CN105551859A - Preparation method of flake silver graphite electrical contact material - Google Patents

Preparation method of flake silver graphite electrical contact material Download PDF

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Publication number
CN105551859A
CN105551859A CN201511009658.XA CN201511009658A CN105551859A CN 105551859 A CN105551859 A CN 105551859A CN 201511009658 A CN201511009658 A CN 201511009658A CN 105551859 A CN105551859 A CN 105551859A
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silver
graphite
powder
electrical contact
preparation
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CN105551859B (en
Inventor
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

Abstract

The invention discloses a preparation method of a flake silver graphite electrical contact material. Particularly, the method comprises the following steps: calculating required graphite powder and silver carbonate powder according to the material proportions for a to-be-prepared silver graphite electrical contact, and weighing the graphite powder and the silver carbonate powder for later use; mixing the silver carbonate powder with the graphite powder, and obtaining a silver graphite billet coated with a silver layer at the outer side of the billet from the obtained silver carbonate and graphite mixed powder through the procedures of molding, roasting, sintering and decarbonizing; and further processing the silver graphite billet into strips through hot extrusion, and carrying out rolling and stamping to obtain the flake silver graphite electrical contact. According to the method disclosed by the invention, direct contact of brittle phase graphite and silver particles can be effectively reduced; mechanical and physical properties and the processability of the prepared product are relatively excellent; and a metallographic structure is relatively uniform.

Description

A kind of preparation method of sheet silver-graphite electrical contact material
Technical field
The present invention relates to electrical contact material, be specifically related to a kind of preparation method of sheet silver-graphite electrical contact material.
Background technology
Silver-graphite electrical contact is owing to having excellent heat-conductivity conducting performance and resistance fusion welding energy and being widely used in the low-voltage electrical apparatuses such as miniature circuit breaker, line protection switch, failure current protection switch.As a rule, the preparation method of silver-graphite electrical contact material mainly contains powder mixing method and electroless plating method two kinds.
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, the method adopts mechanical mixture mode that silver powder, graphite powder are mixed, then mixed powder is carried out 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, and silver is mainly distributed between Argent grain when carrying out powder mixing machine, brittlement phase graphite is directly contacted with Argent grain, thus affects drawing abillity.Electroless plating method refers to graphite powder to join in liquor argenti nitratis ophthalmicus and forms aaerosol solution, then adds reducing agent and obtains silver-colored graphite coat powder, and through a series of processing such as cleaning, oven dry, isostatic pressed, sintering, extruding, finally obtains silver-graphite electrical contact.The shortcoming of this kind of method is that graphite powder not easily fully disperses in liquor argenti nitratis ophthalmicus, in material structure, easily occurs that graphite is assembled, affect materials microstructure performance, and meanwhile, this kind of method complicated process of preparation, the process-cycle is long, and production cost is relatively high.Therefore, how under the prerequisite ensureing material property and not obvious increase cost, prepare the silver-colored graphite material that structure property is excellent, become difficult point and the focus of research at present.
Publication number is that the patent of invention of CN101763956A discloses a kind of silver-graphite electrical contact material and preparation method thereof.First the method is that graphite and ceramic composite powder, reducing agent, deionized water are made reduction suspension, then joined in silver ammino solution, obtain silver-plated graphite ceramic composite powder, finally silver-rare earth alloy powder obtained with water atomization for silver-plated graphite ceramic composite powder is mixed, obtain silver-graphite electrical contact material.The deficiency of this technology is that graphite not easily fully disperses in reduction suspension, thus affects the metallographic structure of material.
Publication number is that the patent of invention of CN1234591A discloses a kind of method for preparing silver-graphite electrical contact belt.The method is that spherical graphite powder and cebollite ink powder are mixed powder according to a certain percentage with atomization silver powder and chemical silver powder, then through overmolding, sintering, and extrude wrap up one deck silver layer outside silver-colored graphite spindle after, obtain the silver-colored graphite tape of silver-coated layer, eventually pass rolling, cover the operation such as solder, annealing after obtain silver-graphite electrical contact belt finished product.There is the problem that brittlement phase graphite directly contacts with Argent grain equally in this invention.
Summary of the invention
For the deficiency that prior art exists, the invention provides a kind of preparation method of new sheet silver-graphite electrical contact material, propose with decomposition in situ legal system for silver-graphite electrical contact material, adopt the method for the invention effectively can reduce brittlement phase graphite to contact with the direct of Argent grain, make products obtained therefrom have excellent mechanical and physical character and processing characteristics, metallographic structure is simultaneously more even.
The preparation method of sheet silver-graphite electrical contact material of the present invention, comprises the following steps:
1) calculate according to the material mixture ratio of the silver-graphite electrical contact of required preparation needed for graphite powder and the consumption of silver carbonate powder, take for subsequent use;
2) get silver carbonate powder and graphite powder carries out mixed powder, obtain silver carbonate graphite mixed powder;
3) gained silver carbonate graphite mixed powder isostatic compaction is placed on roasting in vacuum, obtains silver-colored graphite billet;
4) gained silver graphite billet is placed in vacuum or hydrogen or inert gas and sinters, and is placed in air afterwards again and carries out decarburization, obtain the silver-colored graphite billet wrapping up silver layer outside spindle;
5) the silver-colored graphite billet wrapping up silver layer outside gained spindle is processed into band through hot extrusion under hydrogen or inert gas shielding, is rolled afterwards again, then through punch process, obtains sheet silver-graphite electrical contact.
The present invention adopts silver carbonate and graphite powder to carry out mixed powder, and the silver carbonate graphite billet after shaping obtains silver-colored graphite billet after the operation such as roasting, sintering.Because decomposition in situ reaction can occur silver carbonate in vacuum baking process, in this process, silver carbonate can be that medium generation decomposition in situ forms Argent grain with graphite, a part of Argent grain is made to be adsorbed on the surface of graphite by decomposing diffusion, thus effectively can reduce brittlement phase graphite to contact with the direct of Argent grain, improve mechanical and physical character and the processing characteristics of material; Meanwhile, the Argent grain that decomposition in situ is formed more disperse is even, and also disperse is even more to make materials microstructure.
The step 1 of above-mentioned preparation method) in, the particle mean size of described silver carbonate powder is preferably 5 ~ 8 μm, and the particle mean size of graphite powder is preferably 3 ~ 6 μm.
The step 2 of above-mentioned preparation method) in, the mixed powder of described silver carbonate and graphite powder operates same as the prior art, normally carries out at V-type blender or double cone mixer, preferably under rotating speed is the condition of 20 ~ 40r/min, stirs 1 ~ 4h.
The step 3 of above-mentioned preparation method) in, described isostatic compaction and baking operation are all identical with existing routine operation, and particularly, the briquetting pressure of isostatic compaction is generally 100 ~ 150MPa; Described vacuum baking, is normally placed in vacuum roasting 2 ~ 4h under 150 ~ 300 DEG C of temperature conditions by the silver carbonate graphite billet after isostatic compaction, to obtain silver-colored graphite billet.
The step 4 of above-mentioned preparation method) in, described sintering and Decarburization Operation are all identical with existing routine operation, normally by step 3) obtain silver-colored graphite billet and be placed in vacuum or hydrogen or inert gas sinter 4 ~ 8h under 880 ~ 920 DEG C of temperature conditions; Silver-colored graphite billet after sintering is placed in air decarburization 1 ~ 3h under 600 ~ 700 DEG C of temperature conditions, to obtain the silver-colored graphite billet wrapping up silver layer outside spindle.
The step 5 of above-mentioned preparation method) in, the operation such as described hot extrusion is all identical with existing routine operation, and particularly, the temperature of hot extrusion is generally 800 ~ 900 DEG C, and extrusion ratio is 10 ~ 200.When band is processed in the silver-colored graphite billet hot extrusion of wrapping up silver layer outside spindle; gained band carries out repeatedly rolling by existing common process, annealing (under hydrogen or inert gas shielding) obtain required size after again through punch ram, obtain the silver-graphite electrical contact material of sheet.
Compared with prior art, feature of the present invention is:
1, in the method for the invention there is decomposition in situ reaction in silver carbonate in vacuum baking process, in this process, silver carbonate can be that medium generation decomposition in situ forms Argent grain with graphite, a part of Argent grain is made to be adsorbed on the surface of graphite by decomposing diffusion, thus effectively minimizing brittlement phase graphite contacts with the direct of Argent grain, and then improve mechanical and physical character and the processing characteristics of material.
2, because of the Argent grain that formed during silver carbonate generation decomposition in situ, disperse is even more, and also disperse is even more to make materials microstructure, thus has excellent mechanical and physical character and processing characteristics.
3, preparation method's technique is simple, is applicable to industrial production.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure (500 ×) of the contact material that the embodiment of the present invention 1 obtains;
Fig. 2 is the metallographic structure figure (500 ×) of the contact material that the embodiment of the present invention 2 obtains;
Fig. 3 is the metallographic structure figure (500 ×) of the contact material that the embodiment of the present invention 3 obtains.
Embodiment
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
1) first according to the silver carbonate (Ag needed for the calculating of preparation 10kgAg-1C material mixture ratio 2cO 3) powder and graphite powder (C) consumption, take silver carbonate powder (particle mean size is 6 μm) 12.65kg, graphite powder (particle mean size is 5 μm) 0.1kg, for subsequent use;
2) above-mentioned silver carbonate powder and graphite powder are carried out mixed powder on bipyramid blender, rotating speed 25r/min, time 2h, obtain silver carbonate graphite (Ag 2cO 3c) mixed powder;
3) by shaping on isostatic pressing machine for the silver carbonate graphite mixed powder after above-mentioned mixed powder, briquetting pressure is 120MPa, and the 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 above-mentioned roasting obtained is placed in hydrogen (H 2) in atmosphere with 880 DEG C of temperature sintering 8h;
5) the silver-colored graphite billet after above-mentioned sintering is carried out decarburization in atmosphere, decarburization temperature is 650 DEG C, and decarburization time is 1h, obtains silver-colored graphite (AgC/Ag) billet wrapping up silver layer outside spindle;
6) band is processed in silver-colored graphite billet hot extrusion under hydrogen atmosphere protection of wrapping up silver layer outside the spindle after above-mentioned decarburization, extrusion temperature is 850 DEG C, and mold preheating temperature is 150 DEG C, and extrusion ratio is 200; Band is used after repeatedly rolling, annealing (in hydrogen atmosphere) to required size punch ram slabbing silver graphite (AgC) contact.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 1, in the Ag-1C material that result display adopts technical scheme to prepare, graphite granule is evenly distributed in silver matrix material.
Embodiment 2
1) first according to the silver carbonate (Ag needed for the calculating of preparation 10kgAg-6C material mixture ratio 2cO 3) and graphite powder (C) consumption, take silver carbonate powder (particle mean size is 6 μm) 12.01kg, graphite powder (particle mean size is 5 μm) 0.6kg, for subsequent use;
2) above-mentioned silver carbonate powder and graphite powder are carried out mixed powder on bipyramid blender, rotating speed 25r/min, time 2h, obtain silver carbonate graphite (Ag 2cO 3c) mixed powder;
3) by shaping on isostatic pressing machine for the silver carbonate graphite mixed powder after above-mentioned mixed powder, briquetting pressure is 150MPa, and the 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 above-mentioned roasting obtained is placed in hydrogen (H 2) in atmosphere with 920 DEG C of temperature sintering 4h;
5) the silver-colored graphite billet after above-mentioned sintering is carried out decarburization in atmosphere, decarburization temperature is 620 DEG C, and decarburization time is 1.5h, obtains silver-colored graphite (AgC/Ag) billet wrapping up silver layer outside spindle;
6) band is processed in silver-colored graphite billet hot extrusion under hydrogen atmosphere protection of wrapping up silver layer outside the spindle after above-mentioned decarburization, extrusion temperature is 880 DEG C, and mold preheating temperature is 150 DEG C, and extrusion ratio is 200; Band is used after repeatedly rolling, annealing (in hydrogen atmosphere) to required size punch ram slabbing silver graphite (AgC) contact.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 2, in the Ag-6C material that result display adopts technical scheme to prepare, graphite granule is evenly distributed in silver matrix material.
Embodiment 3
1) first according to the silver carbonate (Ag needed for the calculating of preparation 10kgAg-5C material mixture ratio 2cO 3) and graphite powder (C) consumption, take silver carbonate powder (particle mean size is 6 μm) 12.14kg, graphite powder (particle mean size is 5 μm) 0.5kg, for subsequent use;
2) above-mentioned silver carbonate powder and graphite powder are carried out mixed powder on bipyramid blender, rotating speed 40r/min, time 2h, obtain silver carbonate graphite (Ag 2cO 3c) mixed powder;
3) by shaping on isostatic pressing machine for the silver carbonate graphite mixed powder after above-mentioned mixed powder, briquetting pressure is 100MPa, and the 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 above-mentioned roasting obtained is placed in hydrogen (H 2) in atmosphere with 900 DEG C of temperature sintering 5h;
5) the silver-colored graphite billet after above-mentioned sintering is carried out decarburization in atmosphere, decarburization temperature is 700 DEG C, and decarburization time is 1h, obtains silver-colored graphite (AgC/Ag) billet wrapping up silver layer outside spindle;
6) band is processed in silver-colored graphite billet hot extrusion under hydrogen atmosphere protection of wrapping up silver layer outside the spindle after above-mentioned decarburization, extrusion temperature is 850 DEG C, and mold preheating temperature is 150 DEG C, and extrusion ratio is 200; The repeatedly rolling in hydrogen shield atmosphere of gained band, be annealed to required size after with punch press be processed into sheet silver graphite (AgC) contact.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 3, in the Ag-5C material that result display adopts technical scheme to prepare, graphite granule is evenly distributed in silver matrix material.
Contact material obtained for embodiment 3 is carried out Performance Detection, and compares with the silver-colored graphite contact product that existing routine mixes powder-extrusion obtained, result is as shown in following table 1 and table 2:
Table 1: embodiment 3 and existing routine mix properties of product prepared by powder-extrusion
Table 2: embodiment 3 and existing routine mix the electric life of blade contact prepared by powder-extrusion
From table 1 and table 2, the performance of silver-colored graphite contact material prepared by technical scheme is better than existing routine and mixes silver-colored graphite contact material performance prepared by powder-extrusion.

Claims (4)

1. a preparation method for sheet silver-graphite electrical contact material, is characterized in that comprising the following steps:
1) calculate according to the material mixture ratio of the silver-graphite electrical contact of required preparation needed for graphite powder and the consumption of silver carbonate powder, take for subsequent use;
2) get silver carbonate powder and graphite powder carries out mixed powder, obtain silver carbonate graphite mixed powder;
3) gained silver carbonate graphite mixed powder isostatic compaction is placed on roasting in vacuum, obtains silver-colored graphite billet;
4) gained silver graphite billet is placed in vacuum or hydrogen or inert gas and sinters, and is placed in air afterwards again and carries out decarburization, obtain the silver-colored graphite billet wrapping up silver layer outside spindle;
5) the silver-colored graphite billet wrapping up silver layer outside gained spindle is processed into band through hot extrusion under hydrogen or inert gas shielding, is rolled afterwards again, then through punch process, obtains sheet silver-graphite electrical contact.
2. preparation method according to claim 1, is characterized in that: step 1) in, need in the silver-graphite electrical contact material of preparation, content of graphite is 1 ~ 6wt%, and surplus is silver.
3. preparation method according to claim 1, is characterized in that: the particle mean size of described silver carbonate powder is 5 ~ 8 μm.
4. preparation method according to claim 1, is characterized in that: the particle mean size of described graphite powder is 3 ~ 5 μm.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106098443A (en) * 2016-08-13 2016-11-09 福达合金材料股份有限公司 A kind of preparation technology of high ratio of brazing area vertical fibers silver graphite electric contact
CN107999747A (en) * 2017-12-15 2018-05-08 桂林金格电工电子材料科技有限公司 A kind of preparation method of high solderability parallel construction silver graphite banding contact material
CN108067612A (en) * 2017-12-15 2018-05-25 桂林金格电工电子材料科技有限公司 A kind of preparation process of high solderability sheet parallel construction silver graphite contact
CN113284767A (en) * 2021-04-23 2021-08-20 福达合金材料股份有限公司 Preparation method of silver graphite electrical contact with continuous pure silver layer on side surface
CN113500170A (en) * 2021-07-13 2021-10-15 桂林金格电工电子材料科技有限公司 Method for mixing and recycling 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
CN115246737A (en) * 2022-08-09 2022-10-28 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

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106098443A (en) * 2016-08-13 2016-11-09 福达合金材料股份有限公司 A kind of preparation technology of high ratio of brazing area vertical fibers silver graphite electric contact
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
CN107999747A (en) * 2017-12-15 2018-05-08 桂林金格电工电子材料科技有限公司 A kind of preparation method of high solderability parallel construction silver graphite banding contact material
CN108067612A (en) * 2017-12-15 2018-05-25 桂林金格电工电子材料科技有限公司 A kind of preparation process of high solderability sheet parallel construction silver graphite 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
CN113284767A (en) * 2021-04-23 2021-08-20 福达合金材料股份有限公司 Preparation method of silver graphite electrical contact with continuous pure silver layer on side surface
CN113500170A (en) * 2021-07-13 2021-10-15 桂林金格电工电子材料科技有限公司 Method for mixing and recycling silver tin oxide indium oxide waste and silver graphite waste
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
CN115246737A (en) * 2022-08-09 2022-10-28 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
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

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