CN110129603B - Method for manufacturing silver-tungsten contact material and product thereof - Google Patents
Method for manufacturing silver-tungsten contact material and product thereof Download PDFInfo
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- CN110129603B CN110129603B CN201910297951.2A CN201910297951A CN110129603B CN 110129603 B CN110129603 B CN 110129603B CN 201910297951 A CN201910297951 A CN 201910297951A CN 110129603 B CN110129603 B CN 110129603B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a method for manufacturing a silver-tungsten contact material and a product thereof, wherein the method comprises the following steps: (1) adding tungsten powder and a silver nitrate solution into a reaction container, adding polyethylene glycol, sodium hydroxide and a glucose solution into the reaction container, carrying out reduction reaction under the conditions of ultrasonic oscillation and stirring, and separating out silver and wrapping the silver outside the tungsten powder to form composite powder, wherein the composite powder has the structure that: covering a pure silver shell layer with the thickness of 10-200 nm outside the tungsten particles; (2) mixing the composite powder with silver powder to obtain silver-tungsten powder containing 4% of silver, and pressing the silver-tungsten powder into a contact green compact with porosity of 5-45%; (3) and placing the contact pressed compact and the silver block in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration so as to obtain the silver-tungsten contact material with specified size and components. The invention has the following advantages and effects: the high-compactness infiltration type silver-tungsten material with high tungsten content can be manufactured and obtained, and the mass ratio of tungsten is 50-90 percent usually.
Description
Technical Field
The invention relates to the field of contact materials of low-voltage distribution equipment, in particular to a manufacturing method of a silver-tungsten contact material and a product 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 most commonly used material in the low-voltage circuit breaker is an infiltration silver-tungsten (AgW) material. On one hand, the material contains micron-sized dispersed tungsten 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 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 materials, it is generally necessary to reduce the tungsten particle size in the material and increase the tungsten content. When the tungsten content in the silver-tungsten powder is too high and the tungsten particle size is too small, huge tungsten particle surfaces exist in the mixed powder, and the situation that a large number of tungsten particles are adjacent to the particles in the powder forming process is inevitable. Due to the ultrahigh hardness, when tungsten 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 fabricate silver tungsten material with high tungsten content. This problem also considerably limits the further increase of the breaking performance of the electrical appliance.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for producing a silver-tungsten contact material and a product thereof, which can produce and obtain a highly dense silver-tungsten material having a high tungsten content.
In order to achieve the purpose, the invention provides a method for manufacturing a silver-tungsten contact material, which comprises the following steps:
(1) the dosage m of the silver used for wrapping the tungsten powder particlesAgCalculated using the following formula:
wherein m isWIs the total mass of the tungsten powder, rhoAgIs the density of silver, pWIs the density of tungsten, d is the average particle size of the tungsten powder particles, and the unit is um, and x is the thickness of the coated silver layer, and the unit is um;
(2) converting the silver consumption obtained in the step 1 into silver nitrate consumption, weighing the silver nitrate, dissolving the silver nitrate in deionized water to prepare a silver nitrate solution, adding tungsten powder and the silver nitrate solution into a reaction container, adding polyethylene glycol, sodium hydroxide and a glucose solution into the reaction container, performing reduction reaction under the conditions of ultrasonic oscillation and stirring, separating out silver, and wrapping the silver outside the tungsten powder to form silver-coated tungsten composite powder, wherein the structure of the silver-coated tungsten composite powder is as follows: covering a pure silver shell layer with the thickness of 10-200 nm outside the tungsten powder particles;
(3) mixing the silver-coated tungsten composite powder with silver powder to obtain mixed powder containing 4 wt% of the silver-coated tungsten composite powder, and pressing the mixed powder into a pressed blank with the porosity of 5-45%;
(4) and (3) placing the pressed compact and the silver block in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration to obtain the silver-tungsten contact material with high compactness and tungsten content of 50-90% by mass.
Further, the step (2) comprises the following steps:
(2.1) adding tungsten powder, a certain amount of silver nitrate solution and a proper amount of deionized water into a reaction vessel, adding polyethylene glycol into the reaction vessel, and performing ultrasonic oscillation and stirring to uniformly mix the tungsten powder, the silver nitrate solution and the deionized water;
(2.2) keeping ultrasonic oscillation and stirring, adding a sodium hydroxide solution into the reaction vessel until the pH value of the solution reaches 8-9, and then continuing ultrasonic oscillation and stirring to uniformly mix the solution;
(2.3) keeping ultrasonic oscillation and stirring, gradually adding a glucose solution into the reaction container at the speed of 0.5-2L/min until the reaction is finished, continuing the ultrasonic oscillation and stirring to perform reduction reaction, and wrapping the precipitated silver in tungsten powder to form composite powder;
(2.4) carrying out suction filtration on the reaction product solution in the reaction container, washing the obtained composite powder twice with deionized water, and drying for later use;
further, after the tungsten powder is added, the solid-to-liquid ratio of the tungsten powder to the solution in the suspension is 2-70 g/L. .
Furthermore, the molecular weight of the polyethylene glycol is 500-20000, and the addition amount of the polyethylene glycol is 3-8% of the mass of the tungsten powder.
Further, the concentration of the added glucose solution is as follows: 40-300 g/L.
Furthermore, the average particle size of the tungsten powder is 1-10 um.
Compared with the prior art, the manufacturing method of the silver-tungsten contact material and the product thereof provided by the invention have the following beneficial effects:
according to the invention, a pure silver shell layer with the thickness of 10-200 nm is covered outside tungsten powder particles through a special chemical process, so that the tungsten-silver composite powder body with a monodisperse core-shell structure is obtained. Because silver has very good extensibility, in the process of powder compression molding, adjacent tungsten particles can be mutually meshed 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 high-tungsten content silver-tungsten mixed powder and realizing the manufacture of the high-tungsten content high-compactness silver-tungsten material.
The achievement of the above effect relies on a tungsten-silver composite powder body of a monodispersed core-shell structure, i.e. pure silver must be used to establish physical separation between tungsten-tungsten particles. The conventional coating process cannot avoid tungsten particle agglomeration in the chemical reaction process, and silver generated by the reaction cannot wrap a single tungsten particle but wraps the agglomerates of a plurality of tungsten particles, so that a large number of tungsten particles are in direct contact with the particles in the coated powder, and the powder formability is poor.
In the chemical process, on one hand, polyethylene glycol is added as a stabilizer, and the polyethylene glycol covers the surfaces of tungsten particles in the ultrasonic process, so that the potential energy of the surfaces of the particles is increased, and the agglomeration of the tungsten particles is inhibited. On the other hand, the invention uses low-concentration glucose solution as a reducing agent, inhibits the excessive precipitation of silver, and effectively controls the thickness of the silver shell layer by matching with the growth inhibition effect of polyethylene glycol. By the process, the formation of the single-particle dispersed composite powder is guaranteed, and the powder formability is greatly improved.
Detailed Description
Example 1
The invention provides a method for manufacturing a silver-tungsten contact material, which is embodiment 1 and comprises the following steps:
step 101: dissolving 1.25kg of silver nitrate solid into 3000L of deionized water to prepare a silver nitrate solution; the amount of silver in the silver nitrate is determined according to the following method:
the dosage m of the silver used for wrapping the tungsten powder particlesAgCalculated using the following formula:
wherein m isWIs the total mass of the tungsten powder, rhoAgIs the density of silver, pWIs the density of tungsten, d is the average particle size of the tungsten powder particles, and the unit is um, and x is the thickness of the coated silver layer, and the unit is um; the silver amount obtained in this step is converted into silver nitrate amount and is called silver nitrate.
Step 102: adding 37.5kg of tungsten powder and silver nitrate solution into a reaction container, adding 3.25kg of polyethylene glycol and a proper amount of deionized water into the container, and carrying out ultrasonic treatment and stirring for 2 hours;
step 103: keeping ultrasonic and stirring, adding sodium hydroxide solution into the container until the pH value of the solution reaches 8-9, and then keeping ultrasonic and stirring for 0.5 hour;
step 104: maintaining ultrasound and stirring, gradually adding 120g/L glucose solution into the container at a speed of 1.5L/min, and maintaining ultrasound and stirring for 0.5 hr after all silver in the solution is precipitated;
step 105: carrying out suction filtration on the solution, washing the obtained composite powder twice with deionized water, and drying for later use;
step 106: putting the composite powder and silver powder into a V-shaped powder mixer to be mixed for 10-12 hours to obtain AgW powder with the silver content of 4%;
step 107: pressing the powder into a pressed blank with specific porosity by adopting powder forming equipment;
step 108: placing the pressed compact and the silver block in an ammonia decomposition atmosphere protection sintering furnace, sintering and infiltrating for 2 hours at the temperature of 1200 ℃ to obtain the AgW85 contact material with high compactness;
step 109: the material is discharged after being cooled and cleaned to obtain the product of the invention.
Example 2
The invention provides a method for manufacturing a silver-tungsten contact material, which is embodiment 2 and comprises the following steps:
step 201: dissolving 2.5kg of silver nitrate solid into 6000L of deionized water to prepare a silver nitrate solution; the amount of silver in the silver nitrate is determined according to the following method:
the dosage m of the silver used for wrapping the tungsten powder particlesAgCalculated using the following formula:
wherein m isWIs the total mass of the tungsten powder, rhoAgIs the density of silver, pWIs the density of tungsten, d is the average particle size of the tungsten powder particles, and the unit is um, and x is the thickness of the coated silver layer, and the unit is um; converting the amount of silver obtained in this stepThe dosage of the silver nitrate is obtained and is called as the silver nitrate. Step 202: adding 75kg of tungsten powder and silver nitrate solution into a reaction container, adding 6.5kg of polyethylene glycol and a proper amount of deionized water into the container, and carrying out ultrasonic treatment and stirring for 2 hours;
step 205: keeping ultrasonic and stirring, 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;
step 206: maintaining ultrasound and stirring, gradually adding 120g/L glucose solution into the container at a speed of 1.5L/min, and maintaining ultrasound and stirring for 0.5 hr after silver in the solution is completely precipitated;
step 207: carrying out suction filtration on the solution, washing the obtained composite powder twice with deionized water, and drying for later use;
step 208: putting the composite powder and silver powder into a V-shaped powder mixer to be mixed for 10-12 hours to obtain AgW powder with the silver content of 4%;
step 209: pressing the powder into a pressed blank with specific porosity by adopting powder forming equipment;
step 210: placing the pressed compact and the silver block in an ammonia atmosphere decomposition protection sintering furnace, and sintering-infiltrating for 2 hours at the temperature of 1200 ℃ to obtain the AgW90 material with high compactness;
step 211: and (4) discharging the cooled material out of the furnace to obtain the product of the invention.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (7)
1. The manufacturing method of the silver-tungsten contact material is characterized by comprising the following steps of:
(1) the dosage m of the silver used for wrapping the tungsten powder particlesAgCalculated using the following formula:
wherein m isWIs the total mass of the tungsten powder, rhoAgIs the density of silver, pWIs the density of tungsten, d is the average particle size of the tungsten powder particles in μm, and x is the thickness of the silver layer coated in μm;
(2) converting the silver consumption obtained in the step 1 into silver nitrate consumption; weighing silver nitrate, dissolving the silver nitrate in deionized water to prepare a silver nitrate solution, adding tungsten powder and the silver nitrate solution into a reaction container, adding polyethylene glycol, sodium hydroxide and a glucose solution into the reaction container, carrying out reduction reaction under the conditions of ultrasonic oscillation and stirring, separating out silver, and wrapping the silver outside the tungsten powder to form silver-coated tungsten composite powder, wherein the structure of the silver-coated tungsten composite powder is as follows: covering a pure silver shell layer with the thickness of 10-200 nm outside the tungsten powder particles;
(3) mixing the silver-coated tungsten composite powder with silver powder to obtain mixed powder containing 4 wt% of silver-coated tungsten composite powder, and pressing the mixed powder into a pressed blank with the porosity of 5-45%;
(4) and placing the pressed compact and the silver block in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration to obtain the silver-tungsten contact material with high compactness and tungsten content of 50-90% by mass.
2. The method for manufacturing the silver-tungsten contact material according to claim 1, wherein the method comprises the following steps: the step (2) comprises the following steps:
(2.1) adding tungsten powder and silver nitrate solution into a reaction container, adding polyethylene glycol into the reaction container, and performing ultrasonic oscillation and stirring to uniformly mix the tungsten powder and the silver nitrate solution;
(2.2) keeping ultrasonic oscillation and stirring, adding a sodium hydroxide solution into the reaction vessel until the pH value of the solution reaches 8-9, and then continuing ultrasonic oscillation and stirring to uniformly mix the solution;
(2.3) keeping ultrasonic oscillation and stirring, gradually adding a glucose solution into the reaction container at a speed of 0.5-2L/min, continuously carrying out ultrasonic oscillation and stirring after silver ions in the solution are completely separated out to carry out reduction reaction, and wrapping the separated silver in tungsten powder to form composite powder;
and (2.4) carrying out suction filtration on the reaction product solution in the reaction vessel, washing the obtained composite powder twice with deionized water, and drying.
3. The method for manufacturing the silver-tungsten contact material according to claim 1, wherein the method comprises the following steps: after the tungsten powder is added, the solid-to-liquid ratio of the tungsten powder to the solution in the suspension is 2-70 g/L.
4. The method for manufacturing the silver-tungsten contact material according to claim 1, wherein the method comprises the following steps: the molecular weight of the polyethylene glycol is 500-20000, and the addition amount of the polyethylene glycol is 3-8% of the mass of the tungsten powder.
5. The method for manufacturing the silver-tungsten contact material according to claim 1, wherein the method comprises the following steps: the concentration of the added glucose solution was: 40-300 g/L.
6. The method for manufacturing the silver-tungsten contact material according to claim 1, wherein the method comprises the following steps: the average particle size of the tungsten powder is 1-10 mu m.
7. A silver-tungsten contact material produced by the production method according to any one of claims 1 to 6.
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| CN110129603B true CN110129603B (en) | 2021-03-30 |
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| CN114192774B (en) * | 2021-11-23 | 2023-05-09 | 浙江福达合金材料科技有限公司 | Silver-tungsten electrical contact material with high dispersity and high compactness and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11269579A (en) * | 1998-03-24 | 1999-10-05 | Nippon Kagaku Yakin Co Ltd | Silver-tungsten/wc base sintered type electric contact material and its production |
| CN1651590A (en) * | 2005-02-03 | 2005-08-10 | 西安建筑科技大学 | Preparation technology of tungsten copper or tungsten silver composite material |
| CN101633986A (en) * | 2008-07-25 | 2010-01-27 | 比亚迪股份有限公司 | Method for preparing silver-tungsten composite material |
| CN102392170A (en) * | 2011-11-11 | 2012-03-28 | 扬州乐银合金科技有限公司 | Processing method for manufacturing silver tungsten composite 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 |
| CN105798319A (en) * | 2014-12-31 | 2016-07-27 | 施耐德电气工业公司 | Preparation method and device for silver-tungsten electrical contact material as well as electrical contact material and electrical contact |
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2019
- 2019-04-15 CN CN201910297951.2A patent/CN110129603B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11269579A (en) * | 1998-03-24 | 1999-10-05 | Nippon Kagaku Yakin Co Ltd | Silver-tungsten/wc base sintered type electric contact material and its production |
| CN1651590A (en) * | 2005-02-03 | 2005-08-10 | 西安建筑科技大学 | Preparation technology of tungsten copper or tungsten silver composite material |
| CN101633986A (en) * | 2008-07-25 | 2010-01-27 | 比亚迪股份有限公司 | Method for preparing silver-tungsten composite material |
| CN102392170A (en) * | 2011-11-11 | 2012-03-28 | 扬州乐银合金科技有限公司 | Processing method for manufacturing silver tungsten composite 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 |
| CN105798319A (en) * | 2014-12-31 | 2016-07-27 | 施耐德电气工业公司 | Preparation method and device for silver-tungsten electrical contact material as well as electrical contact material and electrical contact |
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Effective date of registration: 20220913 Address after: 325025 No. 308, Binhai fifth road, Wenzhou Economic and Technological Development Zone, Wenzhou City, Zhejiang Province Patentee after: Zhejiang Fuda alloy material technology Co.,Ltd. Address before: No. 518, Binhai 4th Road, Binhai Park, Wenzhou Economic and Technological Development Zone, Zhejiang Province, 325000 Patentee before: FUDA ALLOY MATERIALS Co.,Ltd. |