EP2537949B1 - Method for preparing fibrous silver-based electrical contact material - Google Patents

Method for preparing fibrous silver-based electrical contact material Download PDF

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Publication number
EP2537949B1
EP2537949B1 EP11844208.6A EP11844208A EP2537949B1 EP 2537949 B1 EP2537949 B1 EP 2537949B1 EP 11844208 A EP11844208 A EP 11844208A EP 2537949 B1 EP2537949 B1 EP 2537949B1
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Prior art keywords
powders
silver
powder
hot
green body
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German (de)
French (fr)
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EP2537949A1 (en
EP2537949A4 (en
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Lesheng Chen
Xiao Chen
Gengxin Qi
Chengfa Mu
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/06Alloys based on silver
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1084Alloys containing non-metals by mechanical alloying (blending, milling)
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1094Alloys containing non-metals comprising an after-treatment
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0021Matrix based on noble metals, Cu or alloys thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • H01H1/023Composite material having a noble metal as the basic material
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Definitions

  • the present invention relates to a method for preparing an electrical contact material in a field of materials technology, and more particularly to a method of preparing a fibrous silver-based electrical contact material.
  • the first is a method of conventional powder metallurgy sintering and extrusion, whose main process includes powder mixing, pressing, sintering, extruding, drawing, annealing, drawing and finally obtaining finished products. This method is unable to obtain the desired neat fibrous structure and may produce large reinforcing particles that severely undermine the performance of the products.
  • the second is a modification of the first method with improved extrusion and increased processing deformation as recited in the research (a). This method is unable to provide fibrous silver-based materials when the processing deformation is small, such as extruding into strips or sheets.
  • the third refers to a combination of a pre-design of green body and an extruding method. More precisely, a certain number of reinforcing wires are fixed into a matrix through a mould in advance and subjected to isostatic pressing, sintering and extruding as recited in research (b). Although able to create neat and continuous fibrous structure, the third method is not applied to industrial-scale production because the third method is relatively complex and places particular requirement on the plasticity and ductility of the reinforcing wires.
  • the third method requires that the silver-based wires with reinforcing materials be prepared in advance and fixed into the matrix through the mould. Therefore, it is understood that fibrous silver-based electrical contact materials cannot be obtained either by simple powder mixing or in the situation where the deformation is relatively small or where the reinforcing phase has poor plasticity and ductility.
  • CN101241804 (B ) discloses a silver-zinc oxide electrical contact and preparation method. The method involves preparing Ag-Zn alloy powder with gas atomizing after melting, oxidising after abrasive processing, adding additive, and molding, sintering and hot processing.
  • CN 101608272 (A ) discloses a particular AgNi-based electrical contact material and preparation method. The method involves ball-milling, pressing, sintering and extruding.
  • CN 101649401 discloses an Ag-Ni-oxide electrical contact material and preparation method. The method involved re-oxidizing Ag alloy powder to obtain oxide particle reinforced Ag base powder, mixing with Ni powder to prepare the Ni particle and oxide particle reinforced Ag-Ni-oxide based electrical contact material.
  • the present invention provides a method for preparing silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles which places no particular requirements on processing deformation and the plasticity and ductility of the reinforcing phase.
  • the method has simple process, easy operation, low cost and no specific requirements on the equipment.
  • obtained contact material has better resistance to welding and arc erosion and better conductivity, and processing performance is also improved.
  • the present invention adopts following technical solutions.
  • the present invention provides a method for preparing silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles comprising the following steps:
  • the silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles prepared through the method of the present invention have reinforcing phase with a neat fibrous structure wherein the fibrous structure of the reinforcing material is formed through directional arrangement of particles thereof.
  • the reinforcing particles have an average size between 5 nm and 30 ⁇ m and are made of one material or a mixture of several materials that can form silver-coated particles after being processed through high energy ball milling machine.
  • the method of the present invention is described as follows. Firstly the base silver powders and the reinforcing phase material powders are processed with high energy ball milling for refinement through high energy collision and milling; and the refined silver powders coats on the reinforcing particles or the reinforcing particles are inlaid into the silver particles to further generate aggregates of coated bodies or inlaid bodies. Then, the aggregates and additional base silver powders are uniformly mixed according to a predetermined recipe and orderly processed with isostatic pressing, sintering, hot pressing and hot extruding. During hot extruding, the aggregates move with softened Ag in the matrix of Ag.
  • the reinforcing material can be conveniently separated and exhibits a fibrous structure with directional arrangement along the extrusion direction.
  • Electrical contact materials prepared by the method of the present invention have a neat fibrous arrangement of the reinforcing phase and better performance.
  • the resistance to arc erosion is 10% to 20% higher than the identical electrical contact material dispersion-reinforced by ordinary particles; electrical conductivity along the extrusion direction increases by 5% to 20%; resistance to welding increases by 10% to 20%; and electrical service life increases by 10% to 30%.
  • the electrical contact material prepared by the method of the present invention has good processing performance and is suitable for large scale production.
  • the present invention provides a method of preparing silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles which is suitable for ordinary preparation to yield fiber-reinforced silver-based contact materials with no particular requirements on processing deformation and plasticity and ductility of reinforcing phase.
  • a production process of the method is simple and easy. Besides, there is no particular requirement on equipments.
  • the silver-based electrical contact material prepared by the method of the present invention has a neat fibrous reinforcing material, wherein the fibrous structure of the reinforcing material is formed through directional arrangement of the reinforcing particles.
  • the particles of the reinforcing powder have an average size of 5 nm to 30 ⁇ m.
  • the particles can be of one material or a mixture of materials and mixed with silver powders in such a proportion as to obtain silver-coated particles after being processed with high energy ball milling. In a specific preparation, the reinforcing material ratio is determined according to practical needs.
  • Ag matrix powder is obtained through atomization and sieving. Particle sizes of the silver powders range from 100 meshes to 400 meshes.
  • the matrix power can be obtained by other conventional arts.
  • step 1 the reinforcing powders are uniformly mixed with the silver matrix powders and then placed in a high energy ball mill for milling, wherein the parameters are set as follows.
  • a weight ratio of the reinforcing powder to silver powder is between 0.5 and 3; a milling speed ranges from 180 rpm to 280 rpm; a milling time is 5 to 12 hours.
  • step 2 the ball-milled composite powders obtained from step 1 and silver powders are poured into a powder mixing machine for mixing, wherein the parameters are set as follows.
  • a weight ratio of the composite powders to silver powder is between 1 and 0.136; a rotation speed of the powder mixing machine is between 20 rpm and 30 rpm; the powder mixing lasts for 2 to 4 hours.
  • step 3 the powder obtained from the step 2 is processed with cold isostatic pressing, wherein the parameters are set as follows.
  • the isostatic pressure is between 100 and 500 MPa.
  • step 4 the green body obtained by cold isostatic pressing is sintered, wherein the parameters are set as follows.
  • a sintering temperature is between 600°C and 900°C. The sintering lasts for 5 to 9 hours.
  • step 5 the green body obtained by sintering is processed with hot pressing, wherein the parameters are set as follows.
  • a hot pressing temperature is between 500°C and 900°C.
  • a hot pressing pressure is between 300 to 700 MPa. The hot pressing lasts for 1 min to 30 min.
  • step 6 the green body obtained through hot pressing is hot extruded to obtain silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles wherein the parameters are set as follows.
  • the green body is heated at a temperature between 600-900°C.
  • An extrusion ratio is between 20 and 400 and an extrusion speed is between 5 to 20 cm/min.
  • a pre-heating temperature of extruding moulds is between 300 and 500°C.
  • a preparation of AgSnO 2 (12) contact material is taken as an example, referring to Fig. 1 and 2 .
  • Step 1 obtaining a matrix of Ag powder having a particle size of 200 meshes, wherein the silver is third-level atomized and then sieved through a sieve of 200 meshes;
  • Step 2 600g of reinforcing SnO 2 powder having a particle size of 80 nm on average and 400 g of the Ag powder obtained from step 1 are uniformly mixed and then placed into a high energy ball mill for milling, wherein the ball mill rotates at 280 rpm and the ball milling lasts for 10 hours; a scanning electron photomicrograph of the generated composite powder is showed in Fig. 1 ;
  • Step 3 1 Kg composite powder obtained from Step 2 and 4 Kg silver powder obtained from Step 1 are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at 30 rpm for 4 hours;
  • Step 4 the powder obtained from Step 3 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing, wherein the cold isostatic pressure is 100 MPa;
  • Step 5 the green body obtained through the cold isostatic pressing in Step 4 is sintered at 865°C for 5 hours;
  • Step 6 the sintered green body obtained from Step 5 is processed with hot pressing at 800°C under 500 MPa for 10 min;
  • Step 7 the green body obtained through the hot pressing is processed with hot extrusion at 800°C, wherein an extrusion ratio is 225; an extrusion speed is 5 cm/min; and a pre-heating temperature of extruding moulds is 500°C.
  • the AgSnO 2 (12) contact material with obviously neat fibrous reinforcing SnO 2 is finally obtained, wherein the fiber-like arrangement of SnO 2 is formed through directional arrangement and connection of the nanoparticles of SnO 2 .
  • a metallograph thereof is showed in Fig. 2 .
  • the obtained material has a tensile strength of 285 MPa, an electrical resistivity along the extrusion direction of 2.1 ⁇ cm and a hardness of 85 HV.
  • a preparation of AgCdO12 contact material is taken as an example.
  • Step 1 600 g of reinforcement powder of CdO having particles of 1 ⁇ m on average and 200 g of Ag powder having a particle size of 400 meshes are uniformly mixed and then placed into a high energy ball mill for mixing, wherein the ball mill rotates at a speed of 240 rpm for 10 hours;
  • Step 2 800 g of the composite powder obtained from the step 1 and 4200 g of silver powder having a particle size of 400 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 25 rpm for 4 hours;
  • Step 3 the powder obtained from Step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing under a cold isostatic pressure of 300 MPa;
  • Step 4 the green body obtained from cold isostatic pressing in Step 3 is sintered at 750 °C for 9 hours;
  • Step 5 the sintered green body obtained from Step 4 is processed with hot pressing at 800 °C under a hot pressing pressure of 300 MPa for 20 min;
  • Step 6 the green body obtained from hot pressing is hot extruded into sheets at a hot extrusion temperature of 900 °C, wherein an extrusion ratio is 100; an extrusion speed is 10 cm/min; and a pre-heating temperature of extruding moulds is 300 °C.
  • the fiber-like arrangement of CdO is formed through directional arrangement and connection of a number of CdO particles.
  • the generated material has a tensile strength of 290 MPa, an electrical resistivity of 2.0 ⁇ cm and a hardness of 88 HV.
  • a preparation of AgZnO(8) contact material is taken as an example.
  • Step 1 400 g of reinforcement powder of ZnO having particles of 100 nm on average and 800 g of Ag powder having a particle size of 400 meshes are uniformly mixed and placed in a high energy ball mill for mixing, wherein the ball mill rotates at a speed of 240 rpm for 5 hours;
  • Step 2 1200 g of the composite powder obtained from Step 1 and 3800 g of silver powder having a particle size of 600 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 4 hours;
  • Step 3 the powder obtained from Step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing at a cold isostatic pressure of 100 MPa;
  • Step 4 the green body obtained from the cold isostatic pressing in Step 3 is sintered at 830 °C for 5 hours;
  • Step 5 the sintered green body obtained from Step 4 is processed with hot pressing at 830 °C under a hot pressing pressure of 700 MPa for 1 min;
  • Step 6 the green body after the hot pressing is processed with hot extruding into sheets at a hot extrusion temperature of 800 °C, wherein an extrusion ratio is 324; an extrusion speed is 20 cm/min; and a pre-heating temperature of extruding moulds is 300 °C.
  • AgZnO(8) contact materials having a neat fiber-like arrangement of reinforcing ZnO are finally obtained, wherein the fiber-like arrangement of ZnO is formed through directional arrangement and connection of ZnO particles.
  • the generated material has a tensile strength of 280 MPa, a resistivity of 1.9 ⁇ cm and a hardness of 85 HV.
  • a preparation of Ag-4ZnO-8SnO 2 contact materials is taken as an example.
  • Step 1 a matrix of Ag powder having a particle size of 100 meshes is obtained, wherein the silver is third-level atomized and then sieved through a sieve of 100 meshes;
  • Step 2 200g reinforcing powder of ZnO particles of an average size of 100 nm and 400g reinforcing powder of SnO 2 particles of 80 nm on average and 400g Ag powder obtained from step 1 are uniformly mixed together and then placed into a high energy ball mill for milling, wherein the ball mill rotates at a speed of 280 rpm for 10 hours;
  • Step 3 1000g composite powder obtained from step 2 and 4000g silver powder obtained from step 1 are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 4 hours;
  • Step 4 the powder obtained from Step 3 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing, wherein the cold isostatic pressure is 200 MPa;
  • Step 5 the green body after the cold isostatic pressing obtained from the step 4 is sintered at 865°C for 5 hours;
  • Step 6 the sintered green body obtained from Step 5 is processed with hot pressing at 800°C under 700 MPa for 10 min;
  • Step 7 the green body obtained through hot pressing is processed with hot extrusion at 800°C, wherein an extrusion ratio is 400; an extrusion speed is 5 cm/min; and a pre-heating temperature of extruding moulds is 500°C.
  • the Ag-4ZnO-8SnO 2 contact material with a neat fibre-like arrangement of reinforcing ZnO and SnO 2 particles is finally obtained, wherein the fiber-like arrangement of ZnO and SnO 2 is formed through directional arrangement and connection of nanoparticles of ZnO and SnO 2 .
  • the generated material has a tensile strength of 255 MPa, an electrical resistivity along the extrusion direction of 2.0 ⁇ cm and a hardness of 85 HV.
  • a preparation of AgNi(25) contact materials is taken as an example.
  • Step 1 500g reinforcing powder of Ni having particles of 10 ⁇ m on average and 500g Ag powder having a particle size of 300 meshes are uniformly mixed and then placed in a high energy ball mill for mixing, wherein the ball mill rotates at a speed of 280 rpm for 8 hours;
  • Step 2 1000g of the composite powder obtained from step 1 and 1000g of silver powder having a particle size of 400 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 2 hours;
  • Step 3 the powder obtained from step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing at a cold isostatic pressure of 200 MPa;
  • Step 4 the green body obtained through cold isostatic pressing in Step 3 is sintered at 860 °C for 7 hours;
  • Step 5 the sintered green body obtained from step 4 is processed with hot pressing at 800 °C under a hot pressing pressure of 400 MPa for 20 min;
  • Step 6 the green body is hot-extruded into sheets at a hot extrusion temperature of 860 °C, wherein an extrusion ratio is 225; an extrusion speed is 10 cm/min; and a pre-heating temperature of extruding moulds is 500 °C.
  • the material of AgNi(25) with neat fiber-like arrangement of reinforcing Ni is finally obtained, wherein the fiber-like arrangement of Ni is formed through directional arrangement and connection of nanoparticles of Ni.
  • the generated material has a tensile strength of 300 MPa, a electrical resistivity along an extrusion direction of 2.0 ⁇ cm and a hardness of 80 HV.
  • a preparation of AgFe 7 contact materials is taken as an example.
  • Step 1 a matrix of Ag powder having a particle size of 100 meshes is obtained, wherein the silver is third-level atomized and then sieved through a sieve of 100 meshes;
  • Step 2 350g of reinforcement powder of Fe having particles of 30 ⁇ m on average and 400g of the Ag powder obtained from step 1 are uniformly mixed and then placed into a high energy ball mill for milling wherein the ball mill rotates at a speed of 180 rpm for 12 hours;
  • Step 3 750g of the composite powder obtained from Step 2 and 4250g of the silver powder obtained from Step 1 are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 20 rpm for 4 hours;
  • Step 4 the powder obtained from Step 3 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing, wherein the cold isostatic pressure is 500 MPa;
  • Step 5 the green body obtained from cold isostatic pressing in Step 4 is sintered at 900°C for 5 hours under protection of hydrogen atmosphere;
  • Step 6 the sintered green body obtained from Step 5 is processed with hot pressing at 900°C under 700 MPa for 30 min;
  • Step 7 the green body after the hot pressing is processed with hot extruding at 700°C, wherein an extrusion ratio is 20; an extrusion speed is 10 cm/min; and a pre-heating temperature of extruding moulds is 400°C.
  • the material of AgFe 7 with a neat fiber-like arrangement of reinforcing Fe is finally obtained, wherein the fiber-like arrangement of Fe is formed through directional arrangement and connection of nanoparticles of Fe.
  • the generated material has a tensile strength of 310 MPa, an electrical resistivity along an extrusion direction of 1.9 ⁇ cm and a hardness of 75 HV.
  • a preparation of AgZnO(6) contact material is taken as an example.
  • Step 1 300g of reinforcing powder of ZnO having particles of 5nm on average and 300g of Ag powder having a particle size of 400 meshes are uniformly mixed and then placed in a high energy ball mill for milling, wherein the ball mill rotates at a speed of 180 rpm for 8 hours;
  • Step 2 600g of the composite powder obtained from Step 1 and 4400g of silver powder having a particle size of 200 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 4 hours;
  • Step 3 the powder obtained from Step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing at a cold isostatic pressure of 300 MPa;
  • Step 4 the green body obtained from cold isostatic pressing in Step 3 is sintered at 600 °C for 7 hours;
  • Step 5 the sintered green body obtained from Step 4 is processed with hot pressing at 500 °C under a hot pressing pressure of 500 MPa for 10 min;
  • Step 6 the green body obtained from hot pressing is hot-extruded into sheets at a hot extrusion temperature of 600 °C, wherein an extrusion ratio is 225; an extrusion speed is 5 cm/min; and a pre-heating temperature of extruding moulds is 500 °C.
  • the AgZnO(6) contact material with a neat fiber-like arrangement of reinforcing ZnO is finally obtained, wherein the fiber-like arrangement of ZnO is formed through directional arrangement and connection of nanoparticles of ZnO.
  • the generated material has a tensile strength of 270 MPa, a electrical resistivity along the extrusion direction of 1.85 ⁇ cm and a hardness of 80 HV.

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Description

    Background of the Present Invention Field of Invention
  • The present invention relates to a method for preparing an electrical contact material in a field of materials technology, and more particularly to a method of preparing a fibrous silver-based electrical contact material.
  • Description of Related Arts
  • With the rapid development of the electrical apparatus industry, the application of electrical apparatus switches has brought about increasingly high requirements on the performance of the electrical contact materials such as high resistance to welding and arc erosion and good conductivity. With regard to these requirements, worldwide researchers have made great efforts to improve the performance mainly by designing material composition and reinforcing particles dispersion uniformity. Compared to the silver-based composite material dispersion-reinforced by ordinary particles, the silver-based composite material reinforced by fiber-like arranged particles has better resistance to welding and arc erosion and a good processing property. The development of a simple and practical method which could be applied to large-scale production has attracted tremendous research interest and still remains to be a difficult point in the present research.
  • Some researches on silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles are stated as follows.
    • (a)Yonggen Wang, & etc., Study on the process of the fibrous AgNi composite wire, electrical engineering materials, Vol.20, No.1, 2007;
    • (b)Chinese patent, fibrous structure silver-based electrical contact material and preparation method thereof, having an application number of 200910196283.0 and a publication number of CN101707145A .
  • Three traditional methods of preparing silver-based electrical contact materials are as follows. The first is a method of conventional powder metallurgy sintering and extrusion, whose main process includes powder mixing, pressing, sintering, extruding, drawing, annealing, drawing and finally obtaining finished products. This method is unable to obtain the desired neat fibrous structure and may produce large reinforcing particles that severely undermine the performance of the products. The second is a modification of the first method with improved extrusion and increased processing deformation as recited in the research (a). This method is unable to provide fibrous silver-based materials when the processing deformation is small, such as extruding into strips or sheets. Furthermore, this method is not suitable for reinforcing phase with poor plasticity and ductility, such as SnO2. The third refers to a combination of a pre-design of green body and an extruding method. More precisely, a certain number of reinforcing wires are fixed into a matrix through a mould in advance and subjected to isostatic pressing, sintering and extruding as recited in research (b). Although able to create neat and continuous fibrous structure, the third method is not applied to industrial-scale production because the third method is relatively complex and places particular requirement on the plasticity and ductility of the reinforcing wires. In addition, the third method requires that the silver-based wires with reinforcing materials be prepared in advance and fixed into the matrix through the mould. Therefore, it is understood that fibrous silver-based electrical contact materials cannot be obtained either by simple powder mixing or in the situation where the deformation is relatively small or where the reinforcing phase has poor plasticity and ductility.
  • CN101241804 (B ) discloses a silver-zinc oxide electrical contact and preparation method. The method involves preparing Ag-Zn alloy powder with gas atomizing after melting, oxidising after abrasive processing, adding additive, and molding, sintering and hot processing.
  • CN 101608272 (A ) discloses a particular AgNi-based electrical contact material and preparation method. The method involves ball-milling, pressing, sintering and extruding.
  • CN 101649401 (A ) discloses an Ag-Ni-oxide electrical contact material and preparation method. The method involved re-oxidizing Ag alloy powder to obtain oxide particle reinforced Ag base powder, mixing with Ni powder to prepare the Ni particle and oxide particle reinforced Ag-Ni-oxide based electrical contact material.
  • Summary of the Present Invention
  • With regard to the weakness and defects in prior arts, the present invention provides a method for preparing silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles which places no particular requirements on processing deformation and the plasticity and ductility of the reinforcing phase. The method has simple process, easy operation, low cost and no specific requirements on the equipment. In the method of the present invention, obtained contact material has better resistance to welding and arc erosion and better conductivity, and processing performance is also improved.
  • In order to achieve the above object, the present invention adopts following technical solutions.
  • The present invention provides a method for preparing silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles comprising the following steps:
    1. (1) uniformly mixing reinforcing phase material powders with base silver powders, and then placing the mixed powders into a high energy ball milling tank for ball-milling, wherein the reinforcing phase material powders and the base silver powders are mixed in such a weight proportion between the reinforcing phase material powders and the base silver powders, that composite powders with silver-coated reinforcing phase material and aggregates thereof are obtained, wherein the weight proportion of the reinforcing phase material powders to the base silver powders is between 0.5 and 3; the ball mill rotates at a speed between 180 rpm and 280 rpm; and the ball milling lasts for 5 to 12 hours;
    2. (2) placing the composite powders obtained from step (A) and additional base silver powders into a powder mixing machine and mixing, wherein a weight ratio of the composite powders to the base silver powder is calculated according to composition of desired materials and size of fibrous structure, wherein the weight ratio of the composite powders and the additional base silver powders is between 1 and 1.036; the powder mixing machine rotates at a speed between 20 rpm and 30 rpm; the powder mixing lasts for 2 to 4 hours;
    3. (3) processing powder body obtained from the step (2) with cold isostatic pressing to obtain a green body;
    4. (4) sintering green body obtained from step (3);
    5. (5) hot pressing the green body obtained from step (4);
    6. (6) hot extruding the green body obtained from step (5) to obtain the fibrous silver-based electrical contact material.
  • The silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles prepared through the method of the present invention have reinforcing phase with a neat fibrous structure wherein the fibrous structure of the reinforcing material is formed through directional arrangement of particles thereof. The reinforcing particles have an average size between 5 nm and 30 µm and are made of one material or a mixture of several materials that can form silver-coated particles after being processed through high energy ball milling machine.
  • Different from conventional preparation methods combining mechanical alloying and large plastic deformation, the method of the present invention is described as follows. Firstly the base silver powders and the reinforcing phase material powders are processed with high energy ball milling for refinement through high energy collision and milling; and the refined silver powders coats on the reinforcing particles or the reinforcing particles are inlaid into the silver particles to further generate aggregates of coated bodies or inlaid bodies. Then, the aggregates and additional base silver powders are uniformly mixed according to a predetermined recipe and orderly processed with isostatic pressing, sintering, hot pressing and hot extruding. During hot extruding, the aggregates move with softened Ag in the matrix of Ag. The reinforcing material can be conveniently separated and exhibits a fibrous structure with directional arrangement along the extrusion direction. Electrical contact materials prepared by the method of the present invention have a neat fibrous arrangement of the reinforcing phase and better performance. The resistance to arc erosion is 10% to 20% higher than the identical electrical contact material dispersion-reinforced by ordinary particles; electrical conductivity along the extrusion direction increases by 5% to 20%; resistance to welding increases by 10% to 20%; and electrical service life increases by 10% to 30%. In addition, the electrical contact material prepared by the method of the present invention has good processing performance and is suitable for large scale production.
  • These and other objectives, features, and advantages of the present invention will become apparent from the following detailed description, the accompanying drawings, and the appended claims.
  • Brief Description of the Drawings
    • Fig. 1 is a scanning electron micrograph of aggregates of silver-coated SnO2 particles according to a first preferred embodiment of the present invention.
    • Fig. 2 is a metallograph of fibrous AgSnO2(12) electrical contact material according to the first preferred embodiment of the present invention.
    • Fig. 3 is a metallograph of fibrous AgSnO2(12) rivet contact according to the first preferred embodiment of the present invention.
    Detailed Description of the Preferred Embodiment
  • The following is a more detailed description of the technical solution to the present invention and it is only to clarify the technical solution to the present invention within and with no limitation to the scope of the invention. The scope of protection of the present invention is subject to claims.
  • The present invention provides a method of preparing silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles which is suitable for ordinary preparation to yield fiber-reinforced silver-based contact materials with no particular requirements on processing deformation and plasticity and ductility of reinforcing phase. A production process of the method is simple and easy. Besides, there is no particular requirement on equipments.
  • The silver-based electrical contact material prepared by the method of the present invention has a neat fibrous reinforcing material, wherein the fibrous structure of the reinforcing material is formed through directional arrangement of the reinforcing particles. The particles of the reinforcing powder have an average size of 5 nm to 30 µm. The particles can be of one material or a mixture of materials and mixed with silver powders in such a proportion as to obtain silver-coated particles after being processed with high energy ball milling. In a specific preparation, the reinforcing material ratio is determined according to practical needs.
  • In the present invention, Ag matrix powder is obtained through atomization and sieving. Particle sizes of the silver powders range from 100 meshes to 400 meshes. The matrix power can be obtained by other conventional arts.
  • In the present invention, specific processing operation parameters of steps comprising ball milling, powder mixing, cold isostatic pressing, sintering, hot pressing and hot extruding can be optional. One preferred series of parameters are stated as follows.
  • In step 1, the reinforcing powders are uniformly mixed with the silver matrix powders and then placed in a high energy ball mill for milling, wherein the parameters are set as follows. A weight ratio of the reinforcing powder to silver powder is between 0.5 and 3; a milling speed ranges from 180 rpm to 280 rpm; a milling time is 5 to 12 hours.
  • In step 2, the ball-milled composite powders obtained from step 1 and silver powders are poured into a powder mixing machine for mixing, wherein the parameters are set as follows. A weight ratio of the composite powders to silver powder is between 1 and 0.136; a rotation speed of the powder mixing machine is between 20 rpm and 30 rpm; the powder mixing lasts for 2 to 4 hours.
  • In step 3, the powder obtained from the step 2 is processed with cold isostatic pressing, wherein the parameters are set as follows. The isostatic pressure is between 100 and 500 MPa.
  • In step 4, the green body obtained by cold isostatic pressing is sintered, wherein the parameters are set as follows. A sintering temperature is between 600°C and 900°C. The sintering lasts for 5 to 9 hours.
  • In step 5, the green body obtained by sintering is processed with hot pressing, wherein the parameters are set as follows. A hot pressing temperature is between 500°C and 900°C. A hot pressing pressure is between 300 to 700 MPa. The hot pressing lasts for 1 min to 30 min.
  • In step 6, the green body obtained through hot pressing is hot extruded to obtain silver-based electrical contact materials with fiber-like arrangement of reinforcing nanoparticles wherein the parameters are set as follows. The green body is heated at a temperature between 600-900°C. An extrusion ratio is between 20 and 400 and an extrusion speed is between 5 to 20 cm/min. A pre-heating temperature of extruding moulds is between 300 and 500°C.
  • Preferred embodiments of the present invention are presented as follows to further illustrate the present invention.
  • Embodiment One
  • A preparation of AgSnO2 (12) contact material is taken as an example, referring to Fig. 1 and 2.
  • Step 1: obtaining a matrix of Ag powder having a particle size of 200 meshes, wherein the silver is third-level atomized and then sieved through a sieve of 200 meshes;
  • Step 2: 600g of reinforcing SnO2 powder having a particle size of 80 nm on average and 400 g of the Ag powder obtained from step 1 are uniformly mixed and then placed into a high energy ball mill for milling, wherein the ball mill rotates at 280 rpm and the ball milling lasts for 10 hours; a scanning electron photomicrograph of the generated composite powder is showed in Fig. 1;
  • Step 3: 1 Kg composite powder obtained from Step 2 and 4 Kg silver powder obtained from Step 1 are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at 30 rpm for 4 hours;
  • Step 4: the powder obtained from Step 3 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing, wherein the cold isostatic pressure is 100 MPa;
  • Step 5: the green body obtained through the cold isostatic pressing in Step 4 is sintered at 865°C for 5 hours;
  • Step 6: the sintered green body obtained from Step 5 is processed with hot pressing at 800°C under 500 MPa for 10 min; and
  • Step 7: the green body obtained through the hot pressing is processed with hot extrusion at 800°C, wherein an extrusion ratio is 225; an extrusion speed is 5 cm/min; and a pre-heating temperature of extruding moulds is 500°C.
  • According to the preferred embodiment one, the AgSnO2(12) contact material with obviously neat fibrous reinforcing SnO2 is finally obtained, wherein the fiber-like arrangement of SnO2 is formed through directional arrangement and connection of the nanoparticles of SnO2. A metallograph thereof is showed in Fig. 2. The obtained material has a tensile strength of 285 MPa, an electrical resistivity along the extrusion direction of 2.1 µΩ·cm and a hardness of 85 HV.
  • Embodiment Two
  • A preparation of AgCdO12 contact material is taken as an example.
  • Step 1: 600 g of reinforcement powder of CdO having particles of 1 µm on average and 200 g of Ag powder having a particle size of 400 meshes are uniformly mixed and then placed into a high energy ball mill for mixing, wherein the ball mill rotates at a speed of 240 rpm for 10 hours;
  • Step 2: 800 g of the composite powder obtained from the step 1 and 4200 g of silver powder having a particle size of 400 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 25 rpm for 4 hours;
  • Step 3: the powder obtained from Step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing under a cold isostatic pressure of 300 MPa;
  • Step 4: the green body obtained from cold isostatic pressing in Step 3 is sintered at 750 °C for 9 hours;
  • Step 5: the sintered green body obtained from Step 4 is processed with hot pressing at 800 °C under a hot pressing pressure of 300 MPa for 20 min; and
  • Step 6: the green body obtained from hot pressing is hot extruded into sheets at a hot extrusion temperature of 900 °C, wherein an extrusion ratio is 100; an extrusion speed is 10 cm/min; and a pre-heating temperature of extruding moulds is 300 °C.
  • According to the preferred embodiment two, AgCdO12 contact materials with a neat fiber-like arrangement of reinforcing CdO are finally obtained, wherein the fiber-like arrangement of CdO is formed through directional arrangement and connection of a number of CdO particles. The generated material has a tensile strength of 290 MPa, an electrical resistivity of 2.0 µΩ·cm and a hardness of 88 HV.
  • Embodiment Three
  • A preparation of AgZnO(8) contact material is taken as an example.
  • Step 1: 400 g of reinforcement powder of ZnO having particles of 100 nm on average and 800 g of Ag powder having a particle size of 400 meshes are uniformly mixed and placed in a high energy ball mill for mixing, wherein the ball mill rotates at a speed of 240 rpm for 5 hours;
  • Step 2: 1200 g of the composite powder obtained from Step 1 and 3800 g of silver powder having a particle size of 600 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 4 hours;
  • Step 3: the powder obtained from Step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing at a cold isostatic pressure of 100 MPa;
  • Step 4: the green body obtained from the cold isostatic pressing in Step 3 is sintered at 830 °C for 5 hours;
  • Step 5: the sintered green body obtained from Step 4 is processed with hot pressing at 830 °C under a hot pressing pressure of 700 MPa for 1 min; and
  • Step 6: the green body after the hot pressing is processed with hot extruding into sheets at a hot extrusion temperature of 800 °C, wherein an extrusion ratio is 324; an extrusion speed is 20 cm/min; and a pre-heating temperature of extruding moulds is 300 °C.
  • According to the preferred embodiment three, AgZnO(8) contact materials having a neat fiber-like arrangement of reinforcing ZnO are finally obtained, wherein the fiber-like arrangement of ZnO is formed through directional arrangement and connection of ZnO particles. The generated material has a tensile strength of 280 MPa, a resistivity of 1.9 µΩ·cm and a hardness of 85 HV.
  • Embodiment Four
  • A preparation of Ag-4ZnO-8SnO2 contact materials is taken as an example.
  • Step 1: a matrix of Ag powder having a particle size of 100 meshes is obtained, wherein the silver is third-level atomized and then sieved through a sieve of 100 meshes;
  • Step 2: 200g reinforcing powder of ZnO particles of an average size of 100 nm and 400g reinforcing powder of SnO2 particles of 80 nm on average and 400g Ag powder obtained from step 1 are uniformly mixed together and then placed into a high energy ball mill for milling, wherein the ball mill rotates at a speed of 280 rpm for 10 hours;
  • Step 3: 1000g composite powder obtained from step 2 and 4000g silver powder obtained from step 1 are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 4 hours;
  • Step 4: the powder obtained from Step 3 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing, wherein the cold isostatic pressure is 200 MPa;
  • Step 5: the green body after the cold isostatic pressing obtained from the step 4 is sintered at 865°C for 5 hours;
  • Step 6: the sintered green body obtained from Step 5 is processed with hot pressing at 800°C under 700 MPa for 10 min; and
  • Step 7: the green body obtained through hot pressing is processed with hot extrusion at 800°C, wherein an extrusion ratio is 400; an extrusion speed is 5 cm/min; and a pre-heating temperature of extruding moulds is 500°C.
  • According to the preferred embodiment four, the Ag-4ZnO-8SnO2 contact material with a neat fibre-like arrangement of reinforcing ZnO and SnO2 particles is finally obtained, wherein the fiber-like arrangement of ZnO and SnO2 is formed through directional arrangement and connection of nanoparticles of ZnO and SnO2. The generated material has a tensile strength of 255 MPa, an electrical resistivity along the extrusion direction of 2.0 µΩ·cm and a hardness of 85 HV.
  • Embodiment Five
  • A preparation of AgNi(25) contact materials is taken as an example.
  • Step 1: 500g reinforcing powder of Ni having particles of 10µm on average and 500g Ag powder having a particle size of 300 meshes are uniformly mixed and then placed in a high energy ball mill for mixing, wherein the ball mill rotates at a speed of 280 rpm for 8 hours;
  • Step 2: 1000g of the composite powder obtained from step 1 and 1000g of silver powder having a particle size of 400 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 2 hours;
  • Step 3: the powder obtained from step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing at a cold isostatic pressure of 200 MPa;
  • Step 4: the green body obtained through cold isostatic pressing in Step 3 is sintered at 860 °C for 7 hours;
  • Step 5: the sintered green body obtained from step 4 is processed with hot pressing at 800 °C under a hot pressing pressure of 400 MPa for 20 min; and
  • Step 6: the green body is hot-extruded into sheets at a hot extrusion temperature of 860 °C, wherein an extrusion ratio is 225; an extrusion speed is 10 cm/min; and a pre-heating temperature of extruding moulds is 500 °C.
  • According to the preferred embodiment five, the material of AgNi(25) with neat fiber-like arrangement of reinforcing Ni is finally obtained, wherein the fiber-like arrangement of Ni is formed through directional arrangement and connection of nanoparticles of Ni. The generated material has a tensile strength of 300 MPa, a electrical resistivity along an extrusion direction of 2.0 µΩ·cm and a hardness of 80 HV.
  • Embodiment Six
  • A preparation of AgFe7 contact materials is taken as an example.
  • Step 1: a matrix of Ag powder having a particle size of 100 meshes is obtained, wherein the silver is third-level atomized and then sieved through a sieve of 100 meshes;
  • Step 2: 350g of reinforcement powder of Fe having particles of 30 µm on average and 400g of the Ag powder obtained from step 1 are uniformly mixed and then placed into a high energy ball mill for milling wherein the ball mill rotates at a speed of 180 rpm for 12 hours;
  • Step 3; 750g of the composite powder obtained from Step 2 and 4250g of the silver powder obtained from Step 1 are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 20 rpm for 4 hours;
  • Step 4: the powder obtained from Step 3 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing, wherein the cold isostatic pressure is 500 MPa;
  • Step 5: the green body obtained from cold isostatic pressing in Step 4 is sintered at 900°C for 5 hours under protection of hydrogen atmosphere;
  • Step 6: the sintered green body obtained from Step 5 is processed with hot pressing at 900°C under 700 MPa for 30 min; and
  • Step 7: the green body after the hot pressing is processed with hot extruding at 700°C, wherein an extrusion ratio is 20; an extrusion speed is 10 cm/min; and a pre-heating temperature of extruding moulds is 400°C.
  • According to the sixth preferred embodiment, the material of AgFe7 with a neat fiber-like arrangement of reinforcing Fe is finally obtained, wherein the fiber-like arrangement of Fe is formed through directional arrangement and connection of nanoparticles of Fe. The generated material has a tensile strength of 310 MPa, an electrical resistivity along an extrusion direction of 1.9 µΩ·cm and a hardness of 75 HV.
  • Embodiment Seven
  • A preparation of AgZnO(6) contact material is taken as an example.
  • Step 1: 300g of reinforcing powder of ZnO having particles of 5nm on average and 300g of Ag powder having a particle size of 400 meshes are uniformly mixed and then placed in a high energy ball mill for milling, wherein the ball mill rotates at a speed of 180 rpm for 8 hours;
  • Step 2: 600g of the composite powder obtained from Step 1 and 4400g of silver powder having a particle size of 200 meshes are poured into a V-shaped powder mixing machine to be uniformly mixed, wherein the powder mixing machine rotates at a speed of 30 rpm for 4 hours;
  • Step 3: the powder obtained from Step 2 is placed into a plastic tube having a diameter of 90 cm and a length of 150 cm to be processed with cold isostatic pressing at a cold isostatic pressure of 300 MPa;
  • Step 4: the green body obtained from cold isostatic pressing in Step 3 is sintered at 600 °C for 7 hours;
  • Step 5: the sintered green body obtained from Step 4 is processed with hot pressing at 500 °C under a hot pressing pressure of 500 MPa for 10 min; and
  • Step 6: the green body obtained from hot pressing is hot-extruded into sheets at a hot extrusion temperature of 600 °C, wherein an extrusion ratio is 225; an extrusion speed is 5 cm/min; and a pre-heating temperature of extruding moulds is 500 °C.
  • According to the preferred embodiment seven, the AgZnO(6) contact material with a neat fiber-like arrangement of reinforcing ZnO is finally obtained, wherein the fiber-like arrangement of ZnO is formed through directional arrangement and connection of nanoparticles of ZnO. The generated material has a tensile strength of 270 MPa, a electrical resistivity along the extrusion direction of 1.85 µΩ·cm and a hardness of 80 HV.
  • It should be understood that although exemplary embodiments of the contact materials and methods of the invention are described by way of illustrating the invention, the invention includes all modification and equivalents of the disclosed embodiments of the preparation of silver-based contact materials with fiber-like arrangement of reinforcing nanoparticles falling within the scope of the appended claims.

Claims (8)

  1. A method for preparing a fibrous silver-based electrical contact material, comprising the following steps:
    (1) uniformly mixing reinforcing phase material powders with base silver powders, and then placing the mixed powders into a high energy ball milling tank for ball-milling, wherein the reinforcing phase material powders and the base silver powders are mixed in such a weight proportion between the reinforcing phase material powders and the base silver powders, that composite powders with silver-coated reinforcing phase material and aggregates thereof are obtained, wherein the weight ratio of the reinforcing phase material powders to the base silver powders is between 0.5 and 3; the ball mill rotates at a speed between 180 rpm and 280 rpm; and the ball milling lasts for 5 to 12 hours;
    (2) placing the composite powders obtained from step (1) and additional base silver powders into a powder mixing machine and mixing, wherein a weight ratio of the composite powders to the base silver powders is calculated according to composition of desired materials and size of fibrous structure, wherein the weight ratio of the composite powders and the additional base silver powders is between 1 and 1.036; the powder mixing machine rotates at a speed between 20 rpm and 30 rpm; the powder mixing lasts for 2 to 4 hours;
    (3) processing the mixed powders obtained from step (2) with cold isostatic pressing to obtain a green body;
    (4) sintering the green body obtained from step (3);
    (5) hot-pressing the green body obtained from step (4);
    (6) hot-extruding the green body obtained from step (5) to obtain the fibrous silver-based electrical contact material.
  2. The method, as recited in claim 1, wherein the step (1) adopts the base silver powders having a particle size between 100 meshes and 400 meshes.
  3. The method, as recited in claim 1, wherein in the step (1) the composite powders are any silver coated particle material that has been formed after high energy ball milling the reinforcing phase material powders with the base silver powders, and the reinforcing phase material powders are made of a single material or a mixture of several materials.
  4. The method, as recited in claim 1, wherein the step (3) comprises cold isostatic pressing under a cold isostatic pressure between 100 MPa and 500 MPa.
  5. The method, as recited in claim 1, wherein the step (4) comprises the sintering, wherein the sintering temperature is between 600 °C and 900 °C, and the sintering lasts for 5 hours to 9 hours.
  6. The method, as recited in claim 1, wherein the step (5) comprises the hot pressing, and the hot pressing temperature is between 500°C and 900°C; a hot pressing pressure is between 300 MPa and 700 MPa; and the hot pressing lasts for 1 min to 30 min.
  7. The method, as recited in claim 1, wherein the step (6) comprises hot extrusion, and the green body is hot-extruded under a temperature between 600 °C and 900 °C; the extrusion ratio is between 20 and 400; an extrusion speed is between 5 cm/min and 20 cm/min; and the pre-heating temperature of extruding moulds is between 300 °C and 500 °C.
  8. The method, as recited in claim 1, wherein powder particles of the reinforcing phase material powders have an average size of 5 nm to 30 µm.
EP11844208.6A 2010-12-03 2011-04-11 Method for preparing fibrous silver-based electrical contact material Active EP2537949B1 (en)

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Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002651B (en) * 2010-12-03 2013-04-03 温州宏丰电工合金股份有限公司 Method for preparing silver-based electrical contact material with fibrous structure
CN102312150A (en) * 2011-09-29 2012-01-11 浙江大学 Preparation method of Ag / Ti3SiC2 electric contact composite material
CN102808097B (en) * 2012-08-20 2014-04-16 温州宏丰电工合金股份有限公司 Silver/nickel/metallic oxide electrical contact material preparation method
CN105742083A (en) * 2014-12-11 2016-07-06 福达合金材料股份有限公司 Composite electric contact material with carbon nanotube enhancement, and preparation process thereof
CN107619962A (en) * 2017-08-31 2018-01-23 常州道博化工有限公司 A kind of preparation method of silver-based electric contact material
CN112059168B (en) * 2020-08-08 2022-07-05 浙江福达合金材料科技有限公司 Method for preparing silver metal oxide electric contact material based on nano silver wire modification and 3D gradient printing and product thereof
CN112095057B (en) * 2020-08-08 2021-09-17 福达合金材料股份有限公司 Nano silver wire modified silver-nickel electric contact material and preparation method thereof
CN112375931B (en) * 2020-10-19 2022-03-29 西安工程大学 Preparation method of tetrapod-like whisker reinforced silver zinc oxide contact material
CN112853235A (en) * 2020-12-31 2021-05-28 东莞正丰科技有限公司 Composite oxide electric contact material and preparation method thereof
CN114592159B (en) * 2022-03-22 2023-01-06 重庆材料研究院有限公司 Palladium alloy reinforced composite bonding wire and preparation method thereof
CN115870498A (en) * 2022-12-06 2023-03-31 浙江福达合金材料科技有限公司 Preparation method for improving bonding strength of flaky silver tin oxide electrical contact material
CN117127046B (en) * 2023-08-30 2024-04-16 昆明理工大学 SnO (tin oxide)2@In2O3Preparation method of reinforced silver-based composite material

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1320711A (en) * 2000-12-28 2001-11-07 西安交通大学 Nm-class Ag-base alloy as electric contact material and its preparing process
JP4410066B2 (en) * 2003-10-21 2010-02-03 三菱電機株式会社 Manufacturing method of electrical contact material
CN101034633A (en) * 2006-03-08 2007-09-12 中南大学 Electrical contact material doping AgSnO2 and its preparing method
CN101241804B (en) * 2007-11-23 2010-04-21 中南大学 A silver-ZnO electric contact and its making method
CN101608272A (en) * 2009-07-20 2009-12-23 温州宏丰电工合金有限公司 AgNi electrical contact material and preparation method thereof
CN101649401B (en) * 2009-07-20 2011-03-16 温州宏丰电工合金股份有限公司 Ag-Ni-oxide electrical contact material and preparation method thereof
CN101707145B (en) * 2009-09-24 2011-12-28 温州宏丰电工合金股份有限公司 Fiber structure silver-based electrical contact material and preparation method thereof
CN101707155B (en) * 2009-09-24 2011-11-09 温州宏丰电工合金股份有限公司 Method for preparing tin oxide reinforced silver-based electrical contact materials
CN102002651B (en) * 2010-12-03 2013-04-03 温州宏丰电工合金股份有限公司 Method for preparing silver-based electrical contact material with fibrous structure

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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EP2537949A4 (en) 2014-10-01

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