CN101982558B - Grain refinement technology of silver-nickel electrical contact material and grain refinement technology of silver tin oxide electrical contact material - Google Patents
Grain refinement technology of silver-nickel electrical contact material and grain refinement technology of silver tin oxide electrical contact material Download PDFInfo
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- CN101982558B CN101982558B CN2010105589781A CN201010558978A CN101982558B CN 101982558 B CN101982558 B CN 101982558B CN 2010105589781 A CN2010105589781 A CN 2010105589781A CN 201010558978 A CN201010558978 A CN 201010558978A CN 101982558 B CN101982558 B CN 101982558B
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Abstract
The invention discloses a grain refinement technology of a silver-nickel electrical contact material and a grain refinement technology of a silver tin oxide electrical contact material, belonging to the technical field of a metal-base composite material, which is characterized in that a uniform AgNi wire and a uniform AgSnO2 wire with a certain diameter specification are firstly drawn and thrust into short wires with the length of 1cm-5cm; the thrust wires are pressed into spindles after heat treatment; the spindles are made into the wire through sintering, upsetting and a plurality of hot extrusion, wherein, grain shearing deformation and grain refinement are realized by upsetting before extrusion, so tissue components in an extrusion material (110) are effectively reduced and oxide films on the boundary of powder grains are crushed and dispersed; and a plurality times of extrusion are adopted for extrusion deformation under large hydrostatic pressure, which is beneficial to elimination of tiny holes and combination of material points of the material so that the density and the shaping of the product are enhanced. In the course of extrusion, grain refinement is more obvious, the gross area of the grain boundary is increased, the capability for blocking crack expansion is enhanced, and the concentration of impurities on the grain boundary is reduced, thus avoiding brittle fracture along the grain boundary.
Description
Technical field
The present invention relates to a kind of preparation method of contact material, belong to the metal-base composites technical field.
Background technology
AgNi and AgSnO
2Electrical contact material is mainly used in the electric switches such as rly., contactor, motor mover, switch.These two kinds of materials are present environment-friendly materials the most frequently used in low-voltage apparatus, and can scale operation.Miniaturized development along with rly. also has resistance fusion welding that the requirement of renewal is also arranged to contact material.Existing AgNi matrix material is to adopt conventional silver nickel to mix the material of powder preparation; There is a nickel thick instable defective that causes electrical property; All researchs in the recent period mainly are through coming the refinement particle with chemical method such as codeposition, coating method, or add its electrical property of additive method raising.Wherein chemical method have a poor working environment, limited by traditional powder mixing method and add the additive method, additive composition ratio is limited, and causes reunion easily, so do not reach best effect.Adopt traditional mixed powder sintering extrusion process for silver tin oxide material, granules of stannic oxide is thick, and material compactness is bad; Additive composition serious agglomeration, single employing coats method, codeposition chemical method, and the strength of materials is poor; Single employing internal oxidation preparation; The barren district of oxide buildup and oxide compound appears in materials processed difficulty easily, is difficult to guarantee the stability of material.
Through retrieval analysis, make a general survey of the research of home and abroad, nearly all method is through the different processes method, adds the resistance fusion welding that one or more different additives attempt to improve material.Specific as follows:
(1) codeposition silver nickel 10 contact materials and application thereof; Electrical alloy collection the 2nd phase of nineteen ninety
(2) Ag-Ni-Y alloy organizing and performance study; Kunming University of Science and Technology's journal
(3) Ag-10Ni alloy mechanize; Precious metal 1,998 19 (4)
(4) electrical contact material used of a kind of low-voltage apparatus; CN10036547C
(5) a kind of preparation method of silver nickel composite material; CN101139663
(6) silver-nickel electric contact producing technology; CN1848323
(7) silver-nickel-based electrical contact material that a kind of resistance fusion welding is high and preparation method thereof; CN1478913
(8) nanometer silver tin oxide electric contact and preparation method thereof; CN1417817
(9) a kind of preparation of silver-tin oxide material; CN1425790
(10) a kind of preparation method of siller tin oxide electric contact; CN1101510479
(11) additive is to the research of the nanocrystalline electrical contact material performance of siller tin oxide; Shanghai non-ferrous metal 2007 3 phase documents (1), (5), (6) are to come the nickel particle of refinement silver nickel-base composite material to improve the temperature rise of contact material through codeposition or codeposition-ball milled; Problems such as resistance fusion welding; This method adopts chemical method, causes environmental pollution easily.Document (3) though ability crystal grain thinning mechanical alloying production capacity is low, is introduced impurity through ball milling prepared by mechanical alloy silver nickel 10 easily.Document (2), (4), (7), mainly be to improve the performance of material through adding micro substances such as one or more additives Y, W or diamond, but it is thick still to fail to solve the nickel particle, the additive phenomenon that is evenly distributed makes not reach best effect.
Document (8) and (11) are respectively to mix the method that TiO2, REE reach grain refinement effect and coat granules of stannic oxide at silver ammino solution through electroless plating; These two kinds of methods all belong to chemical process; The intensity of prepared material is low, and compactness is poor; Document (9) adopts atomization to prepare material, this method different oxidation state, and bill of material reveals different characteristic, and processing difficulties.
Summary of the invention
First purpose of the present invention is in order to overcome the shortcoming and defect that prior art exists; And provide a kind of tissue to carry out refinement to silver nickel composite material; Make size of microcrystal evenly reach grain refining technology; To improve the silver-colored nickel electric contact material of its resistance fusion welding, even more because the nickel particle distributes on silver matrix, the resistance fusion welding of fine material can be good more more for the nickel particle.
Another object of the present invention provides to a kind of crystal grain to siller tin oxide matrix material siller tin oxide electric contact material grain refining technology of carrying out refinement; Make size of microcrystal even; Sull on fragmentation and the dispersed powders granule boundary, and make oxide compound enhanced granule fibrosis, make material have more high-intensity specific modulus; Good dimensional stability and high-temperature behavior; The step refining oxide particle of going forward side by side more even the distributes on silver matrix, and obtains more tiny oxidation particle, has strengthened the resistance fusion welding and the anti-scaling loss property of material.
For realizing first purpose of the present invention, technical scheme of the present invention is to comprise following operation:
(1) preparation AgNi silk material, silk material diameter Ф 0.6mm-Ф 2.0mm; Mix by the AgNi silk material of the silk material diameter Ф 0.6mm ~ Ф 1.0mm that accounts for mass ratio 10% ~ 40% and the AgNi silk material of the silk material diameter Ф 1.0mm ~ Ф 2.0mm that accounts for mass ratio 60% ~ 90% in the AgNi silk material that this step (1) is equipped with; Thereby reach short silk silk material in being pressed into the spindle process pine dress is preferably arranged, guarantee the density of spindle.
(2) AgNi silk material is cut into the long short silk of 1cm-5cm, to the thermal treatment under protective atmosphere of short silk; The heat-treat condition of the short silk of this step (2) is that hydrogen shield atmosphere, 550 ℃ ~ 600 ℃ of thermal treatment temps, heat treatment time are 1.5 h ~ 2.0 hours, eliminates the internal stress of previous silk material, and softening short silk guarantees that material has good compactibility.
(3) will lack silk and be pressed into ingot blank, ingot blank thermal treatment under protective atmosphere with hydropress; The WP of this step (3) hydropress is 25 MPa-30MPa pressure, is pressed into the ingot blank of Ф 80mm-Ф 95mm, ingot blank thermal treatment 1.5 h ~ 2.0 hours under 550 ℃ ~ 600 ℃ steady temperature under the hydrogen shield atmosphere.
(4) carry out pressing again for 2 ~ 3 times jumping-up to obtain the raw ingot base to ingot blank, and the raw ingot base is heated to 750 ℃ ~ 850 ℃; This step (4) is for being processed into ingot blank the raw ingot base of Ф 85mm-Ф 105mm.
(5) the raw ingot base with heating carries out the AgNi silk material that secondary extrusion becomes to obtain grain refining; This step (5) is put into the raw ingot base of heating the extruding copper of diameter Ф 90mm ~ Ф 110mm size; By the AgNi silk material that becomes grain refining greater than 220 extrusion ratio hot extrude; Extrusion ratio is big more; The crimp hydrostaticpressure is big, is more conducive to the elimination of material said minuscule hole and the combination of particle, the grain refine better effects if.
(6) above step (1)-(5) repetitive operation is at least 1 time.
The invention has the advantages that: the jumping-up before the extruding is handled, and makes crystal grain shearing strain, grain refining; Reduced < 110>structural constituent in the squeeze wood effectively, broken with disperseed the borderline sull of powder particle, adopt repeatedly extruding; The crimp hydrostaticpressure is big, helps the elimination of material said minuscule hole and the combination of particle, thereby helps extrudate density and moulding raising; In the extrusion process, grain refining is more obvious, and the crystal boundary total area increases; The ability that hinders crack propagation strengthens, and makes impurity concentration reduction on the crystal boundary, avoids producing along brilliant brittle rupture.Thereby enhancing silver-based composite material each item performance.
For realizing second purpose of the present invention, technical scheme of the present invention is to comprise following operation:
(1) preparation silver tin oxide silk material, silk material diameter Ф 0.6mm-Ф 2.0mm; Mix by the silver tin oxide silk material of the silk material diameter Ф 0.6mm ~ Ф 1.0mm that accounts for mass ratio 10% ~ 40% and the silver tin oxide silk material of the silk material diameter Ф 1.0mm ~ Ф 2.0mm that accounts for mass ratio 60% ~ 90% in the silver tin oxide silk material that said step (1) is equipped with; Thereby reach short silk silk material in being pressed into the spindle process pine dress is preferably arranged, guarantee the density of spindle;
(2) the silver tin oxide silk material is cut the long short silk of 1cm-5cm, thermal treatment under air atmosphere; The heat-treat condition of the short silk of described step (2) is that hydrogen shield atmosphere, 800 ℃ ~ 900 ℃ of thermal treatment temps, heat treatment time are 1.5 h ~ 3.0 hours, eliminates the internal stress of short silk, and a softening silk material guarantees the compactibility of material;
(3) will lack silk and be pressed into ingot blank, ingot blank thermal treatment under air atmosphere with hydropress; The WP of said step (3) hydropress is 25 MPa-30MPa pressure, is pressed into the ingot blank of Ф 80mm-Ф 95mm, ingot blank thermal treatment 1.5 h ~ 3.0 hours under 800 ℃ ~ 900 ℃ the steady temperature under air atmosphere;
(4) carry out pressing again for 2 ~ 3 times jumping-up to obtain the raw ingot base to ingot blank, and the raw ingot base is heated to 750 ℃ ~ 850 ℃; Said step (4) is for being processed into ingot blank the raw ingot base of Ф 85mm-Ф 105mm, and repeatedly distortion makes the distortion of material generation horizontal direction, makes crystal grain shearing strain, grain refining;
(5) the raw ingot base with heating carries out the AgSnO that secondary extrusion obtains grain refining with at least 220 extrusion ratio
2The silk material; Said step (5) is put into the raw ingot base of heating the extruding copper of diameter Ф 90mm ~ Ф 110mm size; Extrusion ratio hot extrude by at least 220 becomes the silver tin oxide silk material of grain refining; Extrusion ratio is big more; The crimp hydrostaticpressure is big, is more conducive to the elimination of material said minuscule hole and the combination of particle, the grain refine better effects if.
(6) above step (1)-(5) repetitive operation is at least 1 time.
The invention has the advantages that: the jumping-up before the extruding is handled, and makes crystal grain shearing strain, grain refining; Reduced < 110>structural constituent in the squeeze wood effectively, broken with disperseed the borderline sull of powder particle, adopt repeatedly extruding; The crimp hydrostaticpressure is big, helps the elimination of material said minuscule hole and the combination of particle, thereby helps extrudate density and moulding raising; In the extrusion process, grain refining is more obvious, and the crystal boundary total area increases; The ability that hinders crack propagation strengthens, and makes impurity concentration reduction on the crystal boundary, avoids producing along brilliant brittle rupture.Thereby the processing characteristics of enhancing silver-based composite material postorder and the electrical property of material.
Below in conjunction with concrete accompanying drawing and embodiment the present invention is done further introduction.
Description of drawings
Fig. 1 has conventional AgNi composite products metallographic structure transverse view now;
The existing AgNi composite products metallographic structure of Fig. 2 is vertically schemed;
Product metallographic structure transverse view after 1 refinement of Fig. 3 embodiment of the invention;
The product metallographic structure is vertically schemed after 1 refinement of Fig. 4 embodiment of the invention;
Fig. 5 once pushes AgSnO
2(15) product metallographic structure transverse view;
Fig. 6 once pushes AgSnO
2(15) metallographic structure is vertically schemed;
The AgSnO of Fig. 7 embodiment of the invention 2
2(15) metallographic structure transverse view;
The AgSnO of Fig. 8 embodiment of the invention 2
2(15) metallographic structure is vertically schemed.
Embodiment
Through embodiment the present invention is carried out concrete description below; Only be used for the present invention is further specified; Can not be interpreted as the qualification to protection domain of the present invention, the technician in this field can make some nonessential improvement and adjustment to the present invention according to the content of foregoing invention.
Embodiment one: get AgNi10 silk material diameter Ф 0.6mm 3kg, the angle material silk material 3kg that the 0.6mm ~ 2mm that produces in the process is clean, 9kg in the silk material diameter 2.0mm scope; Use shears to cut and be the long short silk of 1cm-5cm roughly, under the hydrogen shield atmosphere under 550 ℃ ~ 600 ℃ steady temperature thermal treatment 1.5 h ~ 2.0 hours, on hydropress with 25 MPa-30MP pressure; Be pressed into the spindle of Ф 80mm, spindle thermal treatment 1.5 h ~ after 2.0 hours under 550 ℃ ~ 600 ℃ steady temperature under the hydrogen shield atmosphere, 2 ~ 3 jumping-ups of heat were handled before spindle pushed; Jumping-up is to 82mm for the first time, and jumping-up is to 84mm for the second time, and jumping-up is to 85mm for the third time; Under hydrogen shield atmosphere; Spindle is heated to 850 ℃, puts into the big or small extruding copper of diameter Ф 90mm to spindle, the silk material (extrusion ratio is 225) in the silk footpath of hot extrude Ф 6mm; Be drawn to Ф 1.88mm specification at last, system breaks into corresponding rivet specification.
Adopt the material of the present invention's preparation, with the conventional material performance index
A) material physical property contrast:
B) metallographic structure contrast: like Fig. 1,2,3, shown in 4, the product grains after the refinement of the present invention is even.
Embodiment two: get AgSnO
2(15) silk material diameter wire material diameter Ф 0.6mm 3kg, the angle material silk material 3kg that the 0.6mm ~ 2mm that produces in the process is clean, 9kg in the silk material diameter 2.0mm scope; Use shears to cut and be the long short silk of 1cm-5cm roughly, thermal treatment 1.5 h ~ are 3.0 hours under 800 ℃ ~ 900 ℃ steady temperature, on hydropress with 25 MPa-30MP pressure; Be pressed into the spindle of Ф 80mm, spindle thermal treatment 1.5 h ~ under 800 ℃ ~ 900 ℃ steady temperature were pushed hot upsetting processing 3 times to spindle after 3.0 hours; Jumping-up is to 82mm for the first time, and jumping-up is to 84mm for the second time, and jumping-up is to 85mm for the third time; Under hydrogen shield atmosphere; Spindle is heated to 850 ℃, puts into the big or small extruding copper of diameter Ф 90mm to spindle, the silk material (extrusion ratio is 225) in the silk footpath of hot extrude Ф 6mm; Be drawn to Ф 1.88mm specification at last, system breaks into corresponding rivet specification.
Adopt the material of the present invention's preparation, following with conventional material performance index contrast situation:
A) physicals contrast:
B) metallographic structure contrast: like Fig. 5,6,7, shown in 8, the product grains after the refinement of the present invention is even.
Claims (7)
1. silver-colored nickel electric contact material grains process for refining is characterized in that: comprise following operation:
(1) preparation AgNi silk material, silk material diameter Ф 0.6mm-Ф 2.0mm;
(2) AgNi silk material is cut into short silk different in size in the 1cm-5cm scope, to short silk under the protective atmosphere under 550 ℃ ~ 600 ℃ steady temperature thermal treatment 1.5 h ~ 2.0 hours;
(3) will lack silk and be pressed into ingot blank, ingot blank thermal treatment 1.5 h ~ 2.0 hours under 550 ℃ ~ 600 ℃ steady temperature under the protective atmosphere with hydropress;
(4) carry out pressing again for 2 ~ 3 times jumping-up to obtain the raw ingot base to ingot blank, and under protective atmosphere, the raw ingot base is heated to 750 ℃ ~ 850 ℃ at every turn;
(5) the raw ingot base with heating carries out the AgNi silk material that secondary extrusion obtains grain refining with at least 220 extrusion ratio;
(6) above step (1)-(5) repetitive operation is at least 1 time.
2. a kind of silver-colored nickel electric contact material grains process for refining according to claim 1 is characterized in that: the heat-treat condition of the short silk of described step (2) is that hydrogen shield atmosphere, 550 ℃ ~ 600 ℃ of thermal treatment temps, heat treatment time are 1.5 h ~ 2.0 hours.
3. a kind of silver-colored nickel electric contact material grains process for refining according to claim 2; It is characterized in that: the WP of said step (3) hydropress is 25 MPa-30MPa pressure; Be pressed into the ingot blank of Ф 80mm-Ф 95mm, ingot blank thermal treatment 1.5 h ~ 2.0 hours under 550 ℃ ~ 600 ℃ steady temperature under the hydrogen shield atmosphere.
4. a kind of silver-colored nickel electric contact material grains process for refining according to claim 3 is characterized in that: said step (4) is for being processed into ingot blank the raw ingot base of Ф 85mm-Ф 105mm.
5. a kind of silver-colored nickel electric contact material grains process for refining according to claim 4; It is characterized in that: said step (5) is put into the big or small extruding copper of diameter Ф 90 mm-Ф 110mm to the raw ingot base of heating, and the extrusion ratio hot extrude by at least 220 becomes the AgNi silk material of grain refining.
6. siller tin oxide electric contact material grain refining technology is characterized in that: comprise following operation:
(1) preparation silver tin oxide silk material, silk material diameter Ф 0.6mm-Ф 2.0mm;
(2) the silver tin oxide silk material is cut in the 1cm-5cm scope long short silk, thermal treatment under air atmosphere, the heat-treat condition of the short silk of this step is that air atmosphere, 800 ℃ ~ 900 ℃ of thermal treatment temps, heat treatment time are 1.5 h ~ 3.0 hours;
(3) short silk different in size is pressed into ingot blank with hydropress; The WP of this step hydropress is 25 MPa-30MPa pressure; Be pressed into the ingot blank of Ф 80mm-Ф 95mm, ingot blank thermal treatment 1.5 h ~ 3.0 hours under 800 ℃ ~ 900 ℃ the steady temperature under air atmosphere;
(4) carry out pressing again for 2 ~ 3 times jumping-up to obtain the raw ingot base to ingot blank, and the raw ingot base is heated to 750 ℃ ~ 850 ℃ at every turn;
(5) the raw ingot base with heating carries out the AgSnO that secondary extrusion obtains grain refining with at least 220 extrusion ratio
2The silk material;
(6) above step (1)-(5) repetitive operation is at least 1 time.
7. a kind of siller tin oxide electric contact material grain refining technology according to claim 6; It is characterized in that: said step (4) is for being processed into ingot blank the raw ingot base of Ф 98mm-Ф 105mm; Said step (5) is put into the big or small extruding copper of diameter Ф 90-Ф 110mm to the raw ingot base of heating, and the extrusion ratio hot extrude by at least 220 becomes the silver tin oxide silk material of grain refining.
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| CN107598176B (en) * | 2017-08-02 | 2020-06-05 | 福达合金材料股份有限公司 | Preparation process of silver metal oxide electrical contact material |
| CN109306439B (en) * | 2018-11-15 | 2021-10-26 | 佛山通宝精密合金股份有限公司 | Preparation method of fiber-reinforced silver-nickel material |
| CN109594029B (en) * | 2018-11-23 | 2020-12-25 | 福达合金材料股份有限公司 | Preparation method of AgNi electric contact material with nickel particles dispersed and distributed |
| CN111097808B (en) * | 2019-12-31 | 2022-03-01 | 天津重型装备工程研究有限公司 | Preparation method of GH4169 alloy bar |
| 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 |
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| CN101202169A (en) * | 2007-10-23 | 2008-06-18 | 福达合金材料股份有限公司 | Method of preparing novel silver tin oxide silk electrical contact material |
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| CN101202169A (en) * | 2007-10-23 | 2008-06-18 | 福达合金材料股份有限公司 | Method of preparing novel silver tin oxide silk electrical contact material |
| CN101510479A (en) * | 2009-03-18 | 2009-08-19 | 中国船舶重工集团公司第七二五研究所 | Method for preparing siller tin oxide electric contact material |
| CN101707153A (en) * | 2009-09-24 | 2010-05-12 | 温州宏丰电工合金有限公司 | Preparation method of fine-particle stannic oxide reinforced Ag-based electrical contact material |
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