten carbide contact material prepared by the invention is a high-compactness infiltration type silver tungsten carbide material, and the mass ratio of tungsten carbide is 40-90%.
Description
Technical Field
The invention belongs to the technical field of contact materials, and particularly relates to a silver tungsten carbide contact material and a preparation method thereof.
Background
With the increasing requirements of the power grid distribution terminal on the reliability of the electric appliances, electric appliance manufacturers are continuously providing low-voltage distribution products with higher breaking indexes. Some electronic molded case circuit breakers can reach the index of maximum breaking of 150 kA. The improvement of the breaking index of the electric appliance means that the heat penetration force of the electric arc is extremely strong during breaking, and at the moment, the contact material is extremely easy to be eroded by the electric arc, so that the electric appliance cannot be connected and fails.
Considering the performances of the material in the aspects of conductivity, corrosion resistance and the like comprehensively, the silver tungsten carbide (AgWC) material is the most commonly used material in the high-breaking type low-voltage circuit breaker at the present stage. On one hand, the material contains micron-sized dispersed tungsten carbide particles as a reinforcing phase, so that the arc ablation resistance of the material can be greatly improved; on the other hand, the material is prepared by adopting a powder metallurgy method and a liquid phase sintering (infiltration) process, and can ensure that silver and tungsten carbide particles form good wetting, thereby avoiding the material from splashing under the action of high-temperature electric arc.
To improve the arc resistance of silver tungsten carbide materials, it is generally desirable to reduce the particle size of tungsten carbide in the material while increasing the content of tungsten carbide. The silver tungsten carbide material used in special equipment such as large-scale smelting furnaces and the like needs to be increased to 60% or even higher by mass percent, and the average particle size of the tungsten carbide is reduced to below 1 micron, which puts very high requirements on the manufacturing process of the material.
When the content of tungsten carbide in the silver tungsten carbide powder is too high and the particle size of tungsten carbide is too small, huge surfaces of tungsten carbide particles exist in the mixed powder, and the situation that a large number of tungsten carbide particles are adjacent to the particles in the powder forming process is inevitable. Due to the ultrahigh hardness, when tungsten carbide particles are in contact with the surfaces of the particles and pressed, plastic deformation hardly occurs, so that mutual engagement between the particles cannot be formed, cracks are easy to occur in a pressed compact, and the pressed compact cannot be molded.
Therefore, it has been a difficult problem in the industry to produce silver tungsten carbide materials with high tungsten carbide content. This problem also considerably limits the further increase of the breaking performance of the electrical appliance.
The conventional coating process can not avoid the agglomeration of tungsten carbide particles in the chemical reaction process, and the silver generated by the reaction can not coat a single tungsten carbide particle but coat the agglomerates of a plurality of tungsten carbide particles, so that a large number of tungsten carbide particles are in direct contact with the particles in the coated powder, and the powder formability is poor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a silver tungsten carbide contact material and a preparation method thereof. The compactness of the silver tungsten carbide contact material can be effectively improved.
The invention is realized by the following technical scheme:
a preparation method of a silver tungsten carbide contact material comprises the following steps:
s1, uniformly mixing a silver nitrate solution, polyethylene glycol, a sodium hydroxide solution and a glucose solution, carrying out reduction reaction under the conditions of ultrasonic oscillation and stirring, and separating out silver and wrapping the silver outside tungsten carbide powder to form silver-wrapped tungsten carbide composite powder; the dosage of the silver nitrate solution is converted from the dosage of silver, and the dosage of the silver is converted
Calculated using the following formula:
wherein
Is the total mass of the tungsten carbide used,
is the density of the silver and is,
is the density of the tungsten carbide,
is the average grain diameter of the tungsten carbide powder,
the unit of (a) is um,
the thickness of the silver layer in the silver-coated tungsten carbide composite powder;
s2, mixing the silver-coated tungsten carbide powder and the silver powder and pressing the mixture into a pressed compact;
and S3, placing the pressed compact and the silver block prepared in the step S2 in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration to obtain the silver tungsten carbide contact material.
Further, in the S1, the thickness of the silver layer in the silver-coated tungsten carbide composite powder is 10-200 nm.
Further, in S1, the method further includes: adding tungsten carbide powder and a silver nitrate solution into a reaction container, adding polyethylene glycol into the reaction container, carrying out ultrasonic oscillation and stirring to uniformly mix the tungsten carbide powder and the silver nitrate solution, keeping the ultrasonic oscillation and the stirring, adding a sodium hydroxide solution into the reaction container until the pH value of the solution reaches 8-9, then continuing the ultrasonic oscillation and the stirring to uniformly mix the solution, keeping the ultrasonic stirring, gradually adding a glucose solution into the reaction container, keeping the adding speed warm to 0.5-2L/min, after silver ions in the solution are completely separated out, continuing the ultrasonic oscillation and the stirring to carry out a reduction reaction, wrapping the separated silver on the tungsten carbide powder to form silver-wrapped tungsten carbide composite powder, carrying out suction filtration on a reactant solution in the reaction container, separating the silver-wrapped tungsten carbide composite powder, cleaning and drying.
Further, the solid-to-liquid ratio of the tungsten carbide powder to the silver nitrate solution is 5-70 g/L.
Further, in the S1, the molecular weight of the polyethylene glycol is 500-20000, and the addition amount is 7-12% of the mass of the tungsten carbide powder. By adding polyethylene glycol as a stabilizer, the polyethylene glycol covers the surfaces of the tungsten carbide particles in the ultrasonic process, so that the potential energy of the surfaces of the particles is increased, and the agglomeration of the tungsten carbide particles is inhibited.
Further, in the S1, the concentration of the glucose solution is 30-300 g/L. The low-concentration glucose solution is used as a reducing agent, so that the excessive precipitation of silver is inhibited, and the thickness of the silver shell layer is effectively controlled by matching with the growth inhibition effect of polyethylene glycol.
Further, in the S1, the average particle size of the tungsten carbide powder is 0.5 to 8 μm.
Further, in the S2, the green compact has a porosity of 5 to 55%.
The invention also provides a silver tungsten carbide contact material with the mass percent of tungsten carbide being 40-90%.
According to the invention, a pure silver shell layer with the thickness of 10-200 nm is covered outside tungsten carbide powder particles to obtain tungsten carbide-silver composite powder with a monodisperse core-shell structure, namely silver-coated tungsten carbide composite powder, and physical isolation is established between the tungsten carbide-tungsten carbide particles by using pure silver. Because silver has very good extensibility, in the process of powder compression molding, adjacent tungsten carbide particles can be meshed with each other through the pure silver shell layer covered on the outer layer to form mechanical combination, thereby greatly improving the molding performance of the powder, ensuring the molding of the silver-tungsten carbide mixed powder with high tungsten carbide content and realizing the manufacture of the high-compactness silver-tungsten carbide material with high tungsten carbide content. By the process, the formation of the single-particle dispersed composite powder is guaranteed, and the powder formability is greatly improved.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is an SEM photograph of the structure of a silver tungsten carbide contact material in example 1 of the present invention;
FIG. 2 is a SEM photograph of the structure obtained in the performance test of a conventional silver tungsten carbide contact material in example 1 of the present invention;
FIG. 3 is a metallographic photograph of a silver tungsten carbide contact material according to example 1 of the present invention;
fig. 4 is a metallographic photograph of a silver tungsten carbide contact material in example 2 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Example 1
A preparation method of a silver tungsten carbide contact material comprises the following steps:
a. dissolving 3.25kg of silver nitrate solid into 2500L of deionized water to prepare a silver nitrate solution;
b. adding 33.2kg of tungsten carbide powder and silver nitrate solution into a reaction container, adding 3kg of polyethylene glycol and a proper amount of deionized water into the container, and carrying out ultrasonic treatment and stirring for 2 hours;
c. keeping ultrasonic and stirring, gradually adding sodium hydroxide solution into the container until the pH value of the solution reaches 8-9, and keeping ultrasonic and stirring for 0.5 hour;
d. maintaining ultrasound and stirring, gradually adding 100g/L glucose solution into the container at a speed of 1.5L/min until silver in the solution is completely precipitated, and maintaining ultrasound and stirring for 0.5 h;
e. carrying out suction filtration on the solution, washing the obtained composite powder twice with deionized water, and drying for later use;
f. putting the composite powder obtained in the step e and silver powder into a V-shaped powder mixer to be mixed for 10-12 hours to obtain AgWC powder containing 5% of silver;
g. pressing the AgWC powder obtained in the step f into a pressed blank by adopting powder forming equipment;
h. and g, placing the pressed compact and the silver block obtained in the step g into an ammonia decomposition atmosphere protection sintering furnace, sintering at 1000 ℃, infiltrating for 2 hours, cooling, discharging, and cleaning to obtain the silver tungsten carbide contact material.
It is understood that step h is prior art, and the setting of sintering temperature and infiltration time is not limited to this example and will not be described herein.
The metallographic photograph of the silver tungsten carbide contact material obtained by the method for preparing the silver tungsten carbide contact material in this example 1 is shown in fig. 3, and the structure SEM photograph is shown in fig. 1. In example 1, a commercially available silver tungsten carbide material was subjected to a performance test, and an SEM photograph of the structure is shown in fig. 2. As can be seen from the comparison between fig. 1 and fig. 2, the silver-tungsten carbide contact material in this example 1 has no micropores in the structure, and the silver and the tungsten carbide are well combined and have high compactness.
Example 2
A preparation method of a silver tungsten carbide contact material comprises the following steps:
a. dissolving 6.5kg of silver nitrate solid into 4000L of deionized water to prepare a silver nitrate solution;
b. 66.79kg of tungsten carbide powder and silver nitrate solution are added into a reaction container, 5kg of polyethylene glycol and a proper amount of deionized water are added into the container, and the mixture is subjected to ultrasonic treatment and stirring for 2 hours;
c. keeping ultrasonic and stirring, gradually adding sodium hydroxide solution into the container until the pH value of the solution reaches 8-9, and keeping ultrasonic and stirring for 0.5 hour;
d. keeping ultrasonic and stirring, gradually adding 100g/L glucose solution into the container at a speed of 3L/min, and keeping ultrasonic and stirring for 0.5 hour after all silver in the solution is separated out;
e. carrying out suction filtration on the solution, washing the obtained composite powder twice with deionized water, and drying for later use;
f. putting the composite powder obtained in the step e and silver powder into a V-shaped powder mixer to be mixed for 10-12 hours to obtain AgWC powder with the silver content of 5%;
g. pressing the AgWC powder obtained in the step f into a pressed blank by adopting powder forming equipment;
h. and g, placing the pressed compact and the silver block obtained in the step g into a sintering furnace protected by ammonia decomposition atmosphere, sintering at 1000 ℃, infiltrating for 2 hours, cooling, and discharging to obtain the silver tungsten carbide contact material.
It is understood that step h is prior art, and the setting of sintering temperature and infiltration time is not limited to this example and will not be described herein.
A metallographic photograph of the silver tungsten carbide contact material obtained by the method for preparing the silver tungsten carbide contact material in this embodiment 2 is shown in fig. 4.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (9)
1. The preparation method of the silver tungsten carbide contact material is characterized by comprising the following steps of:
s1, adding tungsten carbide powder and a silver nitrate solution into a reaction container, adding polyethylene glycol into the reaction container, performing ultrasonic oscillation and stirring to uniformly mix the tungsten carbide powder and the silver nitrate solution, keeping the ultrasonic oscillation and stirring, adding a sodium hydroxide solution into the reaction container until the pH value of the solution reaches 8-9, continuing the ultrasonic oscillation and stirring to uniformly mix the solution, keeping the ultrasonic stirring, gradually adding a glucose solution into the reaction container at a speed of 0.5-2L/min, continuing the ultrasonic oscillation and stirring after silver ions in the solution are completely separated out, performing a reduction reaction, and wrapping the separated silver on the tungsten carbide powder to form silver-wrapped tungsten carbide composite powder; the dosage of the silver nitrate solution is converted from the dosage of silver, and the dosage of the silver is converted
Calculated using the following formula:
wherein
Is the total mass of the tungsten carbide used,
is the density of the silver and is,
is the density of the tungsten carbide,
is the average grain diameter of the tungsten carbide powder,
the unit of (a) is um,
the thickness of the silver layer in the silver-coated tungsten carbide composite powder;
s2, mixing the silver-coated tungsten carbide powder and the silver powder and pressing the mixture into a pressed compact;
and S3, placing the pressed compact and the silver block prepared in the step S2 in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration to obtain the silver tungsten carbide contact material.
2. The method for preparing the silver-tungsten carbide contact material according to claim 1, wherein in S1, the thickness of the silver layer in the silver-coated tungsten carbide composite powder is 10-200 nm.
3. The method for preparing the silver-tungsten carbide contact material according to claim 1, wherein the solid-to-liquid ratio of the tungsten carbide powder to the silver nitrate solution is 5-70 g/L.
4. The method for preparing the silver tungsten carbide contact material according to claim 1, wherein in the S1, the molecular weight of the polyethylene glycol is 500-20000, and the addition amount is 7-12% of the mass of the tungsten carbide powder.
5. The method for preparing the silver tungsten carbide contact material according to claim 1, wherein in the step S1, the concentration of the glucose solution is 30-300 g/L.
6. The method for preparing the silver-tungsten carbide contact material according to claim 1, wherein in the step S1, the average particle size of the tungsten carbide powder is 0.5 to 8 μm.
7. The method for preparing the silver tungsten carbide contact material according to claim 1, wherein in the step S2, the porosity of the compact is 5-55%.
8. A silver tungsten carbide contact material, which is prepared by the preparation method of the silver tungsten carbide contact material according to any one of claims 1 to 7.
9. The silver-tungsten carbide contact material according to claim 8, wherein the tungsten carbide is 40 to 90% by mass.
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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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| CN111618297B (en) * | 2020-04-21 | 2022-06-07 | 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 |
| 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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| JPS5776141A (en) * | 1981-05-14 | 1982-05-13 | Sumitomo Electric Ind Ltd | Electric contact meterial |
| US4689196A (en) * | 1985-06-24 | 1987-08-25 | Gte Products Corporation | Silver-tungsten carbide-graphite electrical contact |
| CN101633986A (en) * | 2008-07-25 | 2010-01-27 | 比亚迪股份有限公司 | Method for preparing silver-tungsten composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1411500A (en) * | 1972-09-12 | 1975-10-29 | Siemens Ag | Preparation of a catalytic 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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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5776141A (en) * | 1981-05-14 | 1982-05-13 | Sumitomo Electric Ind Ltd | Electric contact meterial |
| US4689196A (en) * | 1985-06-24 | 1987-08-25 | Gte Products Corporation | Silver-tungsten carbide-graphite electrical contact |
| CN101633986A (en) * | 2008-07-25 | 2010-01-27 | 比亚迪股份有限公司 | Method for preparing silver-tungsten composite material |
| 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 |
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| DE102020113766A1 (en) | 2020-11-26 |
| CN110064762A (en) | 2019-07-30 |
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