CN110129603A - A kind of production method and products thereof of silver tungsten contact material - Google Patents
A kind of production method and products thereof of silver tungsten contact material Download PDFInfo
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- CN110129603A CN110129603A CN201910297951.2A CN201910297951A CN110129603A CN 110129603 A CN110129603 A CN 110129603A CN 201910297951 A CN201910297951 A CN 201910297951A CN 110129603 A CN110129603 A CN 110129603A
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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 kind of production methods and products thereof of silver tungsten contact material, the following steps are included: (1) tungsten powder and silver nitrate solution are added in reaction vessel, and polyethylene glycol, sodium hydroxide and glucose solution are added into reaction vessel, after carrying out reduction reaction under sonic oscillation and stirring condition, silver is precipitated and to be wrapped in tungsten powder external, form composite granule, the structure of the composite granule are as follows: the fine silver shell that covering a layer thickness is 10~200nm outside tungsten particle；(2) composite granule is mixed with silver powder, becomes the silver-colored tungsten powder body of argentiferous 4%, be then pressed into contact green compact of the porosity 5~45%；(3) the contact green compact and silver bullion are placed in the sintering furnace of ammonia dissolving atmosphere protection be sintered, infiltration, to obtain the silver tungsten contact material of predetermined size and ingredient.The present invention has the following advantages and effects: the high compactness infiltration type silver tungsten material of high W content can be made and obtain, usual tungsten mass ratio is in 50%-90%.
Description
Technical field
The present invention relates to the contact material field of low-voltage distribution apparatus, in particular to a kind of production side of silver tungsten contact material
Method and products thereof.
Background technique
Requirement with power grid distribution end to electrical reliability is higher and higher, and appliance manufacturers just constantly release more high breaking
The LV power distribution product of index.Part electronics plastic casing breaker can reach capacity the index of disjunction 150kA.Electric appliance disjunction
The promotion of index means that the thermal break-through power of electric arc when disjunction is extremely powerful, and contact material causes easily by arc erosion at this time
Electric appliance is not turned on, and is broken down.
Comprehensively consider materials conductive, anticorrosive etc. performance, most commonly used material is molten in low-voltage circuit breaker
Seep class silver tungsten (AgW) material.On the one hand, contain in such material micron order dispersion tungsten particle as reinforced phase, can be very big
Promotion material arc ablation resistance ability；On the other hand, such material uses powder metallurgic method, liquid-phase sintering (infiltration) technique system
Make, can ensure that silver forms good wet with tungsten particle, so that material be avoided to splash under high-temperature electric arc effect.
For the arc resistant ability for promoting silver-colored tungsten material, it usually needs by the tungsten particle size reduction in material, while promoting tungsten
Content.When W content is excessively high in silver-colored tungsten powder body, while tungsten particle spends hour, there are huge tungsten particle surface in mixed powder,
The a large amount of tungsten particle situation adjacent with particle is inevitably encountered in powder forming process.And due to its ultrahigh hardness,
When tungsten particle contacts compression with particle surface, hardly it is plastically deformed, therefore intermeshing can not be formed between particle, leads
Cause easily cracked or even green compact in green compact that can not form.
Therefore, the silver-colored tungsten material for making high W 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
In view of the foregoing, it is an object to provide a kind of production method and products thereof of silver tungsten contact material, energy
Enough makes and obtain the high compactness silver tungsten material of high W content.
In order to achieve the above object, the present invention provides a kind of production methods of silver tungsten contact material, comprising the following steps:
(1) for wrapping up the dosage m of the silver of tungsten powder particlesAgIt is calculated using following formula:
Wherein mWIt is tungsten powder gross mass used, ρAgIt is the density of silver, ρWIt is the density of tungsten, d is the average grain of tungsten powder particles
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 tungsten powder body and silver nitrate solution are added in reaction vessel, and adds into reaction vessel
Enter polyethylene glycol, sodium hydroxide and glucose solution, after carrying out reduction reaction under sonic oscillation and stirring condition, silver is precipitated
And it is external to be wrapped in tungsten powder, forms silver-colored packet tungsten composite powder, the structure of the silver-colored packet tungsten composite powder are as follows: outside tungsten powder granule
Portion covers the fine silver shell that a layer thickness is 10~200nm；
(3) the silver-colored packet tungsten composite powder is mixed with silver powder, becomes the mixing of the silver-colored packet tungsten composite powder containing 4wt%
Powder is then pressed into the green compact that porosity is 5~45%；
(4) green compact and silver bullion are placed in the sintering furnace of ammonia dissolving atmosphere protection be sintered, infiltration, obtain high
Silver tungsten contact material of the tungsten institute's mass percent of compactness 50%~90%.
Further, include following steps in the step (2):
(2.1) tungsten powder and quantitative silver nitrate solution and appropriate amount of deionized water are added in reaction vessel, then Xiang Fanying holds
Polyethylene glycol is added in device, 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 later is uniformly mixed it；
(2.3) sonic oscillation and stirring are kept, glucose solution is gradually added into reaction vessel, speed 0.5- is added
2L/min, until reaction end, continuing sonic oscillation and stirring makes it carry out reduction reaction, and the silver of precipitation is wrapped in the tungsten powder bodily form
At composite granule；
(2.4) reaction product solution in reaction vessel being filtered, obtained composite granule is cleaned twice with deionized water,
Drying is stand-by；
Further, after tungsten powder is added, the solid-to-liquid ratio of tungsten powder and solution is 2-70g/L in suspension.
Further, the molecular weight of the polyethylene glycol be 500~20000, additional amount be tungsten powder weight 3~
8%.
Further, the glucose concentration being added are as follows: 40-300g/L.
Further, the average grain diameter of the tungsten powder body is in 1~10um.
Compared to the prior art, the production method and products thereof of a kind of silver tungsten contact material provided by the invention, have with
It is lower the utility model has the advantages that
For the present invention by a kind of special chemical technology, it is 10~200nm's that a layer thickness is covered outside tungsten powder particles
Fine silver shell obtains tungsten-argentum composite powder body of monodisperse core-shell structure.Since silver has very good ductility,
In powder compression forming process, it can be intermeshed by being covered on the fine silver shell of outer layer between adjacent tungsten particle, form machine
Tool combines, so that the processability of powder be substantially improved, has ensured the molding of high W content silver tungsten mixed powder, has realized high tungsten
The production of the high compactness silver tungsten material of content.
Said effect is reached, and depends on a kind of tungsten-argentum composite powder body of monodispersed core-shell structural, i.e., must use fine silver
Physical isolation is established between tungsten-tungsten particle.Conventional cladding process not can avoid tungsten particle reunion in chemical reaction process, instead
The silver that should be generated will not parcel form tungsten particle, but the aggregate of several tungsten particles is wrapped up, therefore in coated powder
There are a large amount of tungsten 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 tungsten particle surface in the process, increases particle surface potential energy, it is suppressed that tungsten particle is reunited.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
Embodiment 1
The present invention provides a kind of production method of silver tungsten contact material, is embodiment 1 comprising following steps:
Step 101: silver nitrate solid 1.25kg being dissolved in 3000L deionized water, silver nitrate solution is configured；The silver nitrate
Dosage in silver-colored dosage determined according to following methods:
For wrapping up the dosage m of the silver of tungsten powder particlesAgIt is calculated using following formula:
Wherein mWIt is tungsten powder gross mass used, ρAgIt is the density of silver, ρWIt is the density of tungsten, d is the average grain of tungsten powder particles
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 simultaneously weighs silver nitrate.
Step 102: 37.5kg tungsten powder and silver nitrate solution being added in reaction vessel, then 3.25kg is added into container and gathers
Ethylene glycol and appropriate amount of deionized water, ultrasound and stirring 2 hours；
Step 103: ultrasound and stirring are kept, sodium hydroxide solution is added into container, until solution ph reaches 8-9,
Ultrasound and stirring 0.5 hour are kept later；
Step 104: keeping ultrasound and stirring, the glucose solution that concentration is 120g/L is gradually added into container, is added
Speed 1.5L/min keeps ultrasound and stirring 0.5 hour after silver is all precipitated in solution；
Step 105: solution being filtered, obtained composite granule is cleaned twice with deionized water, and drying is stand-by；
Step 106: above-mentioned composite granule being put into the mixed powder machine of V-type with silver powder and is mixed 10~12 hours, silver content is obtained
4% AgW powder；
Step 107: using powder molding equipment, above-mentioned powder will be pressed into the green compact of specific pore rate；
Step 108: green compact and silver bullion being placed in ammonia dissolving atmosphere protection sintering furnace, at a temperature of 1200 DEG C, sintering-is molten
It seeps 2 hours, obtains the AgW85 contact material of high compactness；
Step 109: coming out of the stove after material is cooling, product of the present invention is obtained after cleaning.
Embodiment 2
The present invention provides a kind of production method of silver tungsten contact material, is embodiment 2 comprising following steps:
Step 201: silver nitrate solid 2.5kg being dissolved in 6000L deionized water, silver nitrate solution is configured；The silver nitrate
Dosage in silver-colored dosage determined according to following methods:
For wrapping up the dosage m of the silver of tungsten powder particlesAgIt is calculated using following formula:
Wherein mWIt is tungsten powder gross mass used, ρAgIt is the density of silver, ρWIt is the density of tungsten, d is the average grain of tungsten powder particles
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 simultaneously weighs silver nitrate.Step 202: 75kg tungsten powder and silver nitrate solution being added in reaction vessel, then into container
6.5kg polyethylene glycol and appropriate amount of deionized water, ultrasound and stirring 2 hours is added；
Step 205: keep ultrasound and stirring, sodium hydroxide solution is added into container, until solution ph reach 8-9 it
Afterwards, ultrasound and stirring 0.5 hour are kept；
Step 206: keeping ultrasound and stirring, the glucose solution that concentration is 120g/L is gradually added into container, is added
Speed 1.5L/min keeps ultrasound and stirring 0.5 hour after silver is precipitated completely in solution；
Step 207: solution being filtered, obtained composite granule is cleaned twice with deionized water, and drying is stand-by；
Step 208: above-mentioned composite granule being put into the mixed powder machine of V-type with silver powder and is mixed 10~12 hours, silver content is obtained
4% AgW powder；
Step 209: using powder molding equipment, above-mentioned powder is pressed into the green compact of specific pore rate；
Step 210: green compact and silver bullion being placed in ammonia atmosphere decomposing protection sintering furnace, at a temperature of 1200 DEG C, sintering-is molten
It seeps 2 hours, obtains the AgW90 material of high compactness；
Step 211: coming out of the stove after material is cooling, obtain product of the present invention.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (8)
1. a kind of production method of silver tungsten contact material, which comprises the following steps:
(1) for wrapping up the dosage m of the silver of tungsten powder particlesAgIt is calculated using following formula:
Wherein mWIt is tungsten powder gross mass used, ρAgIt is the density of silver, ρWIt is the density of tungsten, d is the average grain diameter of tungsten powder particles,
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 tungsten powder body and silver nitrate solution are added in reaction vessel, and is added and gathers into reaction vessel
Silver after carrying out reduction reaction under sonic oscillation and stirring condition, is precipitated and is wrapped by ethylene glycol, sodium hydroxide and glucose solution
It is external to be wrapped in tungsten powder, shape 7 is at silver-colored packet tungsten composite powder, the structure of the silver-colored packet tungsten composite powder are as follows: tungsten powder body extra-granular
Cover the fine silver shell that a layer thickness is 10~200nm；
(3) the silver-colored packet tungsten composite powder is mixed with silver powder, becomes the mixed powder of the silver-colored packet tungsten composite powder containing 4wt%
Body is then pressed into green compact of the porosity 5~45%；
(4) by the green compact and silver bullion, it is placed in sintering, infiltration in the sintering furnace of ammonia dissolving atmosphere protection, obtains high compactness
Silver tungsten contact material of the tungsten institute's mass percent 50%~90%.
2. a kind of production method of silver tungsten contact material according to claim 1, it is characterised in that: the step (2)
In include following steps:
(2.1) tungsten 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 reaches 8-9,
Continuing sonic oscillation and stirring later is uniformly mixed it；
(2.3) sonic oscillation and stirring are kept, glucose solution is gradually added into reaction vessel, speed 0.5-2L/ is added
Min, after silver ion is precipitated completely in the solution, continuing sonic oscillation and stirring makes it carry out reduction reaction, the silver package of precipitation
Composite granule is formed in tungsten powder body；
(2.4) reaction product solution in reaction vessel is filtered, obtained composite granule is cleaned twice with deionized water, is dried
It is dry；
3. a kind of production method of silver tungsten contact material according to claim 1, it is characterised in that: after tungsten powder is added, hang
The solid-to-liquid ratio of tungsten powder and solution is 2-70g/L in turbid.
4. a kind of production method of silver tungsten contact material according to claim 1, it is characterised in that: the polyethylene glycol
Molecular weight be 500~20000, additional amount be tungsten powder weight 3~8%.
5. a kind of production method of silver tungsten contact material according to claim 1, it is characterised in that: the glucose being added
Solution concentration are as follows: 40-300g/L.
6. a kind of production method of silver tungsten contact material according to claim 1, it is characterised in that: the tungsten powder body
Average grain diameter is in 1~10um.
7. silver tungsten contact material made from a kind of production method as described in one of claim 1-6.
8. a kind of silver packet tungsten composite powder, which is characterized in that tungsten powder body and silver nitrate solution are added in reaction vessel, and to anti-
It answers and polyethylene glycol, sodium hydroxide and glucose solution is added in container, reduction reaction is carried out under sonic oscillation and stirring condition
Afterwards, silver is precipitated and to be wrapped in tungsten powder external, form composite granule, the structure of the composite granule are as follows: outside tungsten powder granule
Portion covers the fine silver shell that a layer thickness is 10~200nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910297951.2A CN110129603B (en) | 2019-04-15 | 2019-04-15 | Method for manufacturing silver-tungsten contact material and product thereof |
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| CN201910297951.2A CN110129603B (en) | 2019-04-15 | 2019-04-15 | Method for manufacturing silver-tungsten contact material and product thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192774A (en) * | 2021-11-23 | 2022-03-18 | 浙江福达合金材料科技有限公司 | Silver-tungsten electrical contact material with high dispersion degree and high compactness and preparation method thereof |
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| 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 |
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| 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 |
-
2019
- 2019-04-15 CN CN201910297951.2A patent/CN110129603B/en active Active
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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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192774A (en) * | 2021-11-23 | 2022-03-18 | 浙江福达合金材料科技有限公司 | Silver-tungsten electrical contact material with high dispersion degree and high compactness and preparation method thereof |
| 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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