CN102031408A - Method for preparing silver-based oxide electrical contact material with fibrous structure - Google Patents
Method for preparing silver-based oxide electrical contact material with fibrous structure Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-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
- C22C32/001—Non-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
- C22C32/0015—Non-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
- H01H1/02374—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component CdO
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
- H01H1/02376—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2
Abstract
The invention discloses a method for preparing a silver-based oxide electrical contact material with a fibrous structure, which comprises the following steps of: 1, smelting a silver ingot, a metal ingot and an additive in a smelting furnace to form alloy liquid, and performing atomization comminuting; 2, performing high energy ball milling; 3, performing internal oxidation; 4, performing high energy ball milling granulation and sieving; 5, pouring ball milling granulated and sieved powder and a substrate into a powder mixer for powder mixing; 6, performing cold isostatic pressing; 7, performing sintering; 8, performing hot pressing; and 9, performing hot extrusion. In the method, regardless of the magnitude of machining deformation, the silver-based oxide electrical contact material with the remarkable fibrous structure can be obtained; the plasticity and ductility of a wild phase are not required; the method is simple and convenient to operate; equipment is not required specially; and simultaneously, the wild phase is not required to be externally purchased, so the production cost is greatly saved. The material prepared by the method has greatly improved resistance to fusion welding, greatly improved arc ablation resistance, greatly improved electric conductivity and high machinability.
Description
Technical field
The present invention relates to a kind of preparation method of electrical contact material, specifically, that relate to is a kind of preparation method of fibrous tissue structure ag-oxide contact material.
Background technology
Development along with high voltage power transmission and transforming net large vol, ultra-high voltage, the raising that low-voltage distribution system and Controlling System require automatization level, sensitivity level, and the modernization of electronic industrial products, electrical contact is proposed more and more high functional requirement and long-life service requirements.For this reason, constantly there are new silver-based composite material and preparation technology to be developed.Fibrous tissue structure ag-oxide matrix material becomes the focus of Recent study because of having good resistance fusion welding and arc ablation resistance ability and good processing properties.At present, because fibrous tissue structure ag-oxide material preparation process complexity, the cost height, and continuous fibre ag-oxide material is difficult to shortcomings such as secondary processing, limited the promotion and application of fibrous tissue structure ag-oxide material greatly.Therefore, the preparation method who develops a kind of ag-oxide contact material of simple, practical and fibrous tissue structure that can large-scale production is a focus of current research, also is a difficult point.
By retrieval, both at home and abroad about the research report of the ag-oxide contact material aspect of fibrous tissue structure, as: Chinese invention patent: fiber structure silver-based electrical contact material and preparation method thereof, application number: 200910196283.0, publication number: CN101707145A.
At present, preparation method about the ag-oxide contact material of fibrous tissue structure has two kinds substantially: the one, and traditional powder metallurgy sintered extrusion process and improve fashion of extrusion on this basis, increase the method for machining deformation amount, the main technique flow process is: mix powder → briquetting → sintering → extruding → drawing → annealing → drawing → finished product.The prepared filamentary structure of this method is not obvious, is not suitable for the relatively poor wild phase of plasticity and ductility, and the macrobead that has a wild phase exists, and influences the product use properties.The 2nd, base substrate designs the method that combines with pressing method in advance; promptly in advance the wild phase silk material of some amount is fixed in the matrix with mould; wait the method [document CN101707145A] of static pressure, sintering and extruding then successively; though this method can obtain obviously and the successive filamentary structure; but technology is comparatively complicated; to prepare the silk material of the money base that contains wild phase in advance and be fixed in the matrix with mould; and for the requirement that has of the plasticity of wild phase silk material and ductility, large-scale production is difficulty comparatively.
Summary of the invention
The present invention is directed to deficiency and defective that above-mentioned prior art exists, a kind of preparation method of fibrous tissue structure ag-oxide contact material is provided, no matter big or little in the machining deformation amount this method is, can obtain having obvious filamentary structure ag-oxide electrical contact material, and do not require for wild phase plasticity and ductility, technology is simple, easy to operate, equipment there is not particular requirement, simultaneously, do not need outsourcing wild phase (oxide compound), save production cost greatly.Material resistance fusion welding, arc ablation resistance performance and the specific conductivity of the inventive method preparation all are greatly improved, and processing characteristics is very good.
For realizing above-mentioned purpose, the technical solution used in the present invention is:
The invention provides a kind of preparation method of fibrous tissue structure ag-oxide contact material, may further comprise the steps:
The first step places smelting furnace to be smelted into alloy liquid silver ingot, ingot metal and additive, carries out powder by atomization then.Wherein: metal can form alloy, reductibility than the strong metal that can spontaneous oxidation of Ag with silver for all, and metal species is one or more; Silver ingot and ingot metal part by weight require required calculating to obtain according to required preparation material composition and following process; Additive level obtains according to the metal content for the treatment of oxidation and the required calculating of subsequent technique, and additive is in Bi, In, Cu and the rare earth element one or more.
In second step, the first step is obtained the atomized alloy powder place the high-energy ball milling jar to carry out ball milling.
In the 3rd step, the powder that second step was obtained carries out interior oxidation.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the high-energy ball milling granulation successively and sieves, and fails to place high energy ball mill to reprocess again again by the macrobead powder of screen cloth, and then sieves.
In the 5th step, composite granule behind the sieve that the 4th step was obtained and matrix silver powder are poured into to mix in the powder machine and are mixed powder, and wherein: composite granule and matrix silver powder part by weight are according to required preparation material composition and the required calculating acquisition of fiber size.
In the 6th step, the powder that the 5th step was obtained carries out isostatic cool pressing.
In the 7th step, the base substrate that isostatic cool pressing is obtained carries out sintering.
In the 8th step, the base substrate that sintering is obtained carries out hot pressing.
In the 9th step, the base substrate that hot pressing is obtained carries out hot extrusion, obtains fibrous tissue structure ag-oxide electrical contact material.
The fibrous tissue structure ag-oxide electrical contact material of method for preparing of the present invention, wild phase (oxide compound) material with tangible fibrous arrangement, wherein the structure of fibrous tissue of wild phase (oxide compound) material is arranged by its grain orientation and is formed, and the wild phase particulate material is a kind of material or multiple material blends, depends on the metal species number in the ingot metal in the first step.
Institute of the present invention employing method combines big plastic processing deformation with the mechanical alloying of traditional material in the past, and oxidation preparation method all has remarkable difference in simple, the method that the present invention adopts is: at first by silver, metal and additive are atomized, obtain superfine atomized alloy powder; Again alloy powder is carried out high-energy ball milling, high-energy ball milling makes alloy powder roll in the macro-energy collision and obtains refinement, has formed evenly and the superfine composite granule; Then superfine composite granule behind the ball milling is carried out interior oxidation; Again the composite granule after the oxidation is carried out successively ball milling and sieve the aggregate of formation cladding (Ag is coated on above the oxide particle).Then aggregate and matrix Ag powder are carried out uniform mixing by material composition prescription aequum, carry out isostatic cool pressing, sintering, hot pressing, hot extrusion successively.Cladding flows with remollescent Ag in the Ag matrix in extrusion process, because the coating of Ag makes oxide compound wild phase material be easy to be drawn back, and aligns along the direction of extrusion and to form filamentary structure.This method makes to have tangible fibrous wild phase weave construction in the material structure, its arc ablation resistance can improve 10-20% by the simple particles dispersed enhanced same material system contact material of force rate, improve 5-10% along direction of extrusion electric conductivity, resistance fusion welding improves 10-20%, and electric life has improved 10-25%; And have good processing characteristics and be applicable to large-scale production.
Embodiment
Below technical scheme of the present invention is further described, the following description is only for understanding the usefulness of technical solution of the present invention, is not used in to limit scope of the present invention, protection scope of the present invention is as the criterion with claims.
The invention provides the preparation method of the ag-oxide electrical contact material of above-mentioned fibrous tissue structure, be applicable to the preparation of common fiber reinforcement ag-oxide matrix material, no matter big or little in the machining deformation amount this method is, can obtain having obvious filamentary structure ag-oxide electrical contact material, and do not require for wild phase plasticity and ductility, technology is simple, and is easy to operate, with low cost, equipment there is not particular requirement.
The ag-oxide electrical contact material that obtains according to the inventive method, has tangible fibrous wild phase (oxide compound) material, wherein the structure of fibrous tissue of wild phase (oxide compound) material is arranged by its grain orientation and is formed, and wild phase (oxide compound) material is a kind of material or multiple material blends, depends on the kind and the proportioning of institute's containing metal in the ingot metal in early stage.
Among the present invention, steps such as the powder by atomization of design, ball milling, interior oxidation, ball milling granulation, mixed powder, isostatic cool pressing, sintering, hot pressing and hot extrusion, the parameter of concrete technological operation can be selected, such as:
In the first step, place smelting furnace to carry out melting Ag ingot, ingot metal and additive, then alloy liquid is carried out powder by atomization.Its metal can form alloy, reductibility than the strong metal that can spontaneous oxidation of Ag with silver for all, and metal species is one or more; Additive is one or more in Bi, In, Cu and the rare earth element.Wherein parameter can adopt: Ag ingot and ingot metal part by weight are between 3-0.5; Additive metal content calculates acquisition according to the weight that its oxide weight is no more than wild phase in the ag-oxide (metal oxide except that the additive oxide compound), and concrete kind is according to the required calculating acquisition of material composition.
In second step, the atomized powder that the first step is obtained carries out high-energy ball milling.Rotational speed of ball-mill is between 180 rev/mins-300 rev/mins; The ball milling time was at 5-10 hour; Ratio of grinding media to material (being ball and powder part by weight) is between 10-20.
In the 3rd step, the powder behind the ball milling of second step acquisition is carried out interior oxidation.Wherein parameter can adopt: oxidizing temperature is between 300 ℃-700 ℃; Oxidization time is between 5-15 hour, and oxygen is pressed between the 0.3-1.5MPa.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the high-energy ball milling granulation successively and sieves, and fails to place ball mill to reprocess again again by the macrobead of screen cloth, and then sieves.Wherein parameter can adopt: rotational speed of ball-mill is between 180 rev/mins-280 rev/mins; The ball milling time was at 5-15 hour; Ratio of grinding media to material (being ball and powder part by weight) is between 10-20; The order number that is sieved is between 100 orders-400 order.
In the 5th step, composite granule that the 4th step was obtained and silver powder are poured into to mix in the powder machine and are mixed powder, and composite granule and matrix silver powder part by weight are according to the required calculating acquisition of required preparation material composition.Wherein parameter can adopt: mix powder machine rotating speed between 20 rev/mins-40 rev/mins; Mix the powder time between 2-6 hour, matrix silver powder granularity is between the 50-400 order.
In the 6th step, the powder that the 5th step was obtained carries out isostatic cool pressing.Wherein parameter can adopt: wait static pressure pressure between 100-400Mpa.
In the 7th step, the base substrate that isostatic cool pressing is obtained carries out sintering.Wherein parameter can adopt: sintering temperature is between 600 ℃-800 ℃; Sintering time is between 5-10 hour.
In the 8th step, the base substrate that sintering is obtained carries out hot pressing.Wherein parameter can adopt: hot pressing temperature is between 600 ℃-850 ℃; Hot pressing pressure is between 200-700MPa; Hot pressing time is between the 5min-30min.
In the 9th step, the base substrate that hot pressing is obtained carries out hot extrusion, obtains filamentary structure ag-oxide electrical contact material.Wherein parameter can adopt: the base substrate Heating temperature is between 700-900 ℃; Extrusion ratio is between 80-400, and extrusion speed is between 5-15cm/min; The extrusion mould preheating temperature is between 300-500 ℃.
Below embodiment by concrete application come the detailed technological operation of the present invention is described.
Embodiment one
With preparation AgSnO
2(10) contact material is an example
The first step places smelting furnace to carry out melting Ag ingot 300g, Sn ingot 600g and In additive 70g, then alloy liquid is carried out powder by atomization.
Second step obtained powdered alloy with the first step and places the high-energy ball milling jar to carry out ball milling, and rotational speed of ball-mill is at 300 rev/mins; 10 hours ball milling time; Ratio of grinding media to material is 10.
In the 3rd step, the powder behind the ball milling of second step acquisition is carried out interior oxidation, 700 ℃ of oxidizing temperatures; Oxidization time 5 hours, oxygen is pressed 1.5MPa.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the ball milling granulation successively and sieves, and fails macrobead by screen cloth to turn back in the ball mill and process again, and then sieves.200 rev/mins of rotational speed of ball-mill; 12 hours ball milling time; Ratio of grinding media to material is 15; Several 200 orders of the order that is sieved.
In the 5th step, composite granule and 400 order silver powder 6467g that the 4th step was obtained pour in the mixed powder machine of " V " type, carry out evenly mixing powder.Rotary speed is 40 rev/mins when mixing powder, 6 hours time.
In the 6th step, the powder that the 3rd step the was obtained diameter of packing into is 9cm, in the length 30cm plastic cement tube, carries out isostatic cool pressing, isostatic cool pressing pressure 100MPa.
In the 7th step, the isostatic cool pressing base substrate that the 4th step was obtained carries out sintering, 800 ℃ of sintering temperatures, sintering 5 hours.
In the 8th step, the sintered body that the 5th step was obtained carries out hot pressing, 850 ℃ of temperature, hot pressing pressure 200MPa, hot pressing time 15 minutes.
In the 9th step, the base substrate that hot pressing is good carries out hot extrusion, 900 ℃ of extrusion temperatures, extrusion ratio 300, extrusion speed 5cm/min, 400 ℃ of extrusion mould preheating temperatures.
The final acquisition of present embodiment has obvious SnO
2The AgSnO of fibrous tissue structure
2(10) material, wherein, SnO
2The fibrous tissue structure is by a lot of tiny SnO
2The grain orientation arrangement is formed by connecting.The Tensile strength that obtains is 288Mpa; Along direction of extrusion resistivity is 2.2 μ Ω .cm; Hardness is 88HV.
Embodiment two
With preparation AgCdO12 contact material is example
The first step places smelting furnace to carry out melting Ag ingot 300g, Cd ingot 300g and Cu additive 15g, then alloy liquid is carried out powder by atomization.
Second step obtained powdered alloy with the first step and places the high-energy ball milling jar to carry out ball milling, and rotational speed of ball-mill is at 180 rev/mins; 10 hours ball milling time; Ratio of grinding media to material 12.
In the 3rd step, the powder behind the ball milling of second step acquisition is carried out interior oxidation, 300 ℃ of oxidizing temperatures; Oxidization time 15 hours, oxygen is pressed 0.3MPa.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the ball milling granulation successively and sieves, and fails macrobead by screen cloth to turn back in the ball mill and process again, and then sieves.280 rev/mins of rotational speed of ball-mill; 5 hours ball milling time; Ratio of grinding media to material 20; Several 100 orders of the order that is sieved.
In the 5th step, powder and granularity that the 4th step was obtained are that 400 purpose silver powder 2196g pour in the mixed powder machine of " V " type together, carry out evenly mixing powder.Rotary speed is 20 rev/mins when mixing powder, 4 hours time.
In the 6th step, the powder that the 5th step the was obtained diameter of packing into is 9cm, in the length 10cm plastic cement tube, carries out isostatic cool pressing, isostatic cool pressing pressure 100MPa.
In the 7th step, the isostatic cool pressing base substrate that the 6th step was obtained carries out sintering, 750 ℃ of sintering temperatures, sintering 9 hours.
In the 8th step, the sintered body that the 7th step was obtained carries out hot pressing, 600 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 20min.
In the 9th step, the base substrate that hot pressing is good carries out hot extrusion, is squeezed into sheet material, 900 ℃ of extrusion temperatures, extrusion ratio 300, extrusion speed 10cm/min, 300 ℃ of extrusion mould preheating temperatures.
The AgCdO12 material that the final acquisition of present embodiment has obvious CdO fibrous tissue structure, wherein, CdO fibrous tissue structure is to be arranged by a lot of tiny CdO grain orientations to be formed by connecting.The Tensile strength that obtains is 292Mpa; Along direction of extrusion resistivity is 2.0 μ Ω .cm; Hardness is 83HV.
Embodiment three
With preparation AgZnO (8) contact material is example
The first step places smelting furnace to carry out melting Ag ingot 600g, Zn ingot 200g and Bi additive 18g, then alloy liquid is carried out powder by atomization.
Second step obtained powdered alloy with the first step and places the high-energy ball milling jar to carry out ball milling, and rotational speed of ball-mill is at 300 rev/mins; 5 hours ball milling time; Ratio of grinding media to material 15.
In the 3rd step, the powder behind the ball milling of second step acquisition is carried out interior oxidation, 500 ℃ of oxidizing temperatures; Oxidization time 12 hours; Oxygen is pressed 0.5MPa.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the ball milling granulation successively and sieves, and fails macrobead by screen cloth to turn back in the ball mill and process again, and then sieves.180 rev/mins of rotational speed of ball-mill; 15 hours ball milling time; Ratio of grinding media to material 10; Several 300 orders of the order that is sieved.
In the 5th step, composite granule and granularity that the 4th step was obtained are that 50 purpose silver powder 2246g pour in the mixed powder machine of " V " type together, carry out evenly mixing powder.Rotary speed is 30 rev/mins when mixing powder, 2 hours time.
In the 6th step, the powder that the 5th step the was obtained diameter of packing into is 9cm, in the length 15cm plastic cement tube, carries out isostatic cool pressing, isostatic cool pressing pressure 400MPa.
In the 7th step, the isostatic cool pressing base substrate that the 6th step was obtained carries out sintering, 600 ℃ of sintering temperatures, sintering 8 hours.
In the 8th step, the sintered body that the 7th step was obtained carries out hot pressing, 830 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 5 minutes.
In the 9th step, the base substrate that hot pressing is good carries out hot extrusion, 700 ℃ of extrusion temperatures, extrusion ratio 80, extrusion speed 15cm/min, 300 ℃ of extrusion mould preheating temperatures.
AgZnO (8) material that the final acquisition of present embodiment has obvious ZnO fibrous tissue structure, wherein, ZnO fibrous tissue structure is to be arranged by a lot of tiny nano-ZnO grain orientations to be formed by connecting.The Tensile strength that obtains is 285Mpa; Along direction of extrusion resistivity is 2.1 μ Ω .cm; Hardness is 85HV.
Embodiment four
With preparation Ag-4ZnO-8SnO
2Contact material is an example
The first step is that 26g, In are that 20g places smelting furnace to carry out melting with Ag ingot 600g, Zn ingot 102g, Sn ingot 200g and addition of C e, then alloy liquid is carried out powder by atomization.
Second step obtained powdered alloy with the first step and places the high-energy ball milling jar to carry out ball milling, and rotational speed of ball-mill is at 280 rev/mins; 10 hours ball milling time; Ratio of grinding media to material is 20.
In the 3rd step, the powder behind the ball milling of second step acquisition is carried out interior oxidation, 500 ℃ of oxidizing temperatures; Oxygen oxidization time 15 hours; Oxygen is pressed 1.5MPa.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the ball milling granulation successively and sieves, and fails macrobead by screen cloth to turn back in the ball mill and process again, and then sieves.280 rev/mins of rotational speed of ball-mill; 15 hours ball milling time; Ratio of grinding media to material is 20; Several 400 orders of the order that is sieved.
In the 5th step, composite granule and granularity that the 4th step was obtained are that 300 purpose silver powder 2136g pour in the mixed powder machine of " V " type together, carry out evenly mixing powder.Rotary speed is 30 rev/mins when mixing powder, 4 hours time.
In the 6th step, the powder that the 5th step the was obtained diameter of packing into is 9cm, in the length 15cm plastic cement tube, carries out isostatic cool pressing, isostatic cool pressing pressure 300MPa.
In the 7th step, the isostatic cool pressing base substrate that the 6th step was obtained carries out sintering, 800 ℃ of sintering temperatures, sintering 10 hours.
In the 8th step, the sintered body that the 7th step was obtained carries out hot pressing, 850 ℃ of temperature, hot pressing pressure 700MPa, hot pressing time 10min.
In the 9th step, the base substrate that hot pressing is good carries out hot extrusion, 900 ℃ of extrusion temperatures, extrusion ratio 400, extrusion speed 5cm/min, 500 ℃ of extrusion mould preheating temperatures.
The final acquisition of present embodiment has obvious ZnO and SnO
2The Ag-4ZnO-8SnO of fibrous tissue structure
2The contact material material, wherein, ZnO and SnO
2The fibrous tissue structure is respectively by a lot of tiny ZnO and SnO
2Nano particle aligns and is formed by connecting.The Tensile strength that obtains is 260Mpa; Along direction of extrusion resistivity is 2.3 μ Ω .cm; Hardness is 89HV.
Embodiment five
With preparation AgSnO
2(6) In
2O
3(6) contact material is an example
The first step is that 629g places smelting furnace to carry out melting with Ag ingot 1000g, Sn ingot 600g and additive In, then alloy liquid is carried out powder by atomization.
Second step obtained powdered alloy with the first step and places the high-energy ball milling jar to carry out ball milling, and rotational speed of ball-mill is at 280 rev/mins; 10 hours ball milling time; Ratio of grinding media to material is 15.
In the 3rd step, the powder behind the ball milling of second step acquisition is carried out interior oxidation, 600 ℃ of oxidizing temperatures; Oxidization time 8 hours, oxygen is pressed 1MPa.
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the ball milling granulation successively and sieves, and fails macrobead by screen cloth to turn back in the ball mill and process again, and then sieves.200 rev/mins of rotational speed of ball-mill; 10 hours ball milling time; Ratio of grinding media to material is 20; Several 300 orders of the order that is sieved.
In the 5th step, composite granule and 400 order silver powder 10167g that the 4th step was obtained pour in the mixed powder machine of " V " type, carry out evenly mixing powder.Rotary speed is 40 rev/mins when mixing powder, 6 hours time.
In the 6th step, the powder that the 3rd step the was obtained diameter of packing into is 9cm, in the length 25cm plastic cement tube, carries out isostatic cool pressing, isostatic cool pressing pressure 300MPa.
In the 7th step, the isostatic cool pressing base substrate that the 4th step was obtained carries out sintering, 800 ℃ of sintering temperatures, sintering 5 hours.
In the 8th step, the sintered body that the 5th step was obtained carries out hot pressing, 850 ℃ of temperature, hot pressing pressure 500MPa, hot pressing time 30 minutes.
In the 9th step, the base substrate that hot pressing is good carries out hot extrusion, 900 ℃ of extrusion temperatures, extrusion ratio 300, extrusion speed 5cm/min, 400 ℃ of extrusion mould preheating temperatures.
The final acquisition of present embodiment has obvious SnO
2With additive oxide compound In
2O
3The AgSnO of fibrous tissue structure
2(12) material, wherein, SnO
2With oxide compound In
2O
3The fibrous tissue structure is respectively by a lot of tiny SnO
2Particle and In
2O
3The grain orientation arrangement is formed by connecting, and the Tensile strength of acquisition is 290Mpa; Along direction of extrusion resistivity is 2.9 μ Ω .cm; Hardness is 89HV.
The above only is part preferred embodiment of the present invention, is not that technical scope of the present invention is done any restriction, and the present invention can also be applicable to the preparation of the fibrous tissue structure ag-oxide matrix material of other composition proportion.All any modifications of making within the spirit and principles in the present invention are equal to replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a fibrous tissue structure ag-oxide electrical contact material is characterized in that may further comprise the steps:
The first step places smelting furnace to be smelted into alloy liquid silver ingot, ingot metal and additive, carries out powder by atomization then and handles; Wherein: metal can form alloy, reductibility than the strong metal that can spontaneous oxidation of Ag with silver for all, and metal species is one or more; Silver and other weight metal ratio require required calculating to obtain according to required preparation material composition and following process in the alloy powder; Additive level obtains with metal content and the required calculating of subsequent technique, and additive is in Bi, In, Cu and the rare earth element one or more;
In second step, the first step is obtained the atomized alloy powder place the high-energy ball milling jar to carry out ball milling;
In the 3rd step, the powder that second step was obtained carries out interior oxidation;
In the 4th step, the powder after the interior oxidation that the 3rd step was obtained carries out the high-energy ball milling granulation successively and sieves, and fails to place ball mill to reprocess again again by the macrobead of screen cloth, and then sieves;
In the 5th step, composite granule that the 4th step was obtained and matrix silver powder are poured into to mix in the powder machine and are mixed powder, and wherein: composite granule and matrix silver powder part by weight are according to required preparation material composition and the required calculating acquisition of fiber size;
In the 6th step, the powder that the 5th step was obtained carries out isostatic cool pressing;
In the 7th step, the base substrate that isostatic cool pressing is obtained carries out sintering;
In the 8th step, the base substrate that sintering is obtained carries out hot pressing;
In the 9th step, the base substrate that hot pressing is obtained carries out hot extrusion, obtains fibrous tissue structure ag-oxide electrical contact material.
2. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1, it is characterized in that, in the first step, described Ag ingot and ingot metal part by weight are between 3-0.5, and the oxide compound of described additive metal is no more than 1% of ag-oxide gross weight.
3. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1, it is characterized in that, rotational speed of ball-mill is between 180 rev/mins-300 rev/mins described in second step, and the ball milling time, ratio of grinding media to material was between 10-20 at 5-10 hour; Rotational speed of ball-mill is between 180 rev/mins-280 rev/mins described in the 4th step, and the ball milling time, ratio of grinding media to material was between 10-20 at 5-15 hour, and the order number that is sieved is between 100 orders-400 order.
4. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1, it is characterized in that in the 3rd step, described interior oxidizing temperature is between 300 ℃-700 ℃, oxidization time is between 5-15 hour, and oxygen is pressed between the 0.3-1.5MPa.
5. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1, it is characterized in that in the 5th step, described mixed powder machine rotating speed is between 20 rev/mins-40 rev/mins, mix the powder time between 2-6 hour, matrix silver powder granularity is between the 50-400 order.
6. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1 is characterized in that, in the 6th step, the described static pressure pressure that waits is between 100-400Mpa.
7. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1 is characterized in that, in the 7th step, and described sintering, wherein: sintering temperature is between 600 ℃-800 ℃, and sintering time is between 5-10 hour.
8. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1, it is characterized in that, in the 8th step, described hot pressing, wherein: hot pressing temperature is between 600 ℃-850 ℃, hot pressing pressure is between 200-700MPa, and hot pressing time is between the 5min-30min.
9. the preparation method of a kind of fibrous tissue structure ag-oxide electrical contact material as claimed in claim 1 is characterized in that, in the 9th step, described hot extrusion, wherein: the base substrate Heating temperature is between 700-900 ℃, and extrusion ratio is between 80-400, and extrusion speed is between 5-15cm/min; The extrusion mould preheating temperature is between 300-500 ℃.
10. fibrous tissue structure ag-oxide electrical contact material that adopts the preparation of the described method of claim 1, it is characterized in that, the ag-oxide electrical contact material of described fibrous tissue structure has tangible fibrous wild phase material, and wherein the fibrous tissue structure of wild phase material is arranged by its grain orientation and formed; The wild phase material is a kind of material or multiple material blends, depends on the species number and the proportioning of institute's containing metal in the ingot metal in early stage.
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| CN 201010620071 CN102031408B (en) | 2010-12-30 | 2010-12-30 | Method for preparing silver-based oxide electrical contact material with fibrous structure |
| PCT/CN2011/000633 WO2012088735A1 (en) | 2010-12-30 | 2011-04-11 | Method for preparing fibrous silver-based oxide electrical contact material |
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| CN 201010620071 CN102031408B (en) | 2010-12-30 | 2010-12-30 | Method for preparing silver-based oxide electrical contact material with fibrous structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102808097A (en) * | 2012-08-20 | 2012-12-05 | 温州宏丰电工合金股份有限公司 | Silver/nickel/metallic oxide electrical contact material preparation method |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN108149122A (en) * | 2017-12-27 | 2018-06-12 | 洛阳神佳窑业有限公司 | A kind of preparation method of silver-base alloy contact material |
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| CN112609247B (en) * | 2020-11-06 | 2022-05-10 | 东北大学 | Method for preparing silver tin oxide electric contact material by electrostatic spinning method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101651051A (en) * | 2009-07-20 | 2010-02-17 | 温州宏丰电工合金有限公司 | Cadmium-oxygen-silver multicomponent electrical contact material and preparation method thereof |
| CN101649401A (en) * | 2009-07-20 | 2010-02-17 | 温州宏丰电工合金有限公司 | Ag-Ni-oxide electrical contact material and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5647529A (en) * | 1979-09-22 | 1981-04-30 | Matsushita Electric Works Ltd | Manufacture of electric contact material |
| JPH06104873B2 (en) * | 1986-07-08 | 1994-12-21 | 富士電機株式会社 | Silver-metal oxide contact material and manufacturing method thereof |
| JP4410066B2 (en) * | 2003-10-21 | 2010-02-03 | 三菱電機株式会社 | Manufacturing method of electrical contact material |
| CN101608279B (en) * | 2009-07-20 | 2012-10-03 | 温州宏丰电工合金股份有限公司 | Silver oxide electrical contact material and preparation method thereof |
| 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 |
-
2010
- 2010-12-30 CN CN 201010620071 patent/CN102031408B/en active Active
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101651051A (en) * | 2009-07-20 | 2010-02-17 | 温州宏丰电工合金有限公司 | Cadmium-oxygen-silver multicomponent electrical contact material and preparation method thereof |
| CN101649401A (en) * | 2009-07-20 | 2010-02-17 | 温州宏丰电工合金有限公司 | Ag-Ni-oxide electrical contact material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102808097A (en) * | 2012-08-20 | 2012-12-05 | 温州宏丰电工合金股份有限公司 | Silver/nickel/metallic oxide electrical contact material preparation method |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN108149122A (en) * | 2017-12-27 | 2018-06-12 | 洛阳神佳窑业有限公司 | A kind of preparation method of silver-base alloy contact material |
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| WO2012088735A1 (en) | 2012-07-05 |
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