CN102808097B - Silver/nickel/metallic oxide electrical contact material preparation method - Google Patents
Silver/nickel/metallic oxide electrical contact material preparation method Download PDFInfo
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- CN102808097B CN102808097B CN201210296608.4A CN201210296608A CN102808097B CN 102808097 B CN102808097 B CN 102808097B CN 201210296608 A CN201210296608 A CN 201210296608A CN 102808097 B CN102808097 B CN 102808097B
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Abstract
The invention discloses a silver/nickel/metallic oxide electrical contact material preparation method including the steps: cladding a metallic nickel layer on metallic oxide particles by means of chemical plating; cladding a silver layer on nickel-clad metallic oxides by means of chemical plating; sintering and granulating clad powder of an Ag-Ni-MeO core-shell structure under the protection of nitrogen to obtain intermediate composite particle powder bodies prior to screening; mixing intermediate composite particles with pure silver powder, and lowering the content of the metallic oxides to a set numerical value; and after the processes of powder pressing, protective atmosphere sintering, extrusion and drawing, obtaining novel silver/nickel/metallic oxide materials in funicular distribution in a local area of metallic oxide particles in silver/nickel/metallic oxide materials, and the local area mainly includes metallic nickel and a small quantity of metallic silver except for metallic oxide reinforced-phase particles.
Description
Technical field
What the present invention relates to is a kind of contact material, and specifically, that relate to is the preparation method of a kind of silver/nickel/metal oxide contact material.
Background technology
Ag-based electrical contact is the core parts of electric switch, and it is undertaking the task of the connecting and disconnecting between circuit, is widely used in the low-voltage apparatuses such as all kinds of air switches, rly., AC/DC contactor.In recent years, along with improving constantly of industrial application level and cost performance demand, constantly there are new preparation technology and silver-base electric contact composite material to release.
Through the retrieval of prior art is found, the mandate patent of invention (201010579827.4 of bulletin in 2011, the preparation method of particle-aligned reinforced silver based contact material) in the intermediate composite particles of the coated legal system of a kind of electroless plating for the coated wild phase particle of Ag disclosed, intermediate composite particles is further mixed with fine silver powder, wild phase content is reduced to finished product content, by techniques such as mixed powder, compacting, sintering, hot extrusions, obtain wild phase particle and in matrix, be fibrous Novel electrical contact material of arranging.
Traditional powder metallurgical technique generally mixes disposable to wild phase powder and silver powder, due to the reason of wild phase diameter of particle distribution, cause the undue disperse of ultra-fine wild phase powder of significant proportion in silver matrix, thereby reduce electric conductivity and the unit elongation of contact material.The know-why of above document (patent of invention 201010579827.4) be by material electric property and mechanical property are had dysgenic wild phase particle with fibrous formal constraint of arranging at regional area, thereby improved electric conductivity and the unit elongation of material.The silver of this regional area is only the effect of having played wild phase carrier, and electroconductibility and the unit elongation contribution to integral material of noble silver is wherein comparatively limited.
Further literature search is found, the main contriver of foregoing invention patent electrically contacted in international conference (ICEC2012) and delivered and be entitled as " Ag/ (SnO at the 26th in May, 2012
2) 12Electrical Contact Material with Fibre-like Arrangement of Reinforcing Nanoparticles:Preparation, Formation Mechanism, and Properties " research article; introduced preparation method and material property based on similar principles, specifically described and utilized the method for mechanical alloying to prepare SnO
2content is 60% Ag/ (SnO
2) intermediate composite particles, by Ag/ (SnO
2) intermediate composite particles mixes according to the ratio of 1: 4 with pure Ag powder, makes SnO
2content reduces to 12%, follow-up by techniques such as compacting, sintering and hot extrusions, obtains SnO
2in silver matrix, be the fibrous new A g/ (SnO arranging
2) environmental protection electric contact material.Compared with prior powder metallurgy technique, resistivity is down to 2.08 μ Ω cm from 2.31 μ Ω cm, and unit elongation is increased to 24% by 7%.
Summary of the invention
The present invention is on the basis of above technical literature principle, the preparation method of a kind of silver/nickel/metal oxide contact material is provided, original silver/metal oxide preparation technology is improved, adopt nickel to replace the carrier of noble silver as metal oxide wild phase, prepare nickel/metal oxide intermediate composite particles, thereby metal oxide is constrained in intermediate composite particles, avoid the disadvantageous effect of super-fine metal oxide powder to contact material performance, then this intermediate composite particles is mixed with fine silver powder, repressed, sintering, the techniques such as extruding and drawing, obtain Novel silver/nickel/metal oxide materials that the coated metal oxide particle of nickel is fibrous distribution in material.
The present invention is achieved by the following technical solutions: the present invention adopts the method for electroless plating, to metal oxide clad metal nickel, and then coated with silver, the composite granule of formation Ag-Ni-MeO nucleocapsid structure.The composite granule obtaining is carried out to the granulation of protective atmosphere sintering; obtain the intermediate composite particles of high metal oxide content and high nickel content; intermediate composite particles is mixed with fine silver powder; through techniques such as compacting, sintering, extruding and drawings, make the coated metal oxide particle of nickel in material, be fibrous distribution.
Aforesaid method concrete steps of the present invention are as follows:
The first step, adopts the method for electroless plating to make metal oxide particle be coated layer of metal nickel;
Second step, adopts the method for electroless plating to be coated the further coated one deck silver of metal oxide particle after nickel to the first step;
The 3rd step, adopts nitrogen protection to carry out sintering granulation to the powder of the coated rear Ag-Ni-MeO nucleocapsid structure forming of second step, obtains intermediate composite particles powder, then screening;
The 4th step, mixes the intermediate composite particles after the 3rd step screening with fine silver powder, lower the content of metal oxide to setting numerical value;
The 5th step; the pressed by powder that the 4th step is mixed; nitrogen protection atmosphere sintering; again through extruding, drawing; obtain metal oxide particle is fibrous distribution Novel silver/nickel/metal oxide contact material at regional area; and this regional area is except metal oxide wild phase, be mainly metallic nickel and a small amount of argent.
Aforesaid method:
In the first step, adopting the weight in average degree of metal oxide in the powder after the coated nickel of electroless plating is 40%～80%, and the weight in average degree of nickel is 20%～60%.
In second step, adopt the weight in average degree of silver in the powder after electroless plating coated with silver to be less than 10%.
In the 3rd step, adopt nitrogen protection to carry out sintering granulation to the powder of the Ag-Ni-MeO nucleocapsid structure forming after coated, the temperature of sintering is 700 ℃～800 ℃.
In the 3rd step, by the intermediate composite particles powder screening obtaining, continue to employ granularity for-100 orders～+ 400 order.
In the 4th step, intermediate composite particles is mixed with fine silver powder, the weight percent content of metal oxide is reduced to 8%～20%.
In aforesaid method of the present invention, described metal oxide is the metal oxide that can be applicable to contact material and realize above-mentioned purpose, and preferably, metal oxide includes but not limited to CdO, SnO
2, ZnO, CuO, Ni
2o, WO
3, and the mixture of these metal oxides.
Aforesaid method of the present invention; after the mixed powder of the 4th step and the 5th step, pressed by powder, protective atmosphere sintering, extruding, drawing process; in the silver/nickel/metal oxide contact material obtaining: metal oxide particle is fibrous distribution at regional area; be that fibrous tissue structure is aligned and formed by metal oxide particle; and this regional area is except metal oxide wild phase, be mainly metallic nickel and a small amount of argent.
The present invention adopts the method for electroless plating to the coated one deck nickel of metal oxide particle, and then coated with silver, form Ag-Ni-MeO nucleocapsid structure, improved the interface imbibition characteristic of metal oxide particle and silver matrix, eliminated in prior powder metallurgy method because of the poor disadvantageous effect to contact material mechanical property of interface imbibition characteristic.The more important thing is and replaced coated by metallic nickel the silver in intermediate composite particles in above document, thereby reduced silver-colored consumption.The coated Main Function of silver is improve the oxidation-resistance of intermediate composite particles and improve the performance of sintering granulation, and the deformability of intermediate composite particles in the course of processing, thereby improves processing performance.
Embodiment
Below embodiments of the invention are elaborated: the present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The present invention adopts the method for electroless plating, to the coated nickel of metal oxide particle, and then coated with silver, form the composite granule of Ag-Ni-MeO nucleocapsid structure, wherein chemical nickel plating and silver-plated method can adopt operation in following examples to realize, but be not limited to this operation, also can adopt the method for other existing electroless platings to realize.The inventive method the 4th step and the 5th step adopt respectively mixed powder of the prior art, pressed by powder, nitrogen protection atmosphere sintering, extruding, drawing process, are specifically not limited to operation and processing parameter in following examples.
Embodiment 1:
1. pair CdO powder adopts the coated one deck nickel of method of electroless plating, and making the average content (weight percent) of CdO in powder is 80%, and the weight in average degree of nickel is 20%; In the present embodiment, can adopt following technique to realize:
A) before plating, disperse: the quality of nanoparticulate dispersed effect is directly connected to distribution and the content of its particulate in composite deposite, and then directly has influence on the performance of composite deposite.Preferably, the present embodiment adopts sodium alginate (or Polyvinylpyrolidone (PVP)) to make dispersion agent.The concrete CdO nanoparticle that first soaks 12.5g with the dehydrated alcohol of 200mL; Then take the sodium alginate of 7.5g, be dissolved in 1L deionized water; Then will slowly join in sodium alginate soln by the wetting CdO nanoparticle of dehydrated alcohol, ultrasonic wave is disperseed and mechanical stirring, can obtain dispersion liquid;
B) sensitization and activation: by above-mentioned solution at the SnCl at 16g/L
22H O and 0.18g/L PdCl
2in colloidal pd activation solution, carry out sensitization and activation; In this process, Sn (OH) CL is by Pd
2+be reduced into Pd, Pd is adsorbed in matrix CdO surface and becomes the catalytic activation center of chemical nickel plating, filters, and cleans, stand-by.
C) reduction: adopt 30g/L NaH
2pO
32H
2o solution, puts into reduced liquid 3min by the CdO powder particle of activated processing, and reduction may residue in its surperficial Pd
2+, prevent that it from bringing into and in plating solution, cause plating solution to decompose, filter, obtain the CdO powder of surface with Pd, prepare chemical nickel plating;
D) chemical nickel plating: the above-mentioned CdO powder of handling well is slowly joined to (electroplate liquid formulation: single nickel salt 30g/L, sodium hypophosphite 25g/L, anhydrous sodium acetate 6g/L, Trisodium Citrate 5.5g/L, 65 ℃ of temperature, pH 4.5) in the 200mL chemical plating fluid configuring.Plating temperature is (83 ± 3) ℃, and the plating time is 90min.Then distilled water flushing, dries.
2, chemical silvering: the CdO to coated nickel further adopts electroless plating to be coated one deck silver, in coated rear powder, the weight in average degree of silver is less than 10%;
3, the Ag/Ni/CdO core-shell structured powder preparing is put into the granulation of nitrogen sintering oven sintering, sintering temperature is 700 ℃, after granulation, sieves, and removes fine particle, continues to employ the intermediate composite particles powder between the order of granularity-100 order～+ 400;
4, Ag/Ni/CdO intermediate composite particles powder screening being obtained mixes with fine silver powder, the CdO weight in average degree that makes to mix in rear powder is 20%, in the mixed powder machine of " V " type of then powder being poured into, evenly mixes powder, 30 revs/min of rotating speeds during mixed powder, 4 hours time;
5, the powder mixing being packed into diameter is 90cm, in length 150cm plastic cement cylinder, carries out isostatic cool pressing, isostatic cool pressing pressure 200Mpa;
6, the base substrate obtaining after isostatic cool pressing is carried out to nitrogen protection atmosphere sintering, 800 ℃ of sintering temperatures, sintering 5 hours;
7, the base substrate obtaining after sintering is carried out to hot pressing, 800 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 10min;
8, base substrate good hot pressing is carried out to hot extrusion, 600 ℃ of extrusion temperatures, extrusion ratio 180, extrusion speed 5cm/min, 500 ℃ of extrusion mould preheating temperatures;
The present embodiment finally obtains Cadmium oxide particle is fibrous distribution new A g/Ni/CdO contact material at regional area, and this regional area is except CdO wild phase, is mainly metallic nickel and a small amount of argent.The material obtaining is 3.9 μ Ω .cm along direction of extrusion resistivity; Hardness is 87HV.
Embodiment 2:
1. couple SnO
2the coated one deck nickel of method that adopts electroless plating, makes SnO in powder
2weight in average degree be 60%, the weight in average degree of nickel is 40%;
2. the SnO of pair coated nickel
2further adopt the coated one deck silver of electroless plating, in coated rear powder, the weight in average degree of silver is less than 10%; In the present embodiment, can adopt following existing techniques in realizing:
Ni-CdO powder is put into reduced liquid mechanical dispersed with stirring 5min, silver ammino solution is dropwise added drop-wise in reduced liquid and mechanical stirring with dropper, make silver ion reduction be deposited on Ni-CdO surface, clean up with deionized water, 50 ℃ of oven dry obtain has nucleocapsid structure Ag/Ni/CdO powder;
In the present embodiment, described silver ammino solution and reduced liquid were according to preparation respectively in 1: 1; The preparation of described 50ml reduced liquid: formaldehyde 1.1ml, adds water to 50ml; In the deionized water of the preparation of described 50ml silver ammino solution: 30ml, add 1.75g Silver Nitrate, after stirring and dissolving, add again people 10ml ammoniacal liquor and constantly stir, and improving pH value with appropriate NaOH solution, then adding water to 50ml.
3. couple Ag/Ni/SnO preparing
2core-shell structured powder is put into the granulation of nitrogen sintering oven sintering, and sintering temperature is 800 ℃, after granulation, sieves, and removes fine particle, continues to employ the intermediate composite particles powder between the order of granularity-100 order～+ 400;
4. Ag/Ni/SnO screening being obtained
2intermediate composite particles powder mixes with fine silver powder, makes to mix the SnO in rear powder
2weight in average degree is 12%, in the mixed powder machine of " V " type of then powder being poured into, evenly mixes powder;
5. the powder mixing being packed into diameter is 90cm, in length 150cm plastic cement cylinder, carries out isostatic cool pressing, isostatic cool pressing pressure 200Mpa;
6. the base substrate obtaining after isostatic cool pressing is carried out to nitrogen protection atmosphere sintering, 865 ℃ of sintering temperatures, sintering 5 hours;
7. the base substrate obtaining after sintering is carried out to hot pressing, 800 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 10min;
8. base substrate good hot pressing is carried out to hot extrusion, 600 ℃ of extrusion temperatures, extrusion ratio 180, extrusion speed 5cm/min, 500 ℃ of extrusion mould preheating temperatures;
The present embodiment finally obtains SnO
2particle is the new A g/Ni/SnO of fibrous distribution at regional area
2contact material, and this regional area is except SnO
2beyond wild phase, be mainly metallic nickel and a small amount of argent.The material obtaining is 3.0 μ Ω .cm along direction of extrusion resistivity; Hardness is 78HV.
Embodiment 3:
1. couple ZnO adopts the coated one deck nickel of method of electroless plating, and the weight in average degree that makes ZnO in powder is 40%, and the weight in average degree of nickel is 60%;
2. the ZnO of pair coated nickel further adopts electroless plating to be coated one deck silver, and in coated rear powder, the weight in average degree of silver is less than 10%;
3. pair Ag/Ni/ZnO core-shell structured powder preparing is put into the granulation of nitrogen sintering oven sintering, and sintering temperature is 700 ℃, after granulation, sieves, and removes fine particle, continues to employ the intermediate composite particles powder between the order of granularity-100 order～+ 400;
4. Ag/Ni/ZnO intermediate composite particles powder screening being obtained mixes with fine silver powder, the ZnO weight in average degree that makes to mix in rear powder is 10%, in the mixed powder machine of " V " type of then powder being poured into, evenly mixes powder, 30 revs/min of rotating speeds during mixed powder, 4 hours time;
5. the powder the 4th step being mixed, adopts prior art to carry out pressed by powder, nitrogen protection atmosphere sintering, then through extruding, drawing, obtain silver/nickel/metal oxide contact material.
The present embodiment finally obtains ZnO particle is fibrous distribution new A g/Ni/MeO contact material at regional area, and this regional area is except ZnO wild phase, is mainly metallic nickel and a small amount of argent.The material obtaining is 3.4 μ Ω .cm along direction of extrusion resistivity; Hardness is 75HV.
Embodiment 4:
1. couple SnO
2the coated one deck nickel of method that adopts electroless plating, makes SnO in powder
2weight in average degree be 50%, the weight in average degree of nickel is 50%;
2. the SnO of pair coated nickel
2further adopt the coated one deck silver of electroless plating, in coated rear powder, the weight in average degree of silver is less than 10%;
3. couple Ag/Ni/SnO preparing
2core-shell structured powder is put into the granulation of nitrogen sintering oven sintering, and sintering temperature is 800 ℃, after granulation, sieves, and removes fine particle, continues to employ the intermediate composite particles powder between the order of granularity-100 order～+ 400;
4. Ag/Ni/SnO screening being obtained
2intermediate composite particles powder mixes with fine silver powder, makes to mix the SnO in rear powder
2weight in average degree is 8%, in the mixed powder machine of " V " type of then powder being poured into, evenly mixes powder;
5. the powder the 4th step being mixed, carries out the cold compacting of Denging to powder, nitrogen protection atmosphere sintering, then through extruding, drawing, obtain silver/nickel/metal oxide contact material.
The present embodiment finally obtains SnO
2particle is the new A g/Ni/SnO of fibrous distribution at regional area
2contact material, and this regional area is except SnO
2beyond wild phase, be mainly metallic nickel and a small amount of argent.The material obtaining is 2.5 μ Ω .cm along direction of extrusion resistivity; Hardness is 70HV.
More than for part embodiment of the present invention, it should be pointed out that the present invention also has other embodiment, such as conversion is implemented parameter or replaced the respective operations in above-described embodiment by prior art.Although content of the present invention has been done detailed introduction by above-described embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.Those skilled in the art, read after foregoing, for multiple modification of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a preparation method for silver/nickel/metal oxide contact material, is characterized in that comprising the following steps:
The first step, adopts the method for electroless plating to make metal oxide particle be coated layer of metal nickel;
Second step, adopts the method for electroless plating to be coated the further coated one deck silver of metal oxide particle after nickel to the first step;
The 3rd step, adopts nitrogen protection to carry out sintering granulation to the powder of the coated rear Ag-Ni-MeO nucleocapsid structure forming of second step, obtains intermediate composite particles powder, and then screening, removed thick and meticulous particle;
The 4th step, mixes the intermediate composite particles after the 3rd step screening with fine silver powder, lower the content of metal oxide to setting numerical value;
The 5th step; the pressed by powder that the 4th step is mixed; protective atmosphere sintering; again through extruding, drawing; obtain metal oxide particle is fibrous distribution silver/nickel/metal oxide contact material at regional area; and this regional area is except metal oxide wild phase, be mainly metallic nickel and a small amount of argent.
2. the preparation method of silver/nickel as claimed in claim 1/metal oxide contact material, it is characterized in that, in the first step, adopting the average content of metal oxide in the powder after the coated nickel of electroless plating is 40%～80%, the average content of nickel is 20%～60%, and described content refers to weight percent content.
3. the preparation method of silver/nickel as claimed in claim 1/metal oxide contact material, is characterized in that, in second step, adopts the average content of silver in the powder after electroless plating coated with silver to be less than 10%, and described content refers to weight percent content.
4. the preparation method of silver/nickel as claimed in claim 1/metal oxide contact material, is characterized in that, in the 4th step, intermediate composite particles is mixed with fine silver powder, and the weight percent content of metal oxide is reduced to 8%～20%.
5. the preparation method of silver/nickel as claimed in claim 1/metal oxide contact material, it is characterized in that, in the first step, adopting the average content of metal oxide in the powder after the coated nickel of electroless plating is 40%～80%, and the average content of nickel is 20%～60%; In second step, adopt the average content of silver in the powder after electroless plating coated with silver to be less than 10%, described content refers to weight percent content.
6. the preparation method of silver/nickel as claimed in claim 1/metal oxide contact material, it is characterized in that, in the first step, adopting the average content of metal oxide in the powder after the coated nickel of electroless plating is 40%～80%, and the average content of nickel is 20%～60%; In second step, adopt the average content of silver in the powder after electroless plating coated with silver to be less than 10%; In the 4th step, intermediate composite particles is mixed with fine silver powder, the weight percent content of metal oxide is reduced to 8%～20%; Described content refers to weight percent content.
7. the preparation method of the silver/nickel/metal oxide contact material as described in claim 1-6 any one; it is characterized in that; in the 3rd step, adopt nitrogen protection to carry out sintering granulation to the powder of the Ag-Ni-MeO nucleocapsid structure forming after coated, the temperature of sintering is 700 ℃～800 ℃.
8. the preparation method of the silver/nickel/metal oxide contact material as described in claim 1-6 any one, is characterized in that, in the 3rd step, by the intermediate composite particles powder screening obtaining, continues to employ granularity for-100 orders～+ 400 order.
9. the preparation method of the silver/nickel/metal oxide contact material as described in claim 1-6 any one, is characterized in that, described metal oxide includes but not limited to CdO, SnO
2, ZnO, CuO, Ni
2o, WO
3, and the mixture of these metal oxides.
10. silver/nickel/metal oxide contact material that described in a claim 1-9, method obtains, it is characterized in that: in described silver/nickel/metal oxide contact material: metal oxide particle is fibrous distribution at regional area, be that fibrous tissue structure is aligned and formed by metal oxide particle, and this regional area is except metal oxide wild phase, be mainly metallic nickel and a small amount of argent.
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| CN201210296608.4A CN102808097B (en) | 2012-08-20 | 2012-08-20 | Silver/nickel/metallic oxide electrical contact material preparation method |
| EP13830377.1A EP2913413B1 (en) | 2012-08-20 | 2013-03-21 | Preparation method for electrical contact materials |
| US14/890,908 US10099286B2 (en) | 2012-08-20 | 2013-03-21 | Preparation method of electrical contact material |
| PCT/CN2013/072978 WO2014029210A1 (en) | 2012-08-20 | 2013-03-21 | Preparation method for electrical contact materials |
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| CN201210296608.4A CN102808097B (en) | 2012-08-20 | 2012-08-20 | Silver/nickel/metallic oxide electrical contact material preparation method |
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| JP6067111B2 (en) * | 2013-06-24 | 2017-01-25 | 三菱電機株式会社 | Manufacturing method of electrical contact material |
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| CN107598176B (en) * | 2017-08-02 | 2020-06-05 | 福达合金材料股份有限公司 | Preparation process of silver metal oxide electrical contact material |
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