CN105551859B - A kind of preparation method of sheet silver-graphite electrical contact material - Google Patents

A kind of preparation method of sheet silver-graphite electrical contact material Download PDF

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Publication number
CN105551859B
CN105551859B CN201511009658.XA CN201511009658A CN105551859B CN 105551859 B CN105551859 B CN 105551859B CN 201511009658 A CN201511009658 A CN 201511009658A CN 105551859 B CN105551859 B CN 105551859B
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silver
graphite
powder
electrical contact
preparation
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CN105551859A (en
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张天锦
王振宇
王奐然
李波
杨志伟
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Guilin Electrical Equipment Scientific Research Institute 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F3/04Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Powder Metallurgy (AREA)
  • Contacts (AREA)

Abstract

The invention discloses a kind of preparation method of sheet silver-graphite electrical contact material, is specially:Material mixture ratio according to the silver-graphite electrical contact of required preparation calculates required graphite powder and carbonic acid silver powder, weighs standby;Carbonic acid silver powder and graphite powder are subjected to mixed powder, obtained silver carbonate graphite mixed powder obtains the silver-colored graphite billet of parcel silver layer on the outside of spindle through being molded, being calcined, sintering and decarbonization process;Further be processed into band through hot extrusion, after through rolling, punch process, obtain sheet silver-graphite electrical contact.The method of the invention can effectively reduce directly contacting for brittlement phase graphite and Argent grain, make that the mechanical and physical character of obtained product and processing characteristics are more excellent, and metallographic structure is more uniformly distributed.

Description

A kind of preparation method of sheet silver-graphite electrical contact material
Technical field
The present invention relates to electrical contact material, and in particular to a kind of preparation method of sheet silver-graphite electrical contact material.
Background technology
Silver-graphite electrical contact with excellent thermal conductivity and resistance fusion welding energy due to being widely used in small-sized In the low-voltage electrical apparatuses such as breaker, line protection switch, failure current protection switch.As a rule, silver-graphite electrical contact material Preparation method mainly has two kinds of powder mixing method and electroless plating method.
Powder mixing method is that electrical contact manufacturer produces the most frequently used method of silver-colored graphite both at home and abroad at present, and this method is using machinery Hybrid mode mixes silver powder, graphite powder, and mixed powder then is carried out into a series of processing such as isostatic pressed, sintering, extruding, Finally obtain silver-graphite electrical contact.This method preparation technology is simple, the process-cycle is short, production cost is low, but because graphite is Brittlement phase material, it is mainly distributed on when carrying out powder mixing machine with silver between Argent grain so that brittlement phase graphite and Argent grain are direct Contact, so as to influence the processing characteristics of material.Electroless plating method refer to by graphite powder be added in silver nitrate solution formed suspend it is molten Liquid, then add reducing agent and obtain silver-colored graphite coat powder, and add through over cleaning, drying, isostatic pressed, sintering, extruding etc. are a series of Work, finally obtain silver-graphite electrical contact.It is fully dispersed that the shortcomings that this kind of method, is that graphite powder is not easy in silver nitrate solution, easily Occur graphite aggregation in material structure, influence materials microstructure performance, meanwhile, this kind of method preparation technology is complicated, processing week Phase is grown, and production cost is of a relatively high.Therefore, how on the premise of material property and unobvious increase cost is ensured, prepare The excellent silver-colored graphite material of structure property, turns into the difficult point studied at present and focus.
Publication No. CN101763956A patent of invention discloses a kind of silver-graphite electrical contact material and preparation method thereof. This method is that the composite powder of graphite and ceramics, reducing agent, deionized water are made into reduction suspension first, is then added into In silver ammino solution, silver-plated graphite ceramic composite powder is obtained, finally by made from silver-plated graphite ceramic composite powder and water atomization Silver-rare earth alloy powder mixing, obtains silver-graphite electrical contact material.The deficiency of the technology is that graphite is not easy in suspension is reduced It is fully dispersed, so as to influence the metallographic structure of material.
Publication No. CN1234591A patent of invention discloses a kind of method for preparing silver-graphite electrical contact belt.This method That spherical graphite powder and cebollite ink powder and atomization silver powder and chemical silver powder are mixed into powder according to a certain percentage, then through overmolding, Sintering, and extruded after wrapping up one layer of silver layer on the outside of silver-colored graphite spindle, the silver-colored graphite tape of silver-coated layer is obtained, is finally passed through Roll, cover the processes such as solder, annealing after obtain silver-graphite electrical contact belt finished product.The invention equally exists brittlement phase graphite and silver The problem of particle directly contacts.
The content of the invention
In view of the deficienciess of the prior art, the present invention provides a kind of preparation side of new sheet silver-graphite electrical contact material Method, is proposed to prepare silver-graphite electrical contact material with decomposition in situ method, and brittlement phase can be effectively reduced using the method for the invention Graphite directly contacts with Argent grain, products obtained therefrom is had excellent mechanical and physical character and processing characteristics, while metallographic group Knit and be more uniformly distributed.
The preparation method of sheet silver-graphite electrical contact material of the present invention, comprises the following steps:
1) required graphite powder and carbonic acid silver powder are calculated according to the material mixture ratio of the silver-graphite electrical contact of required preparation Dosage, weigh standby;
2) take carbonic acid silver powder to carry out mixed powder with graphite powder, obtain silver carbonate graphite mixed powder;
3) it is placed in vacuum and is calcined after gained silver carbonate graphite mixed powder isostatic pressing, obtains silver-colored graphite billet;
4) the silver-colored graphite billet of gained, which is placed in vacuum or hydrogen or inert gas, sinters, and is placed in air is taken off again afterwards Carbon, obtain the silver-colored graphite billet of parcel silver layer on the outside of spindle;
5) the silver-colored graphite billet of parcel silver layer is processed under hydrogen or inert gas shielding through hot extrusion on the outside of gained spindle Into band, rolled again afterwards, then stamped processing, obtain sheet silver-graphite electrical contact.
The present invention carries out mixed powder using silver carbonate and graphite powder, and the silver carbonate graphite billet after shaping is fired, sinters etc. Silver-colored graphite billet is obtained after process.Because decomposition in situ reaction can occur during vacuum baking for silver carbonate, during this, Silver carbonate can occur decomposition in situ as medium using graphite and form Argent grain so that a part of Argent grain is inhaled by decomposing diffusion It is attached on the surface of graphite, thus can effectively reduces brittlement phase graphite and be contacted with the direct of Argent grain, improves the mechanics of material Physical property and processing characteristics;Meanwhile the Argent grain more disperse that decomposition in situ is formed is uniform so that materials microstructure is also more Disperse is uniform.
In the step 1) of above-mentioned preparation method, the particle mean size of the carbonic acid silver powder is preferably 5~8 μm, graphite powder Particle mean size is preferably 3~6 μm.
In the step 2) of above-mentioned preparation method, the mixed powder operation of the silver carbonate and graphite powder is same as the prior art, leads to It is often in V-type blender or double cone mixer progress, preferably stirs 1~4h under conditions of rotating speed is 20~40r/min.
In the step 3) of above-mentioned preparation method, described isostatic pressing and baking operation with existing routine operation phase Together, specifically, the briquetting pressure of isostatic pressing is usually 100~150MPa;The vacuum baking, typically by isostatic pressed into Silver carbonate graphite billet after type is placed in vacuum 2~4h of roasting under 150~300 DEG C of temperature conditionss, to obtain silver-colored graphite base Ingot.
In the step 4) of above-mentioned preparation method, described sintering and Decarburization Operation are identical with existing routine operation, generally It is step 3) is obtained into silver-colored graphite billet to be placed in vacuum or hydrogen or inert gas to sinter 4 under 880~920 DEG C of temperature conditionss ~8h;Silver-colored graphite billet after sintering is placed in air 1~3h of decarburization under 600~700 DEG C of temperature conditionss, to obtain outside spindle Wrap up the silver-colored graphite billet of silver layer in side.
In the step 5) of above-mentioned preparation method, the operation such as described hot extrusion is identical with existing routine operation, specifically, The temperature of hot extrusion is usually 800~900 DEG C, and extrusion ratio is 10~200.When will on the outside of spindle parcel silver layer silver-colored graphite billet When band is processed into hot extrusion, gained band by existing common process repeatedly roll, anneals and (protected in hydrogen or inert gas Under shield) obtain needed for after size again through punch press punching press, obtain the silver-graphite electrical contact material of sheet.
Compared with prior art, the method have the characteristics that:
1st, decomposition in situ reaction occurs during vacuum baking for silver carbonate in the method for the invention, during this, Silver carbonate can occur decomposition in situ as medium using graphite and form Argent grain so that a part of Argent grain is inhaled by decomposing diffusion It is attached on the surface of graphite, is contacted so as to effectively reduce brittlement phase graphite with the direct of Argent grain, and then improve the mechanics of material Physical property and processing characteristics.
2nd, because when silver carbonate occurs decomposition in situ the Argent grain more disperse that is formed it is uniform so that materials microstructure is also more Disperse is uniform, so as to have excellent mechanical and physical character and processing characteristics.
3rd, preparation method technique is simple, is adapted to industrial production.
Brief description of the drawings
Fig. 1 is the metallographic structure figure (500 ×) of contact material made from the embodiment of the present invention 1;
Fig. 2 is the metallographic structure figure (500 ×) of contact material made from the embodiment of the present invention 2;
Fig. 3 is the metallographic structure figure (500 ×) of contact material made from the embodiment of the present invention 3.
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
1) it is first according to prepare the silver carbonate (Ag needed for the calculating of 10kgAg-1C material mixture ratios2CO3) powder and graphite powder (C) Dosage, carbonic acid silver powder (particle mean size is 6 μm) 12.65kg, graphite powder (particle mean size is 5 μm) 0.1kg are weighed, it is standby;
2) above-mentioned carbonic acid silver powder and graphite powder are subjected to mixed powder on bipyramid blender, rotating speed 25r/min, time 2h, Obtain silver carbonate graphite (Ag2CO3C) mixed powder;
3) the silver carbonate graphite mixed powder after above-mentioned mixed powder is molded on isostatic pressing machine, briquetting pressure 120MPa, and Silver carbonate graphite billet after shaping is placed in vacuum with 150 DEG C of temperature calcination 4h, obtains silver-colored graphite (AgC) billet;
4) the silver-colored graphite billet for obtaining above-mentioned roasting is placed in hydrogen (H2) 8h are sintered with 880 DEG C of temperature in atmosphere;
5) the silver-colored graphite billet after above-mentioned sintering is subjected to decarburization in atmosphere, decarburization temperature is 650 DEG C, and decarburization time is 1h, obtain silver-colored graphite (AgC/Ag) billet of parcel silver layer on the outside of spindle;
6) by the silver-colored graphite billet of parcel silver layer on the outside of the spindle after above-mentioned decarburization, hot extrusion adds under hydrogen atmosphere protection For work into band, extrusion temperature is 850 DEG C, and mold preheating temperature is 150 DEG C, extrusion ratio 200;By band by repeatedly rolling System, annealing use punch press punching press slabbing silver graphite (AgC) contact after arriving required size (in hydrogen atmosphere).
Metallographic structure analysis is carried out to gained contact material, as shown in figure 1, result shows the technical scheme system of using Graphite particle is evenly distributed in silver matrix material in standby Ag-1C materials.
Embodiment 2
1) it is first according to prepare the silver carbonate (Ag needed for the calculating of 10kgAg-6C material mixture ratios2CO3) and graphite powder (C) use Amount, weighs carbonic acid silver powder (particle mean size is 6 μm) 12.01kg, graphite powder (particle mean size is 5 μm) 0.6kg, standby;
2) above-mentioned carbonic acid silver powder and graphite powder are subjected to mixed powder on bipyramid blender, rotating speed 25r/min, time 2h, Obtain silver carbonate graphite (Ag2CO3C) mixed powder;
3) the silver carbonate graphite mixed powder after above-mentioned mixed powder is molded on isostatic pressing machine, briquetting pressure 150MPa, and Silver carbonate graphite billet after shaping is placed in vacuum with 250 DEG C of temperature calcination 4h, obtains silver-colored graphite (AgC) billet;
4) the silver-colored graphite billet for obtaining above-mentioned roasting is placed in hydrogen (H2) 4h are sintered with 920 DEG C of temperature in atmosphere;
5) the silver-colored graphite billet after above-mentioned sintering is subjected to decarburization in atmosphere, decarburization temperature is 620 DEG C, and decarburization time is 1.5h, obtain silver-colored graphite (AgC/Ag) billet of parcel silver layer on the outside of spindle;
6) by the silver-colored graphite billet of parcel silver layer on the outside of the spindle after above-mentioned decarburization, hot extrusion adds under hydrogen atmosphere protection For work into band, extrusion temperature is 880 DEG C, and mold preheating temperature is 150 DEG C, extrusion ratio 200;By band by repeatedly rolling System, annealing use punch press punching press slabbing silver graphite (AgC) contact after arriving required size (in hydrogen atmosphere).
Metallographic structure analysis is carried out to gained contact material, as shown in Fig. 2 result shows the technical scheme system of using Graphite particle is evenly distributed in silver matrix material in standby Ag-6C materials.
Embodiment 3
1) it is first according to prepare the silver carbonate (Ag needed for the calculating of 10kgAg-5C material mixture ratios2CO3) and graphite powder (C) use Amount, weighs carbonic acid silver powder (particle mean size is 6 μm) 12.14kg, graphite powder (particle mean size is 5 μm) 0.5kg, standby;
2) above-mentioned carbonic acid silver powder and graphite powder are subjected to mixed powder on bipyramid blender, rotating speed 40r/min, time 2h, Obtain silver carbonate graphite (Ag2CO3C) mixed powder;
3) the silver carbonate graphite mixed powder after above-mentioned mixed powder is molded on isostatic pressing machine, briquetting pressure 100MPa, and Silver carbonate graphite billet after shaping is placed in vacuum with 280 DEG C of temperature calcination 2h, obtains silver-colored graphite (AgC) billet;
4) the silver-colored graphite billet for obtaining above-mentioned roasting is placed in hydrogen (H2) 5h are sintered with 900 DEG C of temperature in atmosphere;
5) the silver-colored graphite billet after above-mentioned sintering is subjected to decarburization in atmosphere, decarburization temperature is 700 DEG C, and decarburization time is 1h, obtain silver-colored graphite (AgC/Ag) billet of parcel silver layer on the outside of spindle;
6) by the silver-colored graphite billet of parcel silver layer on the outside of the spindle after above-mentioned decarburization, hot extrusion adds under hydrogen atmosphere protection For work into band, extrusion temperature is 850 DEG C, and mold preheating temperature is 150 DEG C, extrusion ratio 200;Gained band is in hydrogen shield Repeatedly rolled in atmosphere, be annealed to after required size and process slabbing silver graphite (AgC) contact with punch press.
Metallographic structure analysis is carried out to gained contact material, as shown in figure 3, result shows the technical scheme system of using Graphite particle is evenly distributed in silver matrix material in standby Ag-5C materials.
Contact material made from embodiment 3 is subjected to performance detection, and silver-colored stone made from powder-extrusion is mixed with existing routine Black contact product is compared, as a result as shown in following Tables 1 and 2s:
Table 1:Embodiment 3 mixes the properties of product of powder-extrusion preparation with existing routine
Table 2:Embodiment 3 mixes the electric life of blade contact prepared by powder-extrusion with existing routine
From Tables 1 and 2, the performance of silver-colored graphite contact material prepared by technical scheme is mixed better than existing routine Silver-colored graphite contact material performance prepared by powder-extrusion.

Claims (4)

1. a kind of preparation method of sheet silver-graphite electrical contact material, it is characterised in that comprise the following steps:
1) use of required graphite powder and carbonic acid silver powder is calculated according to the material mixture ratio of the silver-graphite electrical contact of required preparation Amount, is weighed standby;
2) take carbonic acid silver powder to carry out mixed powder with graphite powder, obtain silver carbonate graphite mixed powder;
3) be placed in after gained silver carbonate graphite mixed powder isostatic pressing in vacuum under 150~300 DEG C of temperature conditionss roasting 2~ 4h, obtain silver-colored graphite billet;
4) the silver-colored graphite billet of gained, which is placed in vacuum or hydrogen or inert gas, sinters, and is placed in again in air carries out decarburization afterwards, Obtain the silver-colored graphite billet of parcel silver layer on the outside of spindle;
5) the silver-colored graphite billet of parcel silver layer is processed into band under hydrogen or inert gas shielding through hot extrusion on the outside of gained spindle Material, rolled again afterwards, then stamped processing, obtain sheet silver-graphite electrical contact.
2. preparation method according to claim 1, it is characterised in that:, it is necessary to the silver-graphite electrical contact prepared in step 1) In material, content of graphite is 1~6wt%, and surplus is silver.
3. preparation method according to claim 1, it is characterised in that:The particle mean size of the carbonic acid silver powder is 5~8 μ m。
4. preparation method according to claim 1, it is characterised in that:The particle mean size of the graphite powder is 3~5 μm.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106098443B (en) * 2016-08-13 2019-02-01 福达合金材料股份有限公司 A kind of preparation process of high ratio of brazing area vertical fibers silver graphite electric contact
CN108067612B (en) * 2017-12-15 2019-09-06 桂林金格电工电子材料科技有限公司 A kind of preparation process of solderable sheet parallel construction silver graphite contact
CN107999747B (en) * 2017-12-15 2019-09-06 桂林金格电工电子材料科技有限公司 A kind of preparation method of the solderable band-like contact material of parallel construction silver graphite
CN113284767B (en) * 2021-04-23 2022-05-27 浙江福达合金材料科技有限公司 Preparation method of silver graphite electrical contact with continuous pure silver layer on side surface
CN113500170B (en) * 2021-07-13 2023-05-05 桂林金格电工电子材料科技有限公司 Method for mixed recycling of silver tin oxide indium oxide waste and silver graphite waste
CN114453584A (en) * 2021-12-28 2022-05-10 温州中希电工合金有限公司 Preparation method of silver graphite electrical contact material
CN115246737B (en) * 2022-08-09 2023-05-26 中钢集团南京新材料研究院有限公司 Roasting method for preparing isostatic pressing graphite product and product thereof

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1396025A (en) * 2002-07-02 2003-02-12 华东师范大学 Process for preparing electric silver/graphite contact material by nano technique

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1396025A (en) * 2002-07-02 2003-02-12 华东师范大学 Process for preparing electric silver/graphite contact material by nano technique

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