CN110000374A - A kind of preparation process and products thereof of silver molybdenum contact material - Google Patents
A kind of preparation process and products thereof of silver molybdenum contact material Download PDFInfo
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- CN110000374A CN110000374A CN201910297990.2A CN201910297990A CN110000374A CN 110000374 A CN110000374 A CN 110000374A CN 201910297990 A CN201910297990 A CN 201910297990A CN 110000374 A CN110000374 A CN 110000374A
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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 kind of preparation processes and products thereof of silver-colored molybdenum contact material, its technique includes that (1) molybdenum powder and silver nitrate solution are added in reaction vessel, and polyethylene glycol, sodium hydroxide solution and glucose solution are passed through into reaction vessel, reduction reaction is carried out under sonic oscillation and stirring condition, silver is precipitated and to be wrapped in molybdenum powder external, form silver-colored packet molybdenum composite granule, the structure of the silver-colored packet molybdenum composite granule are as follows: molybdenum extra-granular covers the fine silver shell that a layer thickness is 10~200nm；(2) the silver-colored packet molybdenum composite granule and silver powder are mixed, becomes the silver-colored molybdenum powder body of argentiferous 5%, is then pressed into contact green compact of the porosity 5~50%；(3) by the contact green compact, be placed in silver bullion in the sintering furnace of ammonia dissolving atmosphere protection be sintered, infiltration, to obtain the silver-colored molybdenum contact material of predetermined size and ingredient.The present invention has the following advantages and effects: the high compactness infiltration type silver molybdenum material of high molybdenum content can be made and obtain, the mass ratio of usual molybdenum is in 45%-85%.
Description
Technical field
The invention belongs to metal contact Material Field, in particular to a kind of preparation processes of silver-colored molybdenum contact material.
Background technique
It is a kind of preferable contact material of comprehensive performance using silver-colored molybdenum (AgMo) material that infiltration process makes, compared to silver-colored tungsten
Material has certain section silver advantage, and application prospect is than broader.
For the arc resistant ability for promoting silver-colored molybdenum material, it usually needs by the molybdenum particle size reduction in material, while promoting molybdenum
Content.When molybdenum content is excessively high in silver-colored molybdenum powder body, there are huge molybdenum particle surfaces in mixed powder, inevitably powder at
The a large amount of molybdenum particle situation adjacent with particle is encountered during type.And due to its high rigidity, molybdenum particle is contacted with particle surface
It when compression, is hardly plastically deformed, therefore intermeshing can not be formed between particle, cause easily to split in green compact
Line or even green compact can not form.
Therefore, the silver-colored molybdenum material for making high molybdenum content is industry problem all the time.This problem is also in quite big degree
On limit the further promotion of electric appliance interrupting performance.
Summary of the invention
The purpose of the invention is to overcome shortcoming and defect of the existing technology, and provide a kind of silver-colored molybdenum contact material
Preparation process.The technique can make to obtain the high compactness silver molybdenum material of high molybdenum content.
As the first aspect of the invention, the material of technique preparation has high molybdenum content, and technical solution includes
Following steps:
(1) for wrapping up the dosage m of the silver of molybdenum powder particleAgIt is calculated using following formula:
Wherein mMoIt is molybdenum powder gross mass used, ρAgIt is the density of silver, ρMoIt is the density of molybdenum, d is the average grain of molybdenum powder particle
Diameter, unit um, x are the thickness of wrapped up silver layer, unit um；
(2) dosage of the obtained silver of step 1 is converted into silver nitrate dosage, weighs silver nitrate, by silver nitrate go from
Silver nitrate solution is made in dissolution in sub- water, and molybdenum powder body and silver nitrate solution are added in reaction vessel, and leads into reaction vessel
Enter polyethylene glycol, sodium hydroxide solution and glucose solution, reduction reaction is carried out under sonic oscillation and stirring condition, silver is analysed
Out and to be wrapped in molybdenum powder external, forms silver-colored packet molybdenum composite granule, the structure of the silver-colored packet molybdenum composite granule are as follows: molybdenum powder granule
The fine silver shell that outside covering a layer thickness is 10~200nm；
(3) the silver-colored packet molybdenum composite granule and silver powder are mixed, becomes the mixing of the silver-colored packet molybdenum composite granule containing 5wt%
Powder is then pressed into porosity in the green compact for 5~50%；
(4) green compact and silver bullion are placed in sintering, infiltration in the sintering furnace of ammonia dissolving atmosphere protection, obtain high compactness
Molybdenum shared by silver-colored molybdenum contact material of the mass percent 45%~85%.
It includes following steps that further setting, which is the step (2):
(2.1) molybdenum powder body and quantitative silver nitrate solution are added in reaction vessel, then poly- second is added into reaction vessel
Glycol, sonic oscillation and stirring are uniformly mixed it；
(2.2) sonic oscillation and stirring are kept, sodium hydroxide solution is added into reaction vessel until solution reaches pH8-
9, continuing sonic oscillation and stirring is uniformly mixed it；
(2.3) ultrasonic agitation is kept, glucose solution is gradually added into reaction vessel, speed 0.5-2L/min is added,
Until reaction end, continues sonic oscillation and stirring, reduction reaction is carried out, the silver of precipitation, which is wrapped on molybdenum powder body, forms silver-colored packet molybdenum
Composite granule；
(2.4) reaction product solution in reaction vessel is filtered, isolates silver-colored packet molybdenum composite granule, and be cleaned and dried.
Further setting is after molybdenum powder is added, and the solid-to-liquid ratio of molybdenum powder and solution is 10-50g/L in suspension.
It is 500~20000 that further setting, which is the molecular weight of the polyethylene glycol, and additional amount is the quality of molybdenum powder body
5~10%.
Further setting is the concentration of glucose solution be added are as follows: 50-200g/L.Further setting is the flat of molybdenum powder body
Equal partial size is at 0.5~10 μm.
Innovation Mechanism and beneficial effect of the invention is:
For the present invention by a kind of special chemical technology, covering a layer thickness in molybdenum powder body extra-granular is 10~200nm
Fine silver shell, obtain molybdenum-argentum composite powder body of monodisperse core-shell structure, i.e., silver-colored packet molybdenum composite granule.Since silver has very
Good ductility, therefore in powder compression forming process, can be by being covered on the fine silver of outer layer between adjacent molybdenum particle
Shell intermeshing forms mechanical bond so that the processability of powder be substantially improved and has ensured high molybdenum content silver molybdenum mixed powder
The molding of body realizes the production of the high compactness silver molybdenum material of high molybdenum content.
Said effect is reached, and depends on a kind of molybdenum-argentum composite powder body of monodispersed core-shell structural, i.e., must use fine silver
Physical isolation is established between molybdenum-molybdenum particle.Conventional cladding process not can avoid molybdenum particle agglomeration in chemical reaction process, instead
The silver that should be generated will not parcel form molybdenum particle, but the aggregate of several molybdenum particles is wrapped up, therefore in coated powder
There are a large amount of molybdenum particles to contact with the direct of particle, and powder formability is poor.
In chemical technology of the present invention, on the one hand, by addition polyethylene glycol as stabilizer, polyethylene glycol is in ultrasound
It is covered on molybdenum particle surface in the process, increases particle surface potential energy, it is suppressed that molybdenum particle agglomeration.On the other hand, the present invention makes
Use low concentration glucose solution as reducing agent, it is suppressed that silver-colored too fast precipitation, while the growth inhibition of polyethylene glycol being cooperated to make
With effectively controlling the thickness of silver-colored shell.The present invention has ensured the formation of individual particle dispersion composite granule by above-mentioned technique,
Greatly improve powder formability.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with embodiment to the present invention make into
One step it is described in detail.
Embodiment one
1. silver nitrate solid 3.75kg is dissolved in 2000L deionized water, silver nitrate solution is configured；The dosage of the silver nitrate
The dosage of middle silver is determined according to following methods:
For wrapping up the dosage m of the silver of molybdenum powder particleAgIt is calculated using following formula:
Wherein mMoIt is molybdenum powder gross mass used, ρAgIt is the density of silver, ρMoIt is the density of molybdenum, d is the average grain of molybdenum powder particle
Diameter, unit um, x are the thickness of wrapped up silver layer, unit um；The dosage of the obtained silver of the step is converted into nitre
Sour silver dosage weighs silver nitrate.
2. 37.5kg molybdenum powder body and silver nitrate solution are added in reaction vessel, then the poly- second two of 2.25kg is added into container
Pure and mild appropriate amount of deionized water, ultrasound and stirring 2 hours；
3. keeping ultrasound and stirring, sodium hydroxide solution is added into container, until solution ph reaches 8-9, keeps super
Sound and stirring 0.5 hour；
4. keeping ultrasound and stirring, it is gradually added into the glucose solution that concentration is 100g/L into container, speed is added
0.7L/min keeps ultrasound and stirring 0.5 hour until silver is precipitated completely in solution；
5. solution is filtered, obtained silver-colored packet molybdenum composite granule is cleaned twice with deionized water, and drying is stand-by, the silver packet molybdenum
The fine silver shell in the outside of composite granule with a thickness of 10nm；
It is mixed 10~12 hours 6. above-mentioned composite granule is put into the mixed powder machine of V-type with silver powder, obtains argentiferous 10%
AgMo powder；
7. using powder molding equipment, above-mentioned powder is pressed into the green compact of specific pore rate；
8. green compact and silver bullion are placed in ammonia dissolving atmosphere protection sintering furnace, at a temperature of 1200 DEG C, sintering, infiltration 2 are small
When, obtain the AgMo80 contact material of high compactness；
9. coming out of the stove after material is cooling, product of the present invention is obtained after cleaning.
Embodiment two
1. silver nitrate solid 7.5kg is dissolved in 3500L deionized water, silver nitrate solution is configured；The dosage of the silver nitrate
The dosage of middle silver is determined according to following methods:
For wrapping up the dosage m of the silver of molybdenum powder particleAgIt is calculated using following formula:
2. wherein mMoIt is molybdenum powder gross mass used, ρAgIt is the density of silver, ρMoIt is the density of molybdenum, d is being averaged for molybdenum powder particle
Partial size, unit um, x are the thickness of wrapped up silver layer, unit um；The dosage of the obtained silver of the step is converted into
Silver nitrate dosage weighs silver nitrate.75kg molybdenum powder body and silver nitrate solution are added in reaction vessel, then 4kg is added into container
Polyethylene glycol and appropriate amount of deionized water are stirred by ultrasonic 2 hours；
3. keeping ultrasound and stirring, sodium hydroxide solution is added into container, until solution ph reaches 8-9, keeps super
Sound and stirring 0.5 hour；
4. keeping ultrasound and stirring, it is gradually added into the glucose solution that concentration is 150g/L into container, speed 1L/ is added
Min keeps ultrasound and stirring 0.5 hour until silver is precipitated completely in solution；
5. solution is filtered, obtained silver-colored packet molybdenum composite granule is cleaned twice with deionized water, and drying is stand-by；
It is mixed 10~12 hours 6. above-mentioned powder is put into the mixed powder machine of V-type with silver powder, obtains the AgMo powder of silver content 5%
End；
7. using powder molding equipment, above-mentioned powder is pressed into the green compact of specific pore rate；
8. green compact and silver bullion are placed in the sintering furnace of ammonia dissolving atmosphere protection, at a temperature of 1200 DEG C, sintering, infiltration 2
Hour, obtain AgMo75 material；
9. coming out of the stove after material is cooling, product of the present invention is obtained.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.
Claims (8)
1. a kind of preparation process of silver molybdenum contact material, it is characterised in that: include following steps:
(1) for wrapping up the dosage m of the silver of molybdenum powder particleAgIt is calculated using following formula:
Wherein mMoIt is molybdenum powder gross mass used, ρAgIt is the density of silver, ρMoIt is the density of molybdenum, d is the average grain diameter of molybdenum powder particle,
Its unit is um, and x is the thickness of wrapped up silver layer, unit um；
(2) dosage of the obtained silver of step 1 is converted into silver nitrate dosage, silver nitrate is weighed, by silver nitrate in deionized water
Silver nitrate solution is made in middle dissolution, and molybdenum powder body and silver nitrate solution are added in reaction vessel, and is passed through into reaction vessel poly-
Ethylene glycol, sodium hydroxide solution and glucose solution carry out reduction reaction under sonic oscillation and stirring condition, and silver is precipitated simultaneously
It is external to be wrapped in molybdenum powder, forms silver-colored packet molybdenum composite granule, the structure of the silver-colored packet molybdenum composite granule are as follows: molybdenum powder body extra-granular
Cover the fine silver shell that a layer thickness is 10~200nm；
(3) the silver-colored packet molybdenum composite granule is mixed with silver powder, becomes the mixed powder of the silver-colored packet molybdenum composite granule containing 5wt%
Body is then pressed into contact green compact of the porosity 5~50%；
(4) the contact green compact and silver bullion are placed in sintering, infiltration in the sintering furnace of ammonia dissolving atmosphere protection, obtain high compactness
Molybdenum shared by silver-colored molybdenum contact material of the mass percent 45%~85%.
2. a kind of preparation process of silver-colored molybdenum contact material according to claim 1, it is characterised in that: the step (2)
Include following steps:
(2.1) molybdenum powder body and silver nitrate solution are added in reaction vessel, then polyethylene glycol is added into reaction vessel, ultrasound vibration
It swings and stirring is uniformly mixed it；
(2.2) sonic oscillation and stirring are kept, sodium hydroxide solution is added into reaction vessel, until solution ph is in 8-9, it
Afterwards, continuing sonic oscillation and stirring is uniformly mixed it；
(2.3) ultrasonic agitation is kept, glucose solution is gradually added into reaction vessel, speed 0.5-2L/min is added, molten
After silver ion in liquid is precipitated completely, continue sonic oscillation and stirring, carry out reduction reaction, the silver of precipitation is wrapped on molybdenum powder body
Form silver-colored packet molybdenum composite granule；
(2.4) reaction product solution in reaction vessel is filtered, isolates silver-colored packet molybdenum composite granule, and be cleaned and dried.
3. a kind of preparation process of silver-colored molybdenum contact material according to claim 1, it is characterised in that: after molybdenum powder is added, hang
The solid-to-liquid ratio of molybdenum powder and solution is 10-50g/L in turbid.
4. a kind of preparation process of silver-colored molybdenum contact material according to claim 1, it is characterised in that: the polyethylene glycol
Molecular weight be 500~20000, additional amount be molybdenum powder weight 5~10%.
5. a kind of preparation process of silver-colored molybdenum contact material according to claim 1, it is characterised in that: glucose be added is molten
The concentration of liquid are as follows: 50-200g/L.
6. a kind of preparation process of silver-colored molybdenum contact material according to claim 1, it is characterised in that: the average grain of molybdenum powder body
Diameter is at 0.5~10 μm.
7. infiltration type silver molybdenum contact material prepared by a kind of preparation process as described in one of claim 1-6.
8. a kind of preparation process of silver packet molybdenum composite granule, it is characterised in that: molybdenum powder body is reacted appearance with silver nitrate solution addition
In device, and polyethylene glycol, sodium hydroxide solution and glucose solution are passed through into reaction vessel, in sonic oscillation and stirring condition
Lower carry out reduction reaction, silver is precipitated and to be wrapped in molybdenum powder external, forms silver-colored packet molybdenum composite granule, the silver-colored packet molybdenum composite powder
The structure of body are as follows: molybdenum powder body extra-granular covers the fine silver shell that a layer thickness is 10~200nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111048339A (en) * | 2019-12-07 | 2020-04-21 | 福达合金材料股份有限公司 | Method for manufacturing silver-molybdenum electrical contact with continuous oxidation-resistant layer on surface and product thereof |
| CN113073245A (en) * | 2021-03-24 | 2021-07-06 | 湖南大学 | Silver-molybdenum alloy film and preparation method and application thereof |
| CN114182122A (en) * | 2021-11-23 | 2022-03-15 | 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 |
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| 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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2019
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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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111048339A (en) * | 2019-12-07 | 2020-04-21 | 福达合金材料股份有限公司 | Method for manufacturing silver-molybdenum electrical contact with continuous oxidation-resistant layer on surface and product thereof |
| 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 |
| CN113073245A (en) * | 2021-03-24 | 2021-07-06 | 湖南大学 | Silver-molybdenum alloy film and preparation method and application thereof |
| CN114182122A (en) * | 2021-11-23 | 2022-03-15 | 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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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. |