CN104384512B - A kind of preparation method of silver-tungsten carbide contact material - Google Patents
A kind of preparation method of silver-tungsten carbide contact material Download PDFInfo
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- CN104384512B CN104384512B CN201410711779.8A CN201410711779A CN104384512B CN 104384512 B CN104384512 B CN 104384512B CN 201410711779 A CN201410711779 A CN 201410711779A CN 104384512 B CN104384512 B CN 104384512B
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Abstract
The invention discloses the preparation method of a kind of silver-tungsten carbide contact material.The method is argentum powder and tungsten carbide powder to be mixed, and gained mixed-powder is placed in ball mill carries out ball milling with high purity nickel ball and water, and the powder body drying after gained ball milling, annealing, molding, infiltration process, and must and get final product；Wherein: described high purity nickel ball is 4～10:1 with the weight ratio of mixed-powder；The consumption of described water adds 130～220ml water by every 1kg mixed-powder and calculates；The time of described ball milling is 15～60h.Mixed-powder and high purity nickel ball and water are placed in ball mill by specific proportioning and carry out ball milling special time by the present invention, have both made the mixing of argentum powder and tungsten carbide powder be more uniformly distributed；Realize again ball milling and addition additive nickel is carried out simultaneously；Also make the nickel by being lost because of ball milling on high purity nickel ball can cover the surface to tungsten particle equably, to reach the purpose being effectively improved silver to the wettability of tungsten carbide；Resulting materials even tissue, consistency is high, resistivity is low.
Description
Technical field
The present invention relates to the preparation method of a kind of silver-tungsten carbide contact material, belong to metal-base composites neck
Territory.
Background technology
Owing to the fusing point of tungsten carbide is high, electrocorrosion-resisting is strong, and silver has excellent electrical and thermal conductivity performance,
Silver tungsten carbide material is with good electrocorrosion-resisting and electrical and thermal conductivity, thus silver tungsten carbide contact material
Material is widely used on low-pressure plastic shell circuit breaker, frame-type circuit breaker.Contact rise connection, carrying and
The effect of breaking current, is the heart component of chopper, and its performance determines chopper to a great extent
Performance and reliability of operation.Therefore chopper has the requirement of harshness to contact, it is desirable to have:
The best arc resistant scaling loss ability, the highest fusion welding resisting ability, 3. long mechanical life, the best
Electrical and thermal conductivity performance.For silver-tungsten carbide contact material, the requirement of chopper to be met, should reach as follows
Requiring: 1. tungsten carbide particle is tiny and is distributed evenly on silver matrix, 2. contact consistency is high, 3. touches
The resistivity of head material is low.
At present, silver-tungsten carbide contact material manufacturing process has mixed powder sintering method and infiltration method, mixed powder sintering method
Technological process be: tungsten carbide powder, argentum powder → mixing → molding → sintering → multiple pressure, obtained contact
Tungsten particle skewness, is easily layered, and consistency is low, it is difficult to meet the use requirement of chopper；Infiltration
Silvering solution body is penetrated in silver tungsten carbide pressed compact by having main steps that at a temperature of more than silver point of method, made
The silver-colored tungsten carbide contact consistency obtained is high, and therefore silver tungsten carbide contact generally uses infiltration method to manufacture；But
Owing to silver is poor to the wettability of tungsten carbide, infiltration method technique is used to need when manufacturing to add trace meter unit
Element, such as nickel, cobalt, ferrum, improves the silver wettability to tungsten carbide, and silvering solution body just can be made to penetrate into silver carbonization
In tungsten pressed compact, to obtain fine and close silver-colored tungsten carbide contact.The common technological process of existing infiltration method is: carbon
Change tungsten powder, argentum powder, the metallic element → mixing → molding → infiltration → shaping → finished product of interpolation trace, by
Being trace in the metallic element added, they are difficult to be uniformly dispersed and can not be effective at tungsten carbides
Particle surface, causes silver to can not get effectively improving to the wettability of tungsten carbide, the silver-colored fluid low of infiltration
With full silver tungsten carbide pressed compact, thus resulting in contact consistency not ideal enough, metallographic structure is uniform not,
Contact arc resistant scaling loss ability is low.
The patent of invention of Publication No. CN101817079A, discloses a kind of silver-tungsten carbide contact material skeleton
The preparation method of cladding powder, particularly as follows: the average particle size through hydrazine hydrate pretreatment is under 1 μm
Tungsten carbide, adds SILVER NITRATE, after chemical reaction, the silver-colored cladded wolfram carbide granule of reduction, generates bag
Cover mixed-powder, as preparing skeleton powder needed for silver-tungsten carbide contact material infiltration process.This invention prepares
Silver-tungsten carbide contact material its fine grained tungsten carbide and silver matrix between be evenly distributed engage firmly make its resist
Electric arc, resistance to scaling loss performance are increased.But this invention uses toxic chemical substance in preparation process
Hydrazine hydrate, not only has an impact the health of production operation personnel, and the problem that there is also environmental pollution is unfavorable
Sustainable development in society；Secondly, need after preparing silver tungsten carbide cladding mixing mud by chemical reaction
Clean with pure water, during this, create substantial amounts of waste water, there is sewage disposal and environment is dirty
The problem of dye.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation side of a kind of new silver-tungsten carbide contact material
Method.The method technique is simple and environmentally-friendly, and the silver-colored tungsten carbide contact metallographic structure of gained is uniform, consistency
Height, resistivity is low.
The preparation method of silver-tungsten carbide contact material of the present invention, is argentum powder and tungsten carbide powder to be mixed,
Gained mixed-powder is placed in ball mill carries out ball milling with high purity nickel ball and water, the powder body warp after gained ball milling
Be dried, annealing, molding, infiltration process, obtain silver-tungsten carbide contact material；Wherein:
Described high purity nickel ball is 4～10:1 with the weight ratio of mixed-powder；
The consumption of described water adds 130～220ml water by every 1kg mixed-powder and calculates；
The time of described ball milling is 15～60h.
Mixed-powder and high purity nickel ball and water are placed in ball mill by specific proportioning that to carry out ball milling special by the present invention
Fix time, on the one hand, be more uniformly distributed by the mixing of ball milling, argentum powder and tungsten carbide powder；On the other hand,
In mechanical milling process, the nickel being lost because of ball milling on high purity nickel ball can be directly appended to silver tungsten as additive
In mixed powder, it is achieved ball milling and addition additive are carried out simultaneously, and applicant is through lot of experiment validation
Finding, when Ball-milling Time limits within the above range, the nickel in gained contact material accounts for silver and carbon just
Change the 0.2～1.5% of tungsten mixed-powder gross weight；Another further aspect, because the hardness ratio of tungsten carbide particle is high-purity
Nickel ball is much higher, and tungsten carbide powder is sufficiently contacted with nickel ball and grinds, by high purity nickel ball because of ball milling
The nickel of loss can cover the surface to tungsten carbide particle equably, thus reaches to be effectively improved silver to carbonization
The purpose of the wettability of tungsten；Therefore, the method for the invention is used to be made to have tungsten carbide
Grain is tiny and the silver-tungsten carbide contact material of organizational structure that is distributed evenly on silver matrix, and contact material
The consistency of material is high, resistivity is low, and whole manufacture process does not produce any waste water and other garbage.
In technique scheme, described high purity nickel ball is highly purified nickel ball, in order to introduce as little as possible
Impurity, preferably uses the nickel ball of nickel content >=99.9%.Under normal circumstances, a diameter of φ 6～φ is used
The high purity nickel ball of 30mm.
In technique scheme, described tungsten carbide powder and the consumption of argentum powder and proportioning can be according to silver to be prepared
Tungsten carbide contact material calculates, it is generally the case that the weight ratio of tungsten carbide powder and argentum powder is 95～50:
5～50.
In technique scheme, the granularity of described tungsten carbide powder and argentum powder is same as the prior art, at this
In bright, it is preferred to use particle mean size is the tungsten carbide powder of 1～10 μm, it is preferred to use granularity be-100～
The argentum powder of-200 mesh.
In technique scheme, it is common that argentum powder and tungsten carbide powder are placed in V-type or bipyramid blender mixed
Closing, the time of mixing is usually 2～3h.
In technique scheme, be dried the powder body after ball milling, anneal, molding and infiltration process
Technique is same as the prior art, in the present invention, described is dried, work that annealing, molding and infiltration process
Skill parameter is preferably:
Be dried be by ball milling after powder body be placed in 80～150 DEG C under the conditions of dry 2～4h；
Annealing be dried powder body is placed under hydrogen or decomposed ammonia atmosphere, temperature is 700～850 DEG C
Under conditions of, it is incubated 1～3h；
Molding is to be placed in punching block and be pressed into pressed compact by the powder body after annealing, and briquetting pressure is 2～4T/cm2；
If necessary, it is also possible to add the forming agent (such as paraffin etc.) of conventional amount used in prior art；
Infiltration be pressed compact is placed under hydrogen or decomposed ammonia atmosphere, under conditions of temperature 1040～1150 DEG C,
Insulation 10～50min.
Compared with prior art, present invention is characterized in that
1, mixed-powder and high purity nickel ball and water are placed in ball mill by specific proportioning and carry out ball milling by the present invention
Special time, on the one hand, be more uniformly distributed by the mixing of ball milling, argentum powder and tungsten carbide powder；On the other hand,
In mechanical milling process, the nickel being lost because of ball milling on high purity nickel ball can be directly appended to silver tungsten as additive
In mixed powder, it is achieved ball milling and addition additive are carried out simultaneously, and applicant is through lot of experiment validation
Finding, when Ball-milling Time limits within the above range, the nickel in gained contact material accounts for silver and carbon just
Change the 0.2～1.5% of tungsten mixed-powder gross weight；Another further aspect, because the hardness ratio of tungsten carbide particle is high-purity
Nickel ball is much higher, and tungsten carbide powder is sufficiently contacted with nickel ball and grinds, by high purity nickel ball because of ball milling
The nickel of loss can cover the surface to tungsten carbide particle equably, thus reaches to be effectively improved silver to carbonization
The purpose of the wettability of tungsten；Therefore, the method for the invention is used to be made to have tungsten carbide
Grain is tiny and the silver-tungsten carbide contact material of organizational structure that is distributed evenly on silver matrix, and contact material
The consistency of material is high, resistivity is low.
2, compared with existing mixed powder sintering method, the metallographic structure of gained contact material evenly, consistency and
Hardness is higher, and arc resistant scaling loss ability is the highest.
3, compared with existing infiltration method, the metallographic structure of gained contact material evenly, consistency and hardness
Higher, arc resistant scaling loss ability is the highest, and resistivity is low.
4, the present invention manufactures silver tungsten carbide mixed-powder and is combined infiltration manufacture silver with the mode of employing chemical reaction
The method of tungsten carbide contact is compared, and whole manufacture process does not produce any waste water and other garbage, and
Technique is the simplest.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure of the contact material that the embodiment of the present invention 3 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, to be more fully understood that the present invention's
Content, but the present invention is not limited to following example.
Embodiment 1:
Choose the tungsten carbide powder of particle mean size 1 μm and the argentum powder of-200 mesh, by tungsten carbide: silver=50:50's
It is 20kg silver tungsten-carbide powder that weight ratio weighs gross weight, and powder is put into 30 liters of V-type blender mixing 2.5
Hour, mixed silver tungsten-carbide powder, the φ 6～φ 30mm of 200kg are combined (weight ratio is φ 6mm:
φ 10mm: φ 20mm: φ 30mm=3:5:1:1) high purity nickel ball (nickel content is 99.99%), 4400ml
Deionized water is put into the tumbling ball mill of 100 liters together and is carried out ball milling (rotating speed is 45 revs/min), ball milling
Time is 60 hours, takes out powder and dries 2 hours at 150 DEG C, the powder of drying is placed in hydrogen gas
Atmosphere is annealed 3 hours (after testing, the nickel content in gained dusty material is 1.46%) at 850 DEG C, uses
2T/cm2Pressure in punching block will annealing after powder be pressed into pressed compact, by silver strip at lower pressed compact at upper knot
Pressed compact and silver strip are placed in graphite boat by structure, infiltration 20 minutes at 1040 DEG C in hydrogen atmosphere, thus
Silver tungsten carbide 40 contact can be prepared.
Embodiment 2:
Choose the tungsten carbide powder of particle mean size 9 μm and the argentum powder of-100 mesh, by tungsten carbide: silver=95:5's
It is 20kg silver tungsten-carbide powder that weight ratio weighs gross weight, and powder is put into 30 liters of V-type blender mixing 2
Hour, by mixed silver tungsten-carbide powder, the high purity nickel ball of φ 30mm of 80kg, 2600ml deionization
Water is put into the tumbling ball mill of 50 liters together and is carried out ball milling (rotating speed is 50 revs/min), Ball-milling Time 15
Hour, take out powder at 80 DEG C, dry that (after testing, the nickel content in gained dusty material is 4 hours
0.20%), the powder of drying is placed in decomposed ammonia atmosphere and anneals 1 hour at 700 DEG C, use 4T/cm2's
Powder after annealing is pressed into pressed compact in punching block by pressure, by silver strip at lower pressed compact upper by pressed compact with silver strip
It is placed in graphite boat, infiltration 60 minutes at 1150 DEG C in decomposed ammonia atmosphere, thus can prepare silver carbon
Change tungsten 70 contact.
Embodiment 3:
Choose the tungsten carbide powder of particle mean size 3 μm and the argentum powder of-200 mesh, by tungsten carbide: silver=55:45
Weight ratio to weigh gross weight be 20kg silver tungsten-carbide powder, powder is put into 30 liters of V-type blenders mixing 3
Hour, by mixed silver tungsten-carbide powder, the high purity nickel ball of φ 20mm of 200kg, 4400ml deionization
Water is put into the tumbling ball mill of 100 liters together and is carried out ball milling (rotating speed is 45 revs/min), Ball-milling Time 60
Hour (after testing, the nickel content in gained dusty material is 1.48%), take out powder and dry at 150 DEG C
2 hours, the powder of drying is placed in hydrogen atmosphere and anneals 3 hours at 850 DEG C, use 2.5T/cm2Pressure
Powder after annealing is pressed into pressed compact in punching block by power, by silver strip lower pressed compact upper structure by pressed compact and
Silver strip is placed in graphite boat, infiltration 40 minutes at 1060 DEG C in hydrogen atmosphere, thus can prepare silver carbon
Changing tungsten 45 contact, the metallographic structure figure of gained contact material is as shown in Figure 1.
Embodiment 4:
Choose the tungsten carbide powder of particle mean size 5 μm and the argentum powder of-200 mesh, by tungsten carbide: silver=80:20
Weight ratio to weigh gross weight be 20kg silver tungsten-carbide powder, powder is put into 30 liters of V-type blenders mixing 3
Hour, by mixed silver tungsten-carbide powder, the high purity nickel ball of φ 10mm of 160kg, 3000ml deionization
Water is put into the tumbling ball mill of 100 liters together and is carried out ball milling (rotating speed is 45 revs/min), and Ball-milling Time is
30 hours, take out powder and dry 3 hours at 90 DEG C, the powder of drying is placed in hydrogen atmosphere 800
Anneal 3 hours (after testing, the nickel content in gained dusty material is 0.65%) at DEG C, use 3.5T/cm2's
Pressure in punching block will annealing after powder be pressed into pressed compact, by silver strip at lower pressed compact in upper structure by pressed compact
It is placed in graphite boat with silver strip, infiltration 30 minutes at 1100 DEG C in hydrogen atmosphere, thus can prepare silver
Tungsten carbide 60 contact.
The contact material that embodiment 1～4 prepares is carried out performance detection, and ooze method molten with existing routine prepares
Silver-colored tungsten carbide 45 contact product contrast, result as described in Table 1:
Table 1:
| Embodiment | Material | Hardness, HB | Relative density, % | Resistivity, μ Ω .cm |
| Embodiment 1 | Silver tungsten carbide 40 | 145 | 99.5 | 3.25 |
| Embodiment 2 | Silver tungsten carbide 70 | 325 | 99.7 | 5.52 |
| Embodiment 3 | Silver tungsten carbide 45 | 175 | 99.6 | 3.55 |
| Embodiment 4 | Silver tungsten carbide 60 | 275 | 99.6 | 4.45 |
| Existing conventional infiltration method product | Silver tungsten carbide 45 | 145～168 | 98.8～99.2 | 3.60～3.72 |
Claims (5)
1. the preparation method of a silver-tungsten carbide contact material, it is characterised in that: by argentum powder and carbonization
Tungsten powder mixes, and gained mixed-powder is placed in ball mill carries out ball milling with high purity nickel ball and water, gained ball
Powder body drying after mill, annealing, molding, infiltration process, and obtain silver-tungsten carbide contact material；Its
In:
Described high purity nickel ball is 4～10:1 with the weight ratio of mixed-powder；
The consumption of described water adds 130～220ml water by every 1kg mixed-powder and calculates；
The time of described ball milling is 15～60h.
Preparation method the most according to claim 1, it is characterised in that: described high purity nickel ball
Nickel content >=99.9%.
Preparation method the most according to claim 1, it is characterised in that: described tungsten carbide powder and
The weight ratio of argentum powder is 95～50:5～50.
4. according to the preparation method according to any one of claims 1 to 3, it is characterised in that: described
The particle mean size of tungsten carbide powder is 1～10 μm.
5. according to the preparation method according to any one of claims 1 to 3, it is characterised in that: described
The granularity of argentum powder is-100～-200 mesh.
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| CN111063568B (en) * | 2019-12-15 | 2021-04-16 | 浙江大学 | Preparation method of silver tungsten carbide electrical contact material for circuit breaker |
| CN111411279A (en) * | 2020-03-03 | 2020-07-14 | 福达合金材料股份有限公司 | Silver tungsten carbide diamond composite contact material and preparation method thereof |
| CN112170862A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver-tungsten contact material |
| CN113245548B (en) * | 2021-05-27 | 2021-10-01 | 攀时（上海）高性能材料有限公司 | Infiltration processing technology and silver-tungsten contact material prepared by same |
| CN116904787B (en) * | 2023-07-14 | 2024-03-19 | 苏州市希尔孚新材料股份有限公司 | Preparation method of silver-saving high-performance silver tungsten carbide nickel contact |
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| CN101834070A (en) * | 2009-03-13 | 2010-09-15 | 上海电科电工材料有限公司 | AgWC (wolfram carbide) electrical contact material and manufacturing method thereof |
| CN101651050B (en) * | 2009-07-20 | 2011-07-20 | 温州宏丰电工合金股份有限公司 | Submicron particle reinforced Ag-based electrical contact material and preparation method thereof |
| CN101817079A (en) * | 2009-10-31 | 2010-09-01 | 福达合金材料股份有限公司 | Method for preparing framework coating powder of silver-tungsten carbide contact material |
| CN103290359B (en) * | 2013-06-08 | 2015-07-08 | 西安工程大学 | Preparation method of silver tungsten carbide contact alloy |
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Effective date of registration: 20161228 Address after: 541004 the Guangxi Zhuang Autonomous Region Dongcheng Qixing District, Guilin City Road No. 8 Patentee after: Guilin Jinge Electrotechnical Electronic Material Science & Technology Co., Ltd. Address before: 541004 the Guangxi Zhuang Autonomous Region Dongcheng Qixing District, Guilin City Road No. 8 Patentee before: Guilin Electrical Equipment Scientific Research Institute Co., Ltd. |