CN104384512A - Silver tungsten carbide contact material preparing method - Google Patents
Silver tungsten carbide contact material preparing method Download PDFInfo
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- CN104384512A CN104384512A CN201410711779.8A CN201410711779A CN104384512A CN 104384512 A CN104384512 A CN 104384512A CN 201410711779 A CN201410711779 A CN 201410711779A CN 104384512 A CN104384512 A CN 104384512A
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Abstract
The invention discloses a silver tungsten carbide contact material preparing method. The method includes mixing sliver powder and tungsten carbide powder, placing the mixed powder, high purity nickel balls and water into a ball mill for ball milling, and obtaining the material after the ball-milled powder is dried, annealed, formed and infiltrated. The weight ratio of the high purity nickel balls and the mixed powder ranges from 4 to 10 : 1, 120 to 220ml water is added into 1kg mixed powder, and the time for ball milling ranges from 15 to 60h. The mixed powder, the high purity nickel balls and the water are placed into the ball mill by special configuration ratio for the special ball milling time, the silver powder and the tungsten carbide powder are mixed more uniformly, the ball milling and additive nickel adding can be performed simultaneously, the nickel, of the high purity nickel balls, consumed by ball milling can coat the surfaces of tungsten particles uniformly, the purpose of effectively improving the wettability of the tungsten carbide can be achieved, and the obtained material is uniform in organization, high in density and low in resistivity.
Description
Technical field
The present invention relates to a kind of preparation method of silver-tungsten carbide contact material, belong to field of metal matrix composite.
Background technology
Because the fusing point of tungsten carbide is high, electrocorrosion-resisting is strong, and silver has excellent electrical and thermal conductivity performance, silver-colored tungsten carbide material is with good electrocorrosion-resisting and electrical and thermal conductivity, and thus silver-tungsten carbide contact material is widely used on low-pressure plastic shell circuit breaker, frame-type circuit breaker.Contact plays a part to connect, carry and breaking current, and be the heart component of breaker, its performance determines performance and the reliability of operation thereof of breaker to a great extent.Therefore breaker has harsh requirement to contact, requires to have: 1. good arc resistant scaling loss ability, 2. high anti-melting welding ability, 3. long mechanical life, 4. good electrical and thermal conductivity performance.For silver-tungsten carbide contact material, the requirement of breaker be met, following requirement should be reached: 1. tungsten carbide particle is tiny and be distributed in equably on silver matrix, and 2. contact density is high, and 3. the resistivity of contact material is low.
At present, silver-tungsten carbide contact material manufacturing process has mixed powder sintering method and infiltration method, the technological process of mixed powder sintering method is: tungsten carbide powder, silver powder → mixing → shaping → sintering → multiple pressure, obtained contact tungsten particle skewness, easy layering, density is low, is difficult to the instructions for use meeting breaker; The key step of infiltration method is infiltrated in silver-colored tungsten carbide pressed compact by silvering solution body at the temperature more than silver point, and obtained silver-colored tungsten carbide contact density is high, and therefore silver-colored tungsten carbide contact adopts infiltration method to manufacture usually; But because the wettability of silver to tungsten carbide is poor, adopt during infiltration method manufacture technics and need to add minor metallic element, as nickel, cobalt, iron, improve the wettability of silver to tungsten carbide, silvering solution body just can be made to infiltrate in silver-colored tungsten carbide pressed compact, to obtain fine and close silver-colored tungsten carbide contact.The common technological process of existing infiltration method is: the metallic element → mixing → shaping → infiltration → shaping → finished product of tungsten carbide powder, silver powder, interpolation trace, because the metallic element added is micro-, they are difficult to be uniformly dispersed and can not effectively cover tungsten carbide particle surface, silver is caused to can not get effective improvement to the wettability of tungsten carbide, the silvering solution body infiltrated is not enough to be full of silver-colored tungsten carbide pressed compact, thus cause contact density not ideal enough, metallographic structure is even not, and contact arc resistant scaling loss ability is low.
Publication number is the patent of invention of CN101817079A, disclose a kind of preparation method of framework coating powder of silver-tungsten carbide contact material, be specially: the tungsten carbide under the pretreated average particle size of hydrazine hydrate is 1 μm, add SILVER NITRATE, after chemical reaction, the silver-colored cladded wolfram carbide particle of reduction, generates coated mixed-powder, as preparing skeleton powder needed for silver-tungsten carbide contact material infiltration process.Obtained its fine grained tungsten carbide of silver-tungsten carbide contact material of this invention be evenly distributed between silver matrix engage firmly make its arc resistant, resistance to scaling loss performance is increased.But this invention adopts toxic chemical substance hydrazine hydrate in preparation process, not only there is impact to the health of production operation personnel, also there is the problem of environmental pollution, be unfavorable for the sustainable development of society; Secondly, need after obtaining the coated mixing mud of silver-colored tungsten carbide by chemical reaction to clean with pure water, in this process, create a large amount of waste water, there is the problem of sewage disposal and environmental pollution.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of new silver-tungsten carbide contact material.The method technique is simple, environmental protection, and the silver-colored tungsten carbide contact metallographic structure of gained is even, and density is high, and resistivity is low.
The preparation method of silver-tungsten carbide contact material of the present invention, by silver powder and tungsten carbide powder mixing, gained mixed-powder and high purity nickel ball and water are placed in ball mill and carry out ball milling, and the powder drying after gained ball milling, annealing, shaping, infiltration process, obtain silver-tungsten carbide contact material; Wherein:
The weight ratio of described high purity nickel ball and mixed-powder is 4 ~ 10:1;
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, and on the one hand, by ball milling, the mixing of silver powder and tungsten carbide powder is more even; On the other hand, in mechanical milling process, by on high purity nickel ball because the nickel of ball milling loss directly can add in silver-colored tungsten mixed powder as additive, realize ball milling and add additive carrying out simultaneously, and applicant finds through lot of experiment validation, when Ball-milling Time is limited in above-mentioned scope, the nickel in gained contact material accounts for 0.2 ~ 1.5% of silver and tungsten carbide mixed-powder gross weight just; Again on the one hand, because the hardness ratio high purity nickel ball of tungsten carbide particle is much higher, tungsten carbide powder is contacted fully with nickel ball and is ground, by on high purity nickel ball because the nickel of ball milling loss can to cover the surface to tungsten carbide particle equably, thus reach and effectively improve the object of silver to the wettability of tungsten carbide; Therefore, adopt the method for the invention to manufacture to obtain having tungsten carbide particle tiny and be distributed in the silver-tungsten carbide contact material of the institutional framework on silver matrix equably, and the density of contact material is high, resistivity is low, whole manufacture process does not produce any waste water and other discarded object.
In technique scheme, described high purity nickel ball is highly purified nickel ball, in order to introduce impurity as little as possible, preferably adopts the nickel ball of nickel content >=99.9%.Under normal circumstances, employing diameter is the high purity nickel ball of φ 6 ~ φ 30mm.
In technique scheme, the consumption of described tungsten carbide powder and silver powder and proportioning can calculate according to the silver-tungsten carbide contact material that will prepare, and under normal circumstances, the weight ratio of tungsten carbide powder and silver powder is 95 ~ 50:5 ~ 50.
In technique scheme, the granularity of described tungsten carbide powder and silver powder is same as the prior art, and in the present invention, preferably employing particle mean size is the tungsten carbide powder of 1 ~ 10 μm, preferably adopts granularity to be-100 ~-200 object silver powder.
In technique scheme, normally silver powder and tungsten carbide powder are placed in V-type or bipyramid blender mixes, the time of mixing is generally 2 ~ 3h.
In technique scheme, carry out drying, annealing, technique that is shaping and infiltration process are same as the prior art to the powder after ball milling, in the present invention, described drying, annealing, technological parameter that is shaping and infiltration process are preferably:
Drying be by ball milling after powder be placed under 80 ~ 150 DEG C of conditions and dry 2 ~ 4h;
Annealing is under dried powder being placed in hydrogen or decomposed ammonia atmosphere, temperature is under the condition of 700 ~ 850 DEG C, insulation 1 ~ 3h;
Shaping be by annealing after powder be placed in punching block and be pressed into pressed compact, briquetting pressure is 2 ~ 4T/cm
2; If necessary, the forming agent (as paraffin etc.) of conventional amount used in prior art can also be added;
Infiltration is under pressed compact being placed in hydrogen or decomposed ammonia atmosphere, under the condition of temperature 1040 ~ 1150 DEG C, insulation 10 ~ 50min.
Compared with prior art, feature of the present invention is:
1, 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, and on the one hand, by ball milling, the mixing of silver powder and tungsten carbide powder is more even; On the other hand, in mechanical milling process, by on high purity nickel ball because the nickel of ball milling loss directly can add in silver-colored tungsten mixed powder as additive, realize ball milling and add additive carrying out simultaneously, and applicant finds through lot of experiment validation, when Ball-milling Time is limited in above-mentioned scope, the nickel in gained contact material accounts for 0.2 ~ 1.5% of silver and tungsten carbide mixed-powder gross weight just; Again on the one hand, because the hardness ratio high purity nickel ball of tungsten carbide particle is much higher, tungsten carbide powder is contacted fully with nickel ball and is ground, by on high purity nickel ball because the nickel of ball milling loss can to cover the surface to tungsten carbide particle equably, thus reach and effectively improve the object of silver to the wettability of tungsten carbide; Therefore, adopt the method for the invention to manufacture to obtain having tungsten carbide particle tiny and be distributed in the silver-tungsten carbide contact material of the institutional framework on silver matrix equably, and the density of contact material is high, resistivity is low.
2, compared with existing mixed powder sintering method, the metallographic structure of gained contact material evenly, density and hardness higher, arc resistant scaling loss ability is also higher.
3, compared with existing infiltration method, the metallographic structure of gained contact material evenly, density and hardness higher, arc resistant scaling loss ability is also higher, and resistivity is low.
4, the present invention and the mode of employing chemical reaction manufacture silver-colored tungsten carbide mixed-powder in conjunction with infiltration manufacture silver tungsten carbide contact method compared with, whole manufacture process does not produce any waste water and other discarded object, and technique is more simple.
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, and to understand content of the present invention better, but the present invention is not limited to following examples.
Embodiment 1:
Choose tungsten carbide powder and-200 object silver powder of particle mean size 1 μm, by tungsten carbide: it is 20kg silver tungsten-carbide powder that the weight ratio of silver=50:50 takes gross weight, powder is put into 30 liters of V-type blenders and mix 2.5 hours, by mixed silver-colored tungsten-carbide powder, φ 6 ~ φ 30mm of 200kg combines the high purity nickel ball (nickel content is 99.99%) of (weight ratio is φ 6mm: φ 10mm: φ 20mm: φ 30mm=3:5:1:1), the tumbling ball mill that 4400ml deionized water puts into 100 liters together carries out ball milling (rotating speed is 45 revs/min), Ball-milling Time is 60 hours, take out powder to dry 2 hours at 150 DEG C, 3 hours are annealed (after testing at the powder of oven dry being placed in hydrogen atmosphere 850 DEG C, nickel content in gained dusty material is 1.46%), use 2T/cm
2pressure in punching block, the powder after annealing is pressed into pressed compact, in upper structure, pressed compact and silver strip are placed in graphite boat at lower pressed compact by silver strip, in hydrogen atmosphere, infiltration 20 minutes at 1040 DEG C, can obtain silver-colored tungsten carbide 40 contact thus.
Embodiment 2:
Choose tungsten carbide powder and-100 object silver powder of particle mean size 9 μm, by tungsten carbide: it is 20kg silver tungsten-carbide powder that the weight ratio of silver=95:5 takes gross weight, powder is put into 30 liters of V-type blenders and mix 2 hours, by mixed silver-colored tungsten-carbide powder, the high purity nickel ball of the φ 30mm of 80kg, the tumbling ball mill that 2600ml deionized water puts into 50 liters together carries out ball milling (rotating speed is 50 revs/min), Ball-milling Time 15 hours, take out powder and at 80 DEG C, dry 4 hours (after testing, nickel content in gained dusty material is 0.20%), anneal 1 hour at the powder of oven dry being placed in decomposed ammonia atmosphere 700 DEG C, use 4T/cm
2pressure in punching block, the powder after annealing is pressed into pressed compact, upper, pressed compact and silver strip are placed in graphite boat at lower pressed compact by silver strip, in decomposed ammonia atmosphere, infiltration 60 minutes at 1150 DEG C, can obtain silver-colored tungsten carbide 70 contact thus.
Embodiment 3:
Choose tungsten carbide powder and-200 object silver powder of particle mean size 3 μm, by tungsten carbide: it is 20kg silver tungsten-carbide powder that the weight ratio of silver=55:45 takes gross weight, powder is put into 30 liters of V-type blenders and mix 3 hours, by mixed silver-colored tungsten-carbide powder, the high purity nickel ball of the φ 20mm of 200kg, the tumbling ball mill that 4400ml deionized water puts into 100 liters together carries out ball milling (rotating speed is 45 revs/min), Ball-milling Time 60 hours (after testing, nickel content in gained dusty material is 1.48%), take out powder to dry 2 hours at 150 DEG C, anneal 3 hours at the powder of oven dry being placed in hydrogen atmosphere 850 DEG C, use 2.5T/cm
2pressure in punching block by annealing after powder be pressed into pressed compact, in upper structure, pressed compact and silver strip are placed in graphite boat at lower pressed compact by silver strip, infiltration 40 minutes at 1060 DEG C in hydrogen atmosphere, can obtain silver-colored tungsten carbide 45 contact thus, the metallographic structure figure of gained contact material as shown in Figure 1.
Embodiment 4:
Choose tungsten carbide powder and-200 object silver powder of particle mean size 5 μm, by tungsten carbide: it is 20kg silver tungsten-carbide powder that the weight ratio of silver=80:20 takes gross weight, powder is put into 30 liters of V-type blenders and mix 3 hours, by mixed silver-colored tungsten-carbide powder, the high purity nickel ball of the φ 10mm of 160kg, the tumbling ball mill that 3000ml deionized water puts into 100 liters together carries out ball milling (rotating speed is 45 revs/min), Ball-milling Time is 30 hours, take out powder to dry 3 hours at 90 DEG C, 3 hours are annealed (after testing at the powder of oven dry being placed in hydrogen atmosphere 800 DEG C, nickel content in gained dusty material is 0.65%), use 3.5T/cm
2pressure in punching block, the powder after annealing is pressed into pressed compact, in upper structure, pressed compact and silver strip are placed in graphite boat at lower pressed compact by silver strip, in hydrogen atmosphere, infiltration 30 minutes at 1100 DEG C, can obtain silver-colored tungsten carbide 60 contact thus.
The contact material that embodiment 1 ~ 4 is obtained carries out Performance Detection, and contrasts with molten silver-colored tungsten carbide 45 contact product of oozing method obtained of existing routine, 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 characterized in that: by silver powder and tungsten carbide powder mixing, gained mixed-powder and high purity nickel ball and water are placed in ball mill and carry out ball milling, powder drying after gained ball milling, annealing, shaping, infiltration process, obtain silver-tungsten carbide contact material; Wherein:
The weight ratio of described high purity nickel ball and mixed-powder is 4 ~ 10:1;
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.
2. preparation method according to claim 1, is characterized in that: nickel content >=99.9% of described high purity nickel ball.
3. preparation method according to claim 1, is characterized in that: the weight ratio of described tungsten carbide powder and silver powder is 95 ~ 50:5 ~ 50.
4. the preparation method according to any one of claims 1 to 3, is characterized in that: the particle mean size of described tungsten carbide powder is 1 ~ 10 μm.
5. the preparation method according to any one of claims 1 to 3, is characterized in that: the granularity of described silver powder is-100 ~-200 orders.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111063568A (en) * | 2019-12-15 | 2020-04-24 | 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 |
CN113245548A (en) * | 2021-05-27 | 2021-08-13 | 攀时(上海)高性能材料有限公司 | Infiltration processing technology and silver-tungsten contact material prepared by same |
CN116904787A (en) * | 2023-07-14 | 2023-10-20 | 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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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111063568A (en) * | 2019-12-15 | 2020-04-24 | 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 |
CN113245548A (en) * | 2021-05-27 | 2021-08-13 | 攀时(上海)高性能材料有限公司 | Infiltration processing technology and silver-tungsten contact material prepared by same |
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 |
CN116904787A (en) * | 2023-07-14 | 2023-10-20 | 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 |
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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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. |