CN102808097A - 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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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/MOX 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.
Retrieval through to prior art is found; The mandate patent of invention (201010579827.4 of bulletin in 2011; The preparation method of grain orientation arrangement enhancing Ag-based electrical contact material) discloses a kind of electroless plating coating legal system in and be equipped with Ag coating wild phase particulate midbody composite particles; The midbody composite particles is further mixed with the fine silver powder; Wild phase content is reduced to finished product content,, obtains the wild phase particle and in matrix, be fibrous novel contact material of arranging through mixing technologies such as powder, compacting, sintering, hot extrusion.
Traditional powder metallurgical technique generally mixes wild phase powder and silver powder are disposable; Reason owing to the distribution of wild phase diameter of particle; The undue disperse of ultra-fine wild phase powder that causes significant proportion is in silver matrix, thus the electric conductivity and the unit elongation of reduction contact material.The know-why of above document (patent of invention 201010579827.4) be with material electric property and mechanical property are had dysgenic wild phase particle with fibrous formal constraint of arranging at regional area, thereby improved the electric conductivity and the unit elongation of material.The silver of this regional area only is the effect of having played the wild phase carrier, and precious metal silver wherein is comparatively limited to the electroconductibility and the unit elongation contribution of integral material.
Further literature search is found, the main contriver of foregoing invention patent electrically contacts to have delivered in the international conference (ICEC2012) at the 26th in May, 2012 and is entitled as " Ag/ (SnO
2) 12Electrical Contact Material with Fibre-like Arrangement of Reinforcing Nanoparticles:Preparation; Formation Mechanism; And Properties " the research article; introduced preparation method and material property, specifically described and utilized the method for mechanical alloying to prepare SnO based on similar principles
2Content is 60% Ag/ (SnO
2) the midbody composite particles, with Ag/ (SnO
2) midbody composite particles and pure Ag powder be according to 1: 4 mixed, makes SnO
2Content reduces to 12%, and is follow-up through technologies such as compacting, sintering and hot extrusions, obtains SnO
2In silver matrix, be the fibrous new A g/ (SnO that arranges
2) the environmental protection contact material.Compare with prior powder metallurgy technology, resistivity is reduced 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/MOX contact material is provided; Original silver/preparation of metal oxides technology is improved; Adopt nickel to replace the carrier of precious metal silver as the MOX wild phase, preparation nickel/metal oxide intermediate composite particles, thus MOX is constrained in the midbody composite particles; Avoid the disadvantageous effect of super-fine metal oxide powder to the contact material performance; Then this midbody composite particles is mixed with the fine silver powder, through technologies such as compacting, sintering, extruding and drawings, the metal oxide particle that obtains the nickel coating is the novel silver/nickel/metal oxide materials of fibrous distribution in material.
The present invention realizes through following technical scheme: the present invention adopts the method for electroless plating, to MOX clad metal nickel, and then coated with silver, the composite granule of formation Ag-Ni-MeO nucleocapsid structure.Composite granule to obtaining carries out the granulation of protective atmosphere sintering; Obtain the midbody composite particles of high metal oxide content and high nickel content; The midbody composite particles is mixed with the fine silver powder; Through technologies such as compacting, sintering, extruding and drawings, the metal oxide particle that nickel is coated is fibrous distribution in material.
Aforesaid method concrete steps of the present invention are following:
The first step adopts the method for electroless plating to make metal oxide particle coat layer of metal nickel;
In second step, the method that adopts electroless plating further coats one deck silver to the metal oxide particle that the first step coats behind the nickel;
In the 3rd step, the powder of the Ag-Ni-MeO nucleocapsid structure that the employing nitrogen protection forms after second step was coated carries out the sintering granulation, acquisition midbody composite particles powder, screening then;
The 4th step, the midbody composite particles after the screening of the 3rd step is mixed with the fine silver powder, the content that lowers MOX is to setting numerical value;
The 5th step; Go on foot the pressed by powder that mixes with the 4th; The nitrogen protection atmosphere sintering again through extruding, drawing, obtains metal oxide particle is fibrous distribution at regional area novel silver/nickel/MOX contact material; And this regional area mainly is metallic nickel and a spot of argent except the MOX wild phase.
Aforesaid method:
In the first step, adopting the weight in average degree of MOX in the powder after electroless plating coats nickel is 40%～80%, and the weight in average degree of nickel is 20%～60%.
In second step, the weight in average degree of silver is less than 10% in the powder behind the employing electroless plating coated with silver.
In the 3rd step, the employing nitrogen protection is carried out the sintering granulation to the powder of the Ag-Ni-MeO nucleocapsid structure of formation after coating, and the agglomerating temperature is 700 ℃～800 ℃.
In the 3rd step,, continue to employ granularity and be-100 orders～+ 400 orders the midbody composite particles powder screening that obtains.
In the 4th step, the midbody composite particles is mixed with the fine silver powder, the weight percent content of MOX is reduced to 8%～20%.
In the aforesaid method of the present invention, said MOX is the MOX that can be applicable to contact material and realize above-mentioned purpose, and more excellent, MOX includes but not limited to CdO, SnO
2, ZnO, CuO, Ni
2O, WO
3, and the mixture of these MOXs.
Aforesaid method of the present invention; Behind the mixed powder that goes on foot through the 4th step and the 5th, pressed by powder, protective atmosphere sintering, extruding, the drawing process; In the silver/nickel that obtains/MOX contact material: metal oxide particle is fibrous distribution at regional area; Be that the fibrous tissue structure is aligned by metal oxide particle and forms, and this regional area mainly is metallic nickel and a spot of argent except the MOX wild phase.
The present invention adopts the method for electroless plating that metal oxide particle is coated one deck nickel; And then coated with silver; Form the Ag-Ni-MeO nucleocapsid structure; Improved the interface imbibition characteristic of metal oxide particle and silver matrix, eliminated in the prior powder metallurgy method because of the disadvantageous effect of interface imbibition characteristic difference to the contact material mechanical property.The more important thing is coating, replaced the silver in the midbody composite particles in the above document, thereby reduce the consumption of silver through metallic nickel.It is to improve the oxidation-resistance of midbody composite particles and the performance that improves the sintering granulation that the coating of silver mainly acts on, and the deformability of midbody composite particles in the course of processing, thereby improves use characteristics.
Embodiment
Elaborate in the face of embodiments of the invention down: present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
The present invention adopts the method for electroless plating; Metal oxide particle is coated nickel; And then coated with silver, the composite granule of formation Ag-Ni-MeO nucleocapsid structure, wherein chemical nickel plating and silver plated method can adopt operation realization in following examples; But be not limited to this operation, also can adopt the method for other existing electroless platings to realize.The 4th step of the inventive method and the 5th step are adopted mixed powder of the prior art, pressed by powder, nitrogen protection atmosphere sintering, extruding, drawing process respectively, specifically are not limited to operation and processing parameter in following examples.
Embodiment 1:
1. adopt the method for electroless plating to coat one deck nickel to the CdO powder, making the average content (weight percent) of CdO in the powder is 80%, and the weight in average degree of nickel is 20%; Can adopt following technology to realize in the present embodiment:
A) disperse before the plating: the quality of nanoparticulate dispersed effect is directly connected to the distribution and the content of its particulate in composite deposite, and then directly has influence on the performance of composite deposite.Preferably, present embodiment adopts sodium-alginate (or PVP K120) to make dispersion agent.Concrete elder generation is with the CdO nanoparticle of the wetting 12.5g of absolute ethyl alcohol of 200mL; Take by weighing the sodium-alginate of 7.5g then, it is dissolved in the 1L deionized water; To slowly join in the sodium alginate soln with the wetting CdO nanoparticle of absolute ethyl alcohol then, ultrasonic dispersing and mechanical stirring can obtain dispersion liquid;
B) sensitization and activation: with above-mentioned solution at SnCl at 16g/L
22H O and 0.18g/L PdCl
2Carry out sensitization and activation in the colloidal pd activation solution; In this process, Sn (OH) CL is with 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, and is for use.
C) reduction: adopt 30g/L NaH
2PO
32H
2O solution is put into reduced liquid 3min with the CdO powder particle of activated processing, and reduction possibly residue in its surperficial Pd
2+, prevent that it from bringing into and cause plating bath to decompose in the plating bath, 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 (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 that configures.Plating temperature is (83 ± 3) ℃, and the plating time is 90min.Distilled water flushing is dried then.
2, chemical silvering: further adopt electroless plating to coat one deck silver to the CdO that coats nickel, the weight in average degree that coats silver in the powder of back is less than 10%;
3, the Ag/Ni/CdO core-shell structured powder for preparing is put into the granulation of nitrogen sintering oven sintering, sintering temperature is 700 ℃, sieves after the granulation, removes fine particle, continues to employ the midbody composite particles powder between granularity-100 order～+ 400 orders;
4, will sieve the Ag/Ni/CdO midbody composite particles powder that obtains mixes with the fine silver powder; Making the CdO weight in average degree that mixes in the powder of back is 20%, and " V " type of then powder being poured into mixes in the powder machine, carries out evenly mixing powder; Rotating speed is 30 rev/mins when mixing powder, 4 hours time;
5, be 90cm with the powder that the mixes diameter of packing into, in the length 150cm plastic cement tube, carry out isostatic cool pressing, isostatic cool pressing pressure 200Mpa;
6, the base substrate that obtains after the isostatic cool pressing is carried out the nitrogen protection atmosphere sintering, 800 ℃ of sintering temperatures, sintering 5 hours;
7, the base substrate that obtains behind the sintering is carried out hot pressing, 800 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 10min;
8, hot pressing is good base substrate carries out hot extrusion, 600 ℃ of extrusion temperatures, extrusion ratio 180, extrusion speed 5cm/min, 500 ℃ of extrusion mould preheating temperatures;
Present embodiment finally obtains the Cadmium oxide particle and is the new A g/Ni/CdO contact material of fibrous distribution at regional area, and this regional area mainly is metallic nickel and a spot of argent except the CdO wild phase.The material that obtains is 3.9 μ Ω .cm along direction of extrusion resistivity; Hardness is 87HV.
Embodiment 2:
1. to SnO
2Adopt the method for electroless plating to coat one deck nickel, make SnO in the powder
2The weight in average degree be 60%, the weight in average degree of nickel is 40%;
2. to coating the SnO of nickel
2Further adopt electroless plating to coat one deck silver, the weight in average degree that coats silver in the powder of back is less than 10%; Can adopt following existing techniques in realizing in the present embodiment:
The Ni-CdO powder is put into reduced liquid and mechanical dispersed with stirring 5min; Dropwise be added drop-wise in reduced liquid and mechanical stirring with dropper silver ammino solution; Make silver ion reduction be deposited on the Ni-CdO surface, clean up with deionized water, 50 ℃ of oven dry promptly get has nucleocapsid structure Ag/Ni/CdO powder;
In the present embodiment, said silver ammino solution and reduced liquid were according to preparation respectively in 1: 1; The preparation of said 50ml reduced liquid: formaldehyde 1.1ml adds water to 50ml; Add the 1.75g Silver Nitrate in the deionized water of the preparation of said 50ml silver ammino solution: 30ml, add people 10ml ammoniacal liquor and constantly stirring after the stirring and dissolving again, and improve pH value, add water to 50ml again with appropriate amount of NaOH solution.
3. the Ag/Ni/SnO to preparing
2Core-shell structured powder is put into the granulation of nitrogen sintering oven sintering, and sintering temperature is 800 ℃, sieves after the granulation, removes fine particle, continues to employ the midbody composite particles powder between granularity-100 order～+ 400 orders;
4. will sieve the Ag/Ni/SnO that obtains
2Midbody composite particles powder mixes with the fine silver powder, makes the SnO that mixes in the powder of back
2The weight in average degree is 12%, and " V " type of then powder being poured into mixes in the powder machine, carries out evenly mixing powder;
5. be 90cm with the powder that the mixes diameter of packing into, in the length 150cm plastic cement tube, carry out isostatic cool pressing, isostatic cool pressing pressure 200Mpa;
6. the base substrate that obtains after the isostatic cool pressing is carried out the nitrogen protection atmosphere sintering, 865 ℃ of sintering temperatures, sintering 5 hours;
7. the base substrate that obtains behind the sintering is carried out hot pressing, 800 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 10min;
8. the base substrate that hot pressing is good carries out hot extrusion, 600 ℃ of extrusion temperatures, extrusion ratio 180, extrusion speed 5cm/min, 500 ℃ of extrusion mould preheating temperatures;
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 the wild phase, mainly be metallic nickel and a spot of argent.The material that obtains is 3.0 μ Ω .cm along direction of extrusion resistivity; Hardness is 78HV.
Embodiment 3:
1. adopt the method for electroless plating to coat one deck nickel to ZnO, the weight in average degree that makes ZnO in the powder is 40%, and the weight in average degree of nickel is 60%;
2. further adopt electroless plating to coat one deck silver to the ZnO that coats nickel, the weight in average degree that coats silver in the powder of back is less than 10%;
3. the Ag/Ni/ZnO core-shell structured powder for preparing is put into the granulation of nitrogen sintering oven sintering, sintering temperature is 700 ℃, sieves after the granulation, removes fine particle, continues to employ the midbody composite particles powder between granularity-100 order～+ 400 orders;
4. will sieve the Ag/Ni/ZnO midbody composite particles powder that obtains mixes with the fine silver powder; Making the ZnO weight in average degree that mixes in the powder of back is 10%, and " V " type of then powder being poured into mixes in the powder machine, carries out evenly mixing powder; Rotating speed is 30 rev/mins when mixing powder, 4 hours time;
5. the powder that the 4th step was mixed adopts prior art to carry out pressed by powder, and the nitrogen protection atmosphere sintering again through extruding, drawing, obtains silver/nickel/MOX contact material.
Present embodiment finally obtains the ZnO particle and is the new A g/Ni/MeO contact material of fibrous distribution at regional area, and this regional area mainly is metallic nickel and a spot of argent except the ZnO wild phase.The material that obtains is 3.4 μ Ω .cm along direction of extrusion resistivity; Hardness is 75HV.
Embodiment 4:
1. to SnO
2Adopt the method for electroless plating to coat one deck nickel, make SnO in the powder
2The weight in average degree be 50%, the weight in average degree of nickel is 50%;
2. to coating the SnO of nickel
2Further adopt electroless plating to coat one deck silver, the weight in average degree that coats silver in the powder of back is less than 10%;
3. the Ag/Ni/SnO to preparing
2Core-shell structured powder is put into the granulation of nitrogen sintering oven sintering, and sintering temperature is 800 ℃, sieves after the granulation, removes fine particle, continues to employ the midbody composite particles powder between granularity-100 order～+ 400 orders;
4. will sieve the Ag/Ni/SnO that obtains
2Midbody composite particles powder mixes with the fine silver powder, makes the SnO that mixes in the powder of back
2The weight in average degree is 8%, and " V " type of then powder being poured into mixes in the powder machine, carries out evenly mixing powder;
5. the powder that the 4th step was mixed carries out the cold compacting of Denging to powder, and the nitrogen protection atmosphere sintering again through extruding, drawing, obtains silver/nickel/MOX contact material.
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 the wild phase, mainly be metallic nickel and a spot of argent.The material that obtains is 2.5 μ Ω .cm along direction of extrusion resistivity; Hardness is 70HV.
More than be part embodiment of the present invention, should be pointed out that the present invention also has other embodiment, implement parameter or replace the respective operations in the foregoing description with prior art such as conversion.Although content of the present invention has been done detailed introduction through the foregoing description, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (10)
1. the preparation method of silver/nickel/MOX contact material is characterized in that may further comprise the steps:
The first step adopts the method for electroless plating to make metal oxide particle coat layer of metal nickel;
In second step, the method that adopts electroless plating further coats one deck silver to the metal oxide particle that the first step coats behind the nickel;
In the 3rd step, the powder of the Ag-Ni-MeO nucleocapsid structure that the employing nitrogen protection forms after second step was coated carries out the sintering granulation, acquisition midbody composite particles powder, and thick and meticulous particle was removed in screening then;
The 4th step, the midbody composite particles after the screening of the 3rd step is mixed with the fine silver powder, the content that lowers MOX is to setting numerical value;
The 5th step; Go on foot the pressed by powder that mixes with the 4th; The protective atmosphere sintering again through extruding, drawing, obtains the oildag particle is fibrous distribution at regional area silver/nickel/MOX contact material; And this regional area mainly is metallic nickel and a spot of argent except the MOX wild phase.
2. the preparation method of silver/nickel as claimed in claim 1/MOX contact material; It is characterized in that; In the first step; Adopting the average content of MOX in the powder after electroless plating coats nickel is 40%～80%, and the average content of nickel is 20%～60%, and said content is meant weight percent content.
3. the preparation method of silver/nickel as claimed in claim 1/MOX contact material is characterized in that, in second step, the average content of silver is less than 10% in the powder behind the employing electroless plating coated with silver, and said content is meant weight percent content.
4. the preparation method of silver/nickel as claimed in claim 1/MOX contact material is characterized in that, in the 4th step, the midbody composite particles is mixed with the fine silver powder, and the weight percent content of MOX is reduced to 8%～20%.
5. the preparation method of silver/nickel as claimed in claim 1/MOX contact material; It is characterized in that; Adopting the average content of MOX in the powder after electroless plating coats nickel in the first step is 40%～80%, and the average content of nickel is 20%～60%; The average content of silver is less than 10% in the powder in second step behind the employing electroless plating coated with silver, and said content is meant weight percent content.
6. the preparation method of silver/nickel as claimed in claim 1/MOX contact material; It is characterized in that; Adopting the average content of MOX in the powder after electroless plating coats nickel in the first step is 40%～80%, and the average content of nickel is 20%～60%; The average content of silver is less than 10% in the powder in second step behind the employing electroless plating coated with silver; In the 4th step the midbody composite particles is mixed with the fine silver powder, the weight percent content of MOX is reduced to 8%～20%; Said content is meant weight percent content.
7. like the preparation method of each described silver/nickel of claim 1-6/MOX contact material; It is characterized in that; In the 3rd step, the employing nitrogen protection is carried out the sintering granulation to the powder of the Ag-Ni-MeO nucleocapsid structure of formation after coating, and the agglomerating temperature is 700 ℃～800 ℃.
8. like the preparation method of each described silver/nickel of claim 1-6/MOX contact material, it is characterized in that, in the 3rd step,, continue to employ granularity and be-100 orders～+ 400 orders the midbody composite particles powder screening that obtains.
9. like the preparation method of each described silver/nickel of claim 1-6/MOX contact material, it is characterized in that described MOX includes but not limited to CdO, SnO
2, ZnO, CuO, Ni
2O, WO
3, and the mixture of these MOXs.
10. silver/nickel/MOX contact material that the said method of claim 1-9 obtains; It is characterized in that: in said silver/nickel/MOX contact material: metal oxide particle is fibrous distribution at regional area; Be that the fibrous tissue structure is aligned by metal oxide particle and forms; And this regional area mainly is metallic nickel and a spot of argent except the MOX wild phase.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210296608.4A CN102808097B (en) | 2012-08-20 | 2012-08-20 | Silver/nickel/metallic oxide electrical contact material preparation method |
| 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 |
| EP13830377.1A EP2913413B1 (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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