CN104362015B - Preparation method of copper-tungsten contact material - Google Patents

Preparation method of copper-tungsten contact material Download PDF

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Publication number
CN104362015B
CN104362015B CN201410714823.0A CN201410714823A CN104362015B CN 104362015 B CN104362015 B CN 104362015B CN 201410714823 A CN201410714823 A CN 201410714823A CN 104362015 B CN104362015 B CN 104362015B
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tungsten
copper
powder
ball
contact material
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CN104362015A (en
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陈名勇
颜培涛
贾波
吴春涛
林毓
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Guilin Jinge Electrotechnical Electronic Material Science & Technology Co., Ltd.
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Guilin Electrical Equipment Scientific Research Institute Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/048Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H69/00Apparatus or processes for the manufacture of emergency protective devices

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Contacts (AREA)

Abstract

The invention discloses a preparation method of a copper-tungsten contact material. The method comprises the steps of performing ball grinding on tungsten powder, high-purity nickel balls and water in a ball grinding machine, and performing drying, annealing, forming, pre-sintering and infiltration treatment on the tungsten powder subjected to ball grinding, wherein the weight ratio of the high-purity nickel balls to the tungsten powder is (4-10) to 1; the use amount of the water is calculated according to a fact that every 1kg of tungsten powder is added to 120-150ml of water; and the ball grinding is executed for 12-48 hours. By the adoption of the special ball grinding technology, adding of nickel and ball grinding are simultaneously executed; furthermore, the added nickel can uniformly cover the surface of the tungsten particles, so that the activated sintering effect of a tungsten framework is effectively enhanced, and a tungsten framework with high performance can be obtained; the copper-tungsten contact material prepared by performing infiltration treatment on the tungsten framework and a copper sheet has a tissue structure that the tungsten particles are uniformly distributed on a copper base body, so that the prepared contact material is perfect in arc erosion resistance and high in high-temperature mechanical strength.

Description

A kind of preparation method of copper tungsten contact material
Technical field
The present invention relates to a kind of preparation method of copper tungsten contact material, belongs to field of metal matrix composite.
Background technology
Because the fusing point of tungsten is high, resistance to arc erosion is strong, and copper has excellent electrical and thermal conductivity performance, and copper tungsten material has concurrently There is good resistance to arc erosion and electrical and thermal conductivity, thus copper tungsten contact material is widely used in SF as arcing contact6 On primary cut-out, play a part of to connect and breaking current.Due to connect and breaking current during, on the one hand produced by Electric arc is all born by arcing contact, and contact will be corroded by electric arc, high temperature and thermal stress are acted on, on the other hand because it is dynamic, The mutual impact friction of static contact, contact will also be acted on by mechanical stress, and the failure of contact is mainly arc erosion and high temperature Caused by mechanical friction deterioration reciprocation, therefore copper tungsten contact will not only have good resistance to arc erosion also to have enough High high temperature mechanical strength.
In this regard, copper tungsten contact should correspondingly possess following performance:1. it is distributed evenly on Copper substrate with tungsten particle Institutional framework, possessing such organizing ability makes contact obtain good resistance to arc erosion, and 2. the W skeleton of contact has foot Enough high high temperature mechanical strengths, and such performance is obtained, it is necessary that the tungsten particle contacted with each other in W skeleton is sintered into Be integrated so that each tungsten particle continuously into an overall W skeleton, so could be formed one at high temperature impact resistance wear and tear Contact body.
At present, copper tungsten contact material fabrication process has:1. 1800 DEG C of high temperature above pre-burning W skeletons, then ooze copper, manufacture Technique is:Tungsten powder → shaping → pre-burning W skeleton → infiltration, can obtain each tungsten particle continuously whole into one using this technique The W skeleton of body, contact has excellent resistance to arc erosion and high high temperature mechanical strength, but Preparation equipment is expensive, and the energy disappears Consumption is high;2. less than 1450 DEG C cryogenic activating sintering W skeletons, then ooze copper, and manufacturing process is:The metallic element of tungsten powder+micro → Mixing → shaping → pre-burning W skeleton → infiltration, adds one kind that micro metallic element mostly is in nickel, cobalt, iron, but because micro Metallic element be difficult to be evenly distributed, the sintering effect of W skeleton is poor, and the high temperature mechanical strength of contact is low, shock resistance under high temperature The performance of abrasion is low, so as to reduce switch reliability of operation.
The patent of invention of Publication No. CN101279365A, discloses a kind of W-Cu electrical contact material of high arc resistant ablation Preparation method, the method carries out according to the following steps:Weigh copper powder, tungsten powder and rare earth simple substance lanthanum or cerium in proportion first;So Afterwards 20~40% copper powder, tungsten powder and whole rare earth simple substance lanthanums or cerium are placed in high energy ball mill and carry out mechanical alloying;Again It is secondary that the nickel powder and ethanol of remaining copper powder, tungsten powder and addition are carried out into common mechanical mixture;It is compressing in a mold;Finally will Pressed compact is fitted in high temperature protection atmosphere sintering furnace the tungsten copper electricity for obtaining high arc resistant ablation using infiltration technique sinter molding and touches Head.But there are the following problems for the method:1. 0.05~0.15% micro activated sintering elemental nickel added, in mechanical mixture mistake It is difficult in journey dispersed;The copper powder of 2.4~17.6% ratios for 2. adding is more much more than the nickel for adding, in mechanical mixture mistake Because the probability that the inhibition tungsten particle of copper powder captures nickel is greatly lowered in journey;3. after mechanical mixture, it is difficult to deposit with avoiding There is measuring copper.Therefore in follow-up melting infiltration sintering, the activated sintering effect of W skeleton can have a greatly reduced quality, in W skeleton mutually The tungsten particle of contact can not be sintered into one, therefore the high temperature mechanical strength of obtained copper tungsten also can be greatly lowered, tungsten The disperse degree of grain is also not high enough.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of copper tungsten contact material.The method may be implemented in The automatic addition of nickel is realized while ball milling, and nickel is uniformly distributed in tungsten powder, obtained copper tungsten contact metallographic structure Uniformly, with excellent resistance to arc erosion and high high temperature mechanical strength.
The preparation method of copper tungsten contact material of the present invention, it is characterised in that:Take tungsten powder, high purity nickel ball and water to be placed in Ball milling is carried out in ball mill, tungsten powder drying, annealing, shaping, pre-sintering, the infiltration process after gained ball milling obtains copper tungsten and touches Head material;Wherein:
The high purity nickel ball is 4~10 with the weight ratio of tungsten powder:1;
The consumption of the water adds 120~150ml water to calculate by per 1kg tungsten powders;
The time of the ball milling is 12~48h.
Tungsten powder and high purity nickel ball and water are placed in ball mill and carry out ball milling special time by the present invention by specific proportioning, a side Face, in mechanical milling process, by high purity nickel ball because ball milling loss nickel can be directly appended in tungsten powder as additive, realize ball Mill and addition additive are carried out simultaneously, and applicant has found through lot of experiment validation, when Ball-milling Time is limited to above-mentioned model When enclosing interior, the nickel in gained contact material accounts for the 0.1~1.0% of tungsten powder gross weight just;On the other hand, because of the hardness of tungsten particle More much higher than high purity nickel ball, tungsten powder is sufficiently contacted and ground with nickel ball, by high purity nickel ball because ball milling loss nickel can Equably to cover the surface to tungsten particle, so as to reach the purpose for effectively improving W skeleton sintering effect;Therefore, using this Bright methods described is made to the copper tungsten contact material with excellent resistance to arc erosion and high high temperature mechanical strength.
In above-mentioned technical proposal, described high purity nickel ball is highly purified nickel ball, in order to introduce impurity as little as possible, preferably It is using the nickel ball of nickel content >=99.9%.Under normal circumstances, using the high purity nickel ball of a diameter of 6~φ of φ 30mm.
In above-mentioned technical proposal, copper sheet is put in infiltration step, and the consumption and proportioning of the tungsten powder and copper sheet can bases The copper tungsten contact material to be prepared is calculating.
In above-mentioned technical proposal, the granularity of the tungsten powder is same as the prior art, in the present invention, it is preferred to using average grain Spend the tungsten powder for 2~9 μm.
In above-mentioned technical proposal, the tungsten powder after ball milling is dried, is annealed, is molded, the work that pre-sintered and infiltration is processed Skill is same as the prior art, and in the present invention, the technological parameter that the drying, annealing, shaping, pre-sintering and infiltration are processed is preferred For:
Drying be the tungsten powder after ball milling is placed in into 80~150 DEG C under the conditions of dry 2~4h;
Annealing be dried tungsten powder is placed in into hydrogen or decomposed ammonia atmosphere under, the condition that temperature is 700~850 DEG C Under, it is incubated 1~3h;
Shaping is that the tungsten powder after annealing is placed in punching block to be pressed into pressed compact, and briquetting pressure is 2~4T/cm2;If must Will, the forming agent (such as paraffin) of conventional amount used in prior art can also be added;
Pre-sintering be pressed compact is placed in into hydrogen or decomposed ammonia atmosphere under, under conditions of 1300~1450 DEG C of temperature, insulation 1 ~2h;
Infiltration be by copper sheet and pre-sintering after pressed compact be placed in hydrogen or decomposed ammonia atmosphere under, 1150~1250 DEG C of temperature Under conditions of, it is incubated 1~2h.
Compared with prior art, the method have the characteristics that:
1st, using special ball-milling technology not only make nickel addition and ball milling while carry out, and the nickel for adding can be uniform Ground covers the surface to tungsten particle, is effectively improved the activated sintering effect of W skeleton so as to obtain tungsten bone of good performance Frame, by gained W skeleton and copper sheet Jing after infiltration process the copper tungsten contact material of gained that there is tungsten particle to be distributed evenly in is copper-based Institutional framework on body, thus contact have excellent resistance to arc erosion and high high temperature mechanical strength (due to during ball milling not Copper powder is added, so pressed compact does not have copper segregation, contact can obtain tungsten particle and be distributed evenly in copper after pre-sintered and infiltration Institutional framework on matrix, the high-melting-point tungsten of even dispersion mutually substantially increases the ability of the resistance to arc erosion of contact.Nickel is equably The surface to tungsten particle is covered, the activated sintering effect of W skeleton is effectively improved so that tungsten particle is sintered into one, tungsten Skeleton becomes high intensity skeleton, can tolerate high-temperature machinery abrasion), gained contact material is applied to SF6It is complete on primary cut-out The reciprocation of arc erosion and high-temperature machinery friction deterioration can be withstood entirely, can be improved the service life of contact and be broken Road device reliability of operation;
2nd, compared with high temperature pre-sintering, the technology of the present invention is capable of achieving using conventional equipment, and low cost, power consumption is low.
Description of the drawings
Fig. 1 is the pre-sintered SEM figures for processing the W skeleton for obtaining of Jing in the embodiment of the present invention 3;
Fig. 2 is the metallographic structure figure of the contact material that the embodiment of the present invention 3 is prepared.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, to more fully understand present disclosure, but The present invention is not limited to following examples.
Embodiment 1:
The tungsten powder of 2 μm of 20kg particle mean sizes is weighed, 6~φ of φ 30mm of tungsten powder, 200kg are combined into (weight ratio therein For φ 6mm:φ10mm:φ20mm:φ 30mm=3:5:1:1) high purity nickel ball, 3000ml deionized waters are put into together 100 liters Tumbling ball mill in carry out ball milling (rotating speed be 45 revs/min), Ball-milling Time 24 hours, taking out powder, that 2 are dried at 150 DEG C is little When, the powder of drying is placed in hydrogen atmosphere into annealing at 700 DEG C, and (after testing, the nickel content in gained dusty material is within 2 hours 0.55%), 2T/cm is used2Pressure the powder after annealing is pressed into into pressed compact in punching block, pressed compact is placed in graphite boat, in hydrogen Sintering obtains W skeleton in 1 hour at 1300 DEG C in gas atmosphere, and by W skeleton base respective quality copper sheet is placed in graphite boat and adds (for the 57% of W skeleton weight), thus infiltration 2 hours at 1200 DEG C in hydrogen atmosphere can be obtained the contact of copper tungsten 70.
Embodiment 2:
The tungsten powder of 9 μm of 20kg particle mean sizes is weighed, by tungsten powder, the high purity nickel ball of the φ 20mm of 80kg, 2400ml deionizations Water is put into together in 50 liters of tumbling ball mill carries out ball milling (rotating speed be 50 revs/min), Ball-milling Time 12 hours, take out powder in Dry 4 hours at 80 DEG C, the powder of drying is placed in in hydrogen atmosphere 1 hour (after testing, gained powder material of annealing at 850 DEG C Nickel content in material is 0.15%), to use 4T/cm2Pressure the powder after annealing is pressed into into pressed compact in punching block, pressed compact is placed in In graphite boat, 1450 DEG C in decomposed ammonia atmosphere at sintering obtain W skeleton within 1 hour, W skeleton base is placed in graphite boat simultaneously Add respective quality copper sheet (for the 24% of W skeleton weight), 1250 DEG C in decomposed ammonia atmosphere at infiltration 1 hour, thus may be used The prepared contact of copper tungsten 85.
Embodiment 3:
Weigh the tungsten powder that 20kg particle mean sizes are 6 μm, by tungsten powder, the high purity nickel ball of the φ 10mm of 160kg, 2600ml go from Sub- water is put into together in 100 liters of tumbling ball mill carries out ball milling (rotating speed is 45 revs/min), and Ball-milling Time 48 hours takes out powder Expect to be dried 3 hours at 100 DEG C, the powder of drying is placed in decomposed ammonia atmosphere at 800 DEG C and anneals 1.5 hours (after testing, Nickel content in gained dusty material is 0.96%), to use 3T/cm2Pressure the powder after annealing is pressed into into pressed compact in punching block, Pressed compact is placed in graphite boat, sintering obtains W skeleton (as shown in Figure 1) for 2 hours at 1400 DEG C in hydrogen atmosphere, by tungsten bone Frame base is placed in graphite boat and adds respective quality copper sheet (for the 31% of W skeleton weight), melts at 1250 DEG C in hydrogen atmosphere Ooze 1 hour, the contact of copper tungsten 80 thus can be obtained, the metallurgical structure figure of gained contact material is as shown in Figure 2.
Carry out performance detection to contact material obtained in embodiment 1~3, and with copper tungsten 80 obtained in existing conventional infiltration method The performance of contact material is contrasted, as a result as described in Table 1:
Table 1:
Embodiment Material Relative density, % Testing Tensile Strength at Elevated Temperature, MPa
Embodiment 1 Copper tungsten 70 99.6 /
Embodiment 2 Copper tungsten 85 99.7 /
Embodiment 3 Copper tungsten 80 99.6 185
Existing infiltration method product Copper tungsten 80 99.1~99.4 125~150

Claims (3)

1. a kind of preparation method of copper tungsten contact material, it is characterised in that:Take tungsten powder, high purity nickel ball and water to be placed in ball mill Row ball milling, tungsten powder drying, annealing, shaping, pre-sintering, the infiltration process after gained ball milling, obtains copper tungsten contact material;Its In:
The high purity nickel ball is 4~10 with the weight ratio of tungsten powder:1;
The consumption of the water adds 120~150ml water to calculate by per 1kg tungsten powders;
The time of the ball milling is 12~48h.
2. preparation method according to claim 1, it is characterised in that:Nickel content >=99.9% of the high purity nickel ball.
3. preparation method according to claim 1 and 2, it is characterised in that:The particle mean size of the tungsten powder is 2~9 μm.
CN201410714823.0A 2014-11-28 2014-11-28 Preparation method of copper-tungsten contact material Active CN104362015B (en)

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CN108950289B (en) * 2018-07-03 2020-07-10 中国科学院金属研究所 Copper-tungsten composite material with micro-oriented structure and preparation method thereof
CN111299594A (en) * 2019-11-29 2020-06-19 安徽恒均粉末冶金科技股份有限公司 Preparation method of copper-tungsten petal contact
CN111863488A (en) * 2020-07-13 2020-10-30 安徽恒均粉末冶金科技股份有限公司 Method for preparing electric appliance switch contact by powder metallurgy copper-tungsten alloy
CN115360032B (en) * 2022-08-30 2024-05-28 中国南方电网有限责任公司超高压输电公司检修试验中心 Copper-tungsten contact and preparation method and application thereof

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JP3675378B2 (en) * 2001-08-20 2005-07-27 三菱マテリアルシ−エムアイ株式会社 High specific gravity high strength tungsten sintered alloy weight
JP2004353006A (en) * 2003-05-27 2004-12-16 Mitsubishi Material Cmi Kk Weight made of tungsten-based sintered alloy
CN101667498B (en) * 2009-10-13 2011-08-24 昆明理工大学 Preparation method of W-Cu electrical contact
CN101928866B (en) * 2010-03-23 2012-09-05 西安理工大学 W-Cu composite material prepared from La-Ni intensified-sintered W skeleton and preparation method thereof
CN102237204A (en) * 2010-04-27 2011-11-09 上海电科电工材料有限公司 High-voltage tungsten-base composite contact material and method for making same
CN102162055B (en) * 2011-04-08 2012-08-22 福州博力达机电有限公司 Method for preparing a tungsten-copper composite material with high arc ablation resistance
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CN103981389B (en) * 2014-05-15 2016-06-15 厦门理工学院 A kind of method that low-temperature sintering W skeleton prepares tungsten-copper alloy

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