CN110000374B - Preparation process of silver-molybdenum contact material and product thereof - Google Patents
Preparation process of silver-molybdenum contact material and product thereof Download PDFInfo
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- CN110000374B CN110000374B CN201910297990.2A CN201910297990A CN110000374B CN 110000374 B CN110000374 B CN 110000374B CN 201910297990 A CN201910297990 A CN 201910297990A CN 110000374 B CN110000374 B CN 110000374B
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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
- 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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- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a preparation process of a silver-molybdenum contact material and a product thereof, wherein the process comprises the steps of (1) adding molybdenum powder and silver nitrate solution into a reaction vessel, introducing polyethylene glycol, sodium hydroxide solution and glucose solution into the reaction vessel, carrying out reduction reaction under the conditions of ultrasonic oscillation and stirring, separating out silver and wrapping the silver outside the molybdenum powder to form silver-coated molybdenum composite powder, and the structure of the silver-coated molybdenum composite powder is as follows: a pure silver shell layer with the thickness of 10-200 nm is covered outside the molybdenum particles; (2) mixing the silver-coated molybdenum composite powder with silver powder to obtain silver-molybdenum powder containing 5% of silver, and pressing the silver-molybdenum powder into a contact green compact with the porosity of 5-50%; (3) and (3) placing the contact pressed compact and the silver block in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration, thereby obtaining the silver-molybdenum contact material with specified size and components. The invention has the following advantages and effects: the high-density infiltration type silver-molybdenum material with high molybdenum content can be prepared and obtained, and the mass ratio of molybdenum is usually 45-85%.
Description
Technical Field
The invention belongs to the field of metal contact materials, and particularly relates to a preparation process of a silver-molybdenum contact material.
Background
The silver-molybdenum (AgMo) material prepared by the infiltration process is a contact material with better comprehensive performance, has certain silver-saving advantage compared with a silver-tungsten material, and has wider application prospect.
To improve the arc resistance of silver-molybdenum materials, it is generally necessary to reduce the molybdenum particle size in the material while increasing the molybdenum content. When the molybdenum content in the silver-molybdenum powder is too high, huge molybdenum particle surfaces exist in the mixed powder, and the situation that a large number of molybdenum particles are adjacent to the particles in the powder forming process is inevitable. Due to the high hardness, when the molybdenum 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 the pressed compact, and the pressed compact cannot be molded.
Therefore, it has been a difficult problem in the industry to produce silver-molybdenum materials with high molybdenum content. This problem also considerably limits the further increase of the breaking performance of the electrical appliance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation process of a silver-molybdenum contact material. The process can be used for preparing the high-compactness silver-molybdenum material with high molybdenum content.
As a first aspect of the invention, the material prepared by the process has high molybdenum content, and the technical scheme comprises the following steps:
(1) the dosage m of the silver used for wrapping the molybdenum powder particlesAgCalculated using the following formula:
wherein m isMoIs the total mass of the molybdenum powder, rhoAgIs the density of silver, pMoIs the density of molybdenum, d is the average particle diameter of the molybdenum powder particles in um, and x is the silver layer coatedThickness, in 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 molybdenum powder and the silver nitrate solution into a reaction container, introducing polyethylene glycol, a sodium hydroxide solution 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 molybdenum powder to form silver-coated molybdenum composite powder, wherein the structure of the silver-coated molybdenum composite powder is as follows: covering a pure silver shell layer with the thickness of 10-200 nm outside the molybdenum powder particles;
(3) mixing the silver-coated molybdenum composite powder with silver powder to obtain mixed powder containing 5wt% of the silver-coated molybdenum composite powder, and pressing the mixed powder into a pressed blank with the porosity of 5-50%;
(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-molybdenum contact material with high compactness, wherein the mass percent of molybdenum is 45-85%.
The step (2) further comprises the following steps:
(2.1) adding molybdenum powder and a quantitative silver nitrate solution into a reaction vessel, adding polyethylene glycol into the reaction vessel, and carrying out ultrasonic oscillation and stirring to uniformly mix the molybdenum 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 continuing the ultrasonic oscillation and stirring to uniformly mix the solution;
(2.3) keeping ultrasonic stirring, gradually adding a glucose solution into the reaction container at a speed of 0.5-2L/min until the reaction end point, continuing ultrasonic oscillation and stirring for carrying out reduction reaction, and coating the separated silver on the molybdenum powder to form silver-coated molybdenum composite powder;
and (2.4) carrying out suction filtration on the reaction product solution in the reaction vessel, separating out the silver-coated molybdenum composite powder, and cleaning and drying.
Further setting that the solid-to-liquid ratio of the molybdenum powder to the solution in the suspension is 10-50g/L after the molybdenum powder is added.
The molecular weight of the polyethylene glycol is further set to be 500-20000, and the addition amount of the polyethylene glycol is 5-10% of the mass of the molybdenum powder.
Further setting the concentration of the added glucose solution as follows: 50-200 g/L. Further, the average grain diameter of the molybdenum powder is set to be 0.5-10 mu m.
The invention has the advantages that:
according to the invention, a pure silver shell layer with the thickness of 10-200 nm is covered outside molybdenum powder particles through a special chemical process to obtain the molybdenum-silver composite powder with a monodisperse core-shell structure, namely the silver-coated molybdenum composite powder. Because silver has very good extensibility, in the process of pressing and forming the powder, adjacent molybdenum particles can be mutually meshed through the pure silver shell layer covered on the outer layer to form mechanical combination, thereby greatly improving the forming performance of the powder, ensuring the forming of the silver-molybdenum mixed powder with high molybdenum content and realizing the manufacture of the silver-molybdenum material with high molybdenum content and high compactness.
The achievement of the above effect relies on a monodispersed core-shell structured molybdenum-silver composite powder, i.e. pure silver must be used to establish physical separation between molybdenum-molybdenum particles. The conventional coating process can not avoid molybdenum particle agglomeration in the chemical reaction process, and silver generated by the reaction can not coat a single molybdenum particle but coat the agglomerates of a plurality of molybdenum particles, so that a large number of molybdenum 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 surface of the molybdenum particles in the ultrasonic process, so that the potential energy of the surface of the particles is increased, and the agglomeration of the molybdenum 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
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the following examples.
Example one
1. Dissolving 3.75kg of silver nitrate solid into 2000L 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 molybdenum powder particlesAgCalculated using the following formula:
wherein m isMoIs the total mass of the molybdenum powder, rhoAgIs the density of silver, pMoIs the density of molybdenum, d is the average particle size of the molybdenum powder particles, and the unit is um, and x is the thickness of the coated silver layer, and the unit is um; and (4) converting the silver consumption obtained in the step into silver nitrate consumption and weighing the silver nitrate.
2. Adding 37.5kg of molybdenum powder and silver nitrate solution into a reaction container, adding 2.25kg of polyethylene glycol and a proper amount of deionized water into the container, and carrying out ultrasonic treatment and stirring for 2 hours;
3. 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;
4. maintaining ultrasound and stirring, gradually adding 100g/L glucose solution into the container at a speed of 0.7L/min until silver in the solution is completely precipitated, and maintaining ultrasound and stirring for 0.5 h;
5. carrying out suction filtration on the solution, washing the obtained silver-coated molybdenum composite powder twice with deionized water, and drying for later use, wherein the thickness of a pure silver shell layer on the outer side of the silver-coated molybdenum composite powder is 10 nm;
6. putting the composite powder and silver powder into a V-shaped powder mixer to be mixed for 10-12 hours to obtain AgMo powder containing 10% of silver;
7. pressing the powder into a pressed blank with specific porosity by adopting powder forming equipment;
8. 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 AgMo80 contact material with high compactness;
9. the material is discharged after being cooled and cleaned to obtain the product of the invention.
Example two
1. Dissolving 7.5kg of silver nitrate solid into 3500L 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 molybdenum powder particlesAgCalculated using the following formula:
2. wherein m isMoIs the total mass of the molybdenum powder, rhoAgIs the density of silver, pMoIs the density of molybdenum, d is the average particle size of the molybdenum powder particles, and the unit is um, and x is the thickness of the coated silver layer, and the unit is um; and (4) converting the silver consumption obtained in the step into silver nitrate consumption and weighing the silver nitrate. Adding 75kg of molybdenum powder and silver nitrate solution into a reaction container, adding 4kg of polyethylene glycol and a proper amount of deionized water into the container, and ultrasonically stirring for 2 hours;
3. 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;
4. keeping ultrasonic and stirring, gradually adding 150g/L glucose solution into the container at a speed of 1L/min until silver in the solution is completely separated out, and keeping ultrasonic and stirring for 0.5 hour;
5. carrying out suction filtration on the solution, washing the obtained silver-coated molybdenum composite powder twice with deionized water, and drying for later use;
6. putting the powder and silver powder into a V-shaped powder mixer to be mixed for 10-12 hours to obtain AgMo powder with the silver content of 5%;
7. pressing the powder into a pressed blank with specific porosity by adopting powder forming equipment;
8. placing the pressed compact and the silver block in a sintering furnace protected by ammonia decomposition atmosphere, sintering and infiltrating for 2 hours at 1200 ℃ to obtain an AgMo75 material;
9. and (4) discharging the cooled material out of the furnace to obtain the product of the invention.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (7)
1. A preparation process of a silver-molybdenum contact material is characterized by comprising the following steps: the method comprises the following steps:
(1) the dosage m of the silver used for wrapping the molybdenum powder particlesAgCalculated using the following formula:
wherein m isMoIs the total mass of the molybdenum powder, rhoAgIs the density of silver, pMoIs the density of molybdenum, d is the average particle size of the molybdenum powder particles in μm, and x is the thickness of the coated silver layer in μm;
(2) converting the silver amount obtained in the step 1 into silver nitrate amount, weighing silver nitrate, dissolving the silver nitrate in deionized water to prepare a silver nitrate solution, adding molybdenum powder and the silver nitrate solution into a reaction container, introducing polyethylene glycol, a sodium hydroxide solution 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 molybdenum powder to form silver-coated molybdenum composite powder, wherein the structure of the silver-coated molybdenum composite powder is as follows: covering a pure silver shell layer with the thickness of 10-200 nm outside the molybdenum powder particles;
(3) mixing the silver-coated molybdenum composite powder with silver powder to obtain mixed powder containing 5wt% of the silver-coated molybdenum composite powder, and pressing the mixed powder into a contact pressed blank with the porosity of 5-50%;
(4) and (3) placing the contact pressed compact and the silver block in a sintering furnace protected by ammonia decomposition atmosphere for sintering and infiltration to obtain the silver-molybdenum contact material with high compactness, wherein the mass percent of molybdenum is 45-85%.
2. The process for preparing a silver-molybdenum contact material according to claim 1, wherein the process comprises the following steps: the step (2) comprises the following steps:
(2.1) adding molybdenum powder and silver nitrate solution into a reaction vessel, adding polyethylene glycol into the reaction vessel, and carrying out ultrasonic oscillation and stirring to uniformly mix the molybdenum 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 is 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 adding speed of 0.5-2L/min, continuing the ultrasonic oscillation and stirring for reduction reaction, completely separating out silver ions in the solution, and coating the separated silver on the molybdenum powder to form silver-coated molybdenum composite powder;
and (2.4) carrying out suction filtration on the reaction product solution in the reaction vessel, separating out the silver-coated molybdenum composite powder, and cleaning and drying.
3. The process for preparing a silver-molybdenum contact material according to claim 1, wherein the process comprises the following steps: after the molybdenum powder is added, the solid-to-liquid ratio of the molybdenum powder to the solution in the suspension is 10-50 g/L.
4. The process for preparing a silver-molybdenum contact material according to claim 1, wherein the process comprises the following steps: the molecular weight of the polyethylene glycol is 500-20000, and the addition amount of the polyethylene glycol is 5-10% of the mass of the molybdenum powder.
5. The process for preparing a silver-molybdenum contact material according to claim 1, wherein the process comprises the following steps: the concentration of the added glucose solution was: 50-200 g/L.
6. The process for preparing a silver-molybdenum contact material according to claim 1, wherein the process comprises the following steps: the average particle size of the molybdenum powder is 0.5-10 μm.
7. An infiltration type silver molybdenum contact material prepared by the preparation process as claimed in any one of claims 1 to 6.
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| CN111048339B (en) * | 2019-12-07 | 2022-03-18 | 浙江福达合金材料科技有限公司 | Method for manufacturing silver-molybdenum electrical contact with continuous oxidation-resistant layer on surface and product thereof |
| CN113073245B (en) * | 2021-03-24 | 2022-10-14 | 湖南大学 | Silver-molybdenum alloy film and preparation method and application thereof |
| CN114182122B (en) * | 2021-11-23 | 2022-06-28 | 浙江福达合金材料科技有限公司 | High-dispersity silver-molybdenum electrical contact material and preparation method thereof |
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|---|---|---|---|---|
| JPH0428805A (en) * | 1990-02-13 | 1992-01-31 | Daido Steel Co Ltd | Method for alloying powder |
| CN201638761U (en) * | 2010-02-24 | 2010-11-17 | 江苏江南电机有限公司 | Contact adhesion prevention type electromagnetic switch |
| CN104377046A (en) * | 2013-08-16 | 2015-02-25 | 通用电气公司 | A system comprising a contact tip |
| CN107737949A (en) * | 2017-10-23 | 2018-02-27 | 重庆云天化瀚恩新材料开发有限公司 | A kind of silver-coated copper powder and preparation method thereof |
-
2019
- 2019-04-15 CN CN201910297990.2A patent/CN110000374B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0428805A (en) * | 1990-02-13 | 1992-01-31 | Daido Steel Co Ltd | Method for alloying powder |
| CN201638761U (en) * | 2010-02-24 | 2010-11-17 | 江苏江南电机有限公司 | Contact adhesion prevention type electromagnetic switch |
| CN104377046A (en) * | 2013-08-16 | 2015-02-25 | 通用电气公司 | A system comprising a contact tip |
| CN107737949A (en) * | 2017-10-23 | 2018-02-27 | 重庆云天化瀚恩新材料开发有限公司 | A kind of silver-coated copper powder and preparation method thereof |
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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. |