CN100452259C - Silver-nickel electric contact producing technology - Google Patents
Silver-nickel electric contact producing technology Download PDFInfo
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- CN100452259C CN100452259C CNB2006100499195A CN200610049919A CN100452259C CN 100452259 C CN100452259 C CN 100452259C CN B2006100499195 A CNB2006100499195 A CN B2006100499195A CN 200610049919 A CN200610049919 A CN 200610049919A CN 100452259 C CN100452259 C CN 100452259C
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- sintering
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- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000005516 engineering process Methods 0.000 title claims description 31
- 239000000843 powder Substances 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 238000005491 wire drawing Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 15
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 12
- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 11
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 10
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 9
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000010721 machine oil Substances 0.000 claims abstract description 8
- 238000006073 displacement reaction Methods 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 50
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 38
- 229910052759 nickel Inorganic materials 0.000 claims description 26
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 230000009467 reduction Effects 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000975 co-precipitation Methods 0.000 claims description 10
- 239000010946 fine silver Substances 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 5
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 5
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010808 liquid waste Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 4
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 4
- 229920004934 Dacron® Polymers 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000003466 welding Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000003628 erosive effect Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000007873 sieving Methods 0.000 abstract description 2
- 238000010009 beating Methods 0.000 abstract 2
- 238000001125 extrusion Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000000754 repressing effect Effects 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 229910017937 Ag-Ni Inorganic materials 0.000 description 4
- 229910017984 Ag—Ni Inorganic materials 0.000 description 4
- 229910017727 AgNi Inorganic materials 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000001238 wet grinding Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000031709 bromination Effects 0.000 description 2
- 238000005893 bromination reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 210000003811 finger Anatomy 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 210000003813 thumb Anatomy 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention provides a silver-nickel electric contact fabrication process which is characterized in that silver-nickel electric contact raw material powders are prepared via a codeposition-ball grinding method; the present invention is formed from the powder body preparation engineering of silver-nickel material and silver-nickel powder body sintering, wire drawing and rivet beating engineering; the powder body preparation engineering comprises treatment processes of material preparation, displacement reaction, powder washing, stoving and sieving, effluent disposal and ball milling crushing and reducing; the powder body preparation engineering has the material preparation process that a rare-earth element of rhenium or cerium of which the mass percent is 0.4% to 1% is added; the powder body preparation engineering has the ball milling crushing process that baked silver-nickel powders go through ball milling via a ball mill; the rotating speed of the ball mill is 200 to 250 r/min, and ball milling time is 2 to 3 hours. Silver-nickel powder body sintering, wire drawing and riveting engineering comprises processes that the silver-nickel powders are pressed into powder ingots in isostatic pressing machine oil; the silver-nickel powders go through sintering, repressing, extrusion, hot wire drawing and rivet beating. The present invention has the advantages of favorable arc extinguishing effect, good resistance performance of welding and arc erosion, good use reliability, long service life and low manufacture cost, and the product price is lower 250 to 300 yuan/kilogram than that of a similar product which is not produced in China.
Description
Technical field
The present invention relates to a kind of production technology field of appliance controling element.Relate in particular to the silver-colored nickel electric contact raw material powder of a kind of employing " ball milling-coprecipitation method " preparation, under the high speed shear mulser is auxiliary, add the rare earth element of trace simultaneously to realize the silver-nickel electric contact producing technology of good arc extinguishing effect.
Background technology
Electrical contact is the critical elements in the electrical apparatus control system, and it is undertaking the task of connection and breaking current, and its performance directly influences reliability, stability and the accuracy of control system and signal transducting system work.
At present, in miscellaneous electrical contact material, silver-oxide (AgMeO) series of products have obtained to use widely owing to having excellent performance.Especially Agcdo AgCdO material is extensive use of in low-voltage electrical apparatus; Because of it has superior anti-melting welding and anti-arc erosion characteristic, become most important electrical contact material; The electrical contact industry is called " omnipotent " contact material at present.Yet, because cadmium wherein is a kind of noxious substance, not only pollute the environment, also can cause damage to health.Therefore European Union just formulated instruction in 2002, promptly " instruct " (ROHS), require to contain 6 kinds of harmful substances such as lead, mercury, cadmium, Cr VI at the Electrical and Electronic product on the July 1st, 2006 of input later on European Union market about in electronic and electrical equipment, banning use of some harmful substance.Because the AgCdO contact is very extensive in the application of electron trade, so this instruction causes the outlet of Chinese electron trade and has a strong impact on.China's Ministry of Information Industry also begins to organize relevant enterprise to carry out the substitution studies of these harmful substances in the main electronics and IT products for this reason, so that crossed over the environmental protection barrier of European Union before the 1 day July in 2006, formulated " electronics and IT products prevention and cure of pollution management method " simultaneously, requirement is from July 1st, 2006, lists in the electronics and IT products that electronics and IT products pollute the keypoint control catalogue to contain lead, mercury, cadmium, Cr VI, polymerization bromination biphenyl (PBB), polymerization bromination biphenyl ether (PBDE) and other harmful substances.In fact Europe just began after having carried out a large amount of tests, to find in relay field silver-nickel (Ag-Ni) it is only material in the alternative work of studying the AgCdO contact material from the beginning of the eighties.Yet because on technology and the cost, silver-nickel (Ag-Ni) does not obtain large-scale application always.Especially the domestic market is still AgCdO and is in leading position.
In addition, along with the development of low-voltage electrical apparatus to miniaturization, high reliability, long-life direction, shortcoming such as the AgCdO contact material also exposes resistance fusion welding can be poor, and arc erosion is serious.But because the Ag-Ni powder when being processed into a thread material the poor and electrical property of processing characteristics be difficult to break through, carry out quite slow so present domestic Ag-Ni substitutes AgCdO work.
Summary of the invention
Purpose of the present invention is exactly at problems of the prior art, provides a kind of employing " ball milling-coprecipitation method " thereby the silver-nickel electric contact producing technology of the silver-colored nickel electric contact raw material powder of preparation, while rare earth element raising product comprehensive electrochemical properties of interpolation trace under the high speed shear mulser is auxiliary.
The objective of the invention is to have by providing a kind of that following silver-nickel electric contact producing technology realizes, it is made up of powder preparing engineering and described silver-nickel powder body sintering, wire drawing, the riveter nail engineering of described silver-nickel material.The powder preparing engineering of described silver-nickel material comprise get the raw materials ready, displacement reaction, powder are cleaned with oven dry and are sieved, liquid waste processing, ball mill grinding and reduction treatment process; Be added with rare earth element in the described procedure for preparation; Described interpolation rare earth element is rhenium or Ce elements; The mass percent of described interpolation rare earth element is 0.4～1% rhenium or Ce elements.
Described silver-nickel powder body sintering, wire drawing, riveter nail engineering comprise isostatic pressing machine powder for molding ingot, sintering, multiple pressure and extruding, hot wire drawing, riveter nail operation.
Described procedure for preparation is that the fine silver block casting by purity 〉=99.95% becomes particle or is cut into chip, and particle is less than 5mm; The pure nickel of purity 〉=99.5% is rolled into 1mm thickness sheet, be cut into 5mm～10mm does not wait piece; Its quantity is fine silver 8.92kg, pure nickel 1kg, rhenium powder 0.04kg, cerium powder 0.04kg; Silver bits and nickel block are clean with the washed with de-ionized water that is heated to boiling point respectively; Industry one-level nitric acid 16L turns off electric furnace after adding deionized water 16L and salpeter solution being heated to about 80 ℃; Earlier nickel block is dissolved; The fine silver bits are joined in the acid solution then in batches, make its whole dissolvings; After the dissolving solution is stirred half an hour in mixer, make it even; In addition 10.5Kg is analyzed pure sodium carbonate, pour in the stainless steel cask of the deionized water that fills about 20L, be heated to 70 ~ 80 ℃, sodium carbonate is dissolved fully; Silver nitrate, nickel nitrate mixed solution are filtered secondary with woven dacron, add the 30L deionized water then mixed liquor is diluted; Analyzing pure sodium carbonate solution dilutes with 15L left and right sides deionized water.
Described displacement reaction operation is that described silver nitrate, nickel nitrate mixed solution and described sodium carbonate liquor are heated to 40～60 ℃ respectively; Described silver nitrate, described nickel nitrate mixed solution are stirred in the intermediate frequency mixer, and described mixer rotating speed is 1000～1200 rev/mins; Add described rhenium, cerium powder more equably; Slowly add sodium carbonate liquor then, make its reaction back co-precipitation generate silver carbonate and nickelous carbonate; Treat that pH value to 7～8 of solution in the agitator o'clock promptly end; Continue again after described reaction finishes to stir 0.5 hour, carry out secondary filter after making it evenly by described intermediate frequency mixer.
Described sodium carbonate liquor adds its discharge of control at 0.5～0.8 liter/minute, and the shower nozzle area reaches more than 0.07 square metre.
Described ball mill grinding operation is that silver-nickel by powder that described oven dry is good carries out ball milling with ball mill, and described drum's speed of rotation is controlled at 200～250r/min, and the described ball milling time is 2～3 hours.
Described reduction treatment process is that described silver-nickel powder that ball milling is good reduces processing in hydrogen furnace; Reduction temperature is 520 ℃; Recovery time is 12 hours; Logical hydrogen pressure is 0.08～0.1 MPa in the described hydrogen furnace.
Described isostatic pressing machine powder for molding ingot operation is the good silver-nickel by powder that sieves reduction to be contained in to be placed in the plastic sheath of sealing be pressed into the powder ingot in 200 tons of isostatic pressing machine oil, and described oil pressure is controlled to be 12～14 MPas.
Described sintering circuit is that sintering temperature is controlled at 600～620 ℃, is incubated 2～3 hours the silver-colored nickel ingot sintering in the nitrogen protection stove that presses; With 630 tons of extruders silver-nickel ingot of calcining is carried out multiple pressure then, pressure is controlled at 12～13 MPas.
Compared with prior art, the invention has the advantages that: 1. good, the resistance fusion welding of the arc extinguishing effect of electrical contact, anti-arc erosion function admirable, thus improved the comprehensive electrochemical properties of product greatly; 2. nontoxic, as not pollute the environment environmentally friendly machine, and dependability is good, working life is longer; 3. low cost of manufacture, product price reduces by 250～300 yuan/kilogram than the like product of external import.
Description of drawings
Fig. 1 is a process chart of the present invention;
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Fig. 1 illustrates an execution mode of silver-nickel electric contact producing technology of the present invention.
Silver-nickel contact material is a kind of ep-type material that developed recently gets up, and its resistance fusion welding, anti-arc erosion performance are all better, can satisfy the high reliability in the electric operation, long-life requirement.Along with the enhancing of people's environmental consciousness, replacing the AgCdO electrical contact material at field silver-nickel electric contact materials such as small-power thermostat, relays will be trend of the times.
The technology of silver-nickel electric contact manufacture of materials comparative maturity mainly contains three kinds: mix powder, ball milling, coprecipitation method.Silver-nickel contact the raw material that wherein mix powder, ball-milling technology production are inhomogeneous, have a strong impact on the processing characteristics and the electrical property of product; Adopting the silver-nickel contact raw material of coprecipitation method explained hereafter mainly is that powder is too thin, and the following process difficulty is difficult to cleaning, wire drawing.
In the silver-nickel electric contact producing technology development process of the present invention, mainly studied chemical deposition (the patent DE10017282 of Degussa (DEGUSSA) company, EP1142661,2002) and relevant United States Patent (USP) (United StatesPatent 5,846,288,1998), and to the world, the achievement of domestic enterprise and research unit is summed up and is analyzed, on this basis, in conjunction with the advantage of oneself, the associating relay, the relevant enterprise of switch industry, through nearly 2 years exploitation, the product that silver-the specific powder metallurgy technology of nickel composite powder employing makes with " coprecipitated-ball-milling method " preparation has better machining property, can carry out wire drawing (hot-drawn---new technology), riveter nail (silver-nickel/copper composite rivet surface flawless), and electrical performance indexes can satisfy customer requirements, promptly 20～80 amperes of direct currents, cut-off melting welding does not take place more than 1500 times.
Silver-nickel electric contact producing technology of the present invention is to adopt " coprecipitated-ball-milling method " preparation silver-nickel electric contact raw material powder production technology; Distribution and the inhomogeneity method of rare earth element (rhenium, cerium) in silver-nickel material of control trace to reach the arc extinguishing effect of strengthening silver-colored nickel electric contact product, makes final electrical contact have better electrical property.
And the electrical contact raw material powder that method for preparing is come out adopts the good silver-colored nickel wire material of specific powder metallurgy process manufacturing property and the contact of different shape, has good electrical properties.
The work flow of silver-nickel electric contact producing technology of the present invention by 1. powder preparing engineering with 2. sintering, wire drawing, two parts of riveter nail engineering are formed; Wherein:
1. the powder preparing engineering comprises: the 1-2-displacement reaction 3-powder of getting the raw materials ready cleans the 4-oven dry 4A-liquid waste processing 5-ball mill grinding 6-reduction of sieving and handles;
2. sintering, wire drawing, riveter nail engineering comprise: be pressed into powder ingot 8-sintering 9-in the 7-isostatic pressing machine oil and press 10-extruding 11-hot wire drawing riveter nail again; The work flow of above-mentioned technology as shown in Figure 1.
The standard and the specific requirement of above-mentioned work flow are:
1-fine silver piece purity 〉=99.95% of getting the raw materials ready is cast particle or is cut into chip, and particle is less than 5mm.Pure nickel purity 〉=99.5% is rolled into 1mm thickness sheet, is cut into 5mm～10mm and does not wait piece.Quantity: fine silver 8.92kg, pure nickel 1kg, rhenium powder 0.04kg, cerium powder 0.04kg; Silver bits and nickel block use deionized water (being heated to boiling point) to clean up respectively; Industry one-level nitric acid 16L adds deionized water 16L.Salpeter solution is heated to about 80 ℃, turns off electric furnace.Earlier nickel block is dissolved; The fine silver bits are joined in the acid solution then in batches, make its whole dissolvings; After the dissolving solution is stirred half an hour in mixer, make it even; The dissolving overall process all must be opened the extract system exhaust; In addition 10.5Kg is analyzed pure sodium carbonate, pour in the stainless steel cask that fills 20L left and right sides deionized water, be heated to 70～80 ℃, sodium carbonate is dissolved fully.Silver nitrate, nickel nitrate mixed solution are filtered secondary with woven dacron, add the 30L deionized water then mixed liquor is diluted; Analyzing pure sodium carbonate solution dilutes with 15L left and right sides deionized water.
The 2-displacement reaction is heated to 40～60 ℃ respectively with silver nitrate, nickel nitrate mixed solution and sodium carbonate liquor; Silver nitrate, nickel nitrate mixed solution are stirred in the intermediate frequency mixer, and the mixer rotating speed is 1000～1200 rev/mins; Add rhenium, cerium powder more equably; Slowly add sodium carbonate liquor then, make its reaction back co-precipitation generate silver carbonate and nickelous carbonate; (sodium carbonate should slowly add equably by self-control spray affair device, and controls its discharge at 0.5～0.8 liter/minute), treat that pH value to 7～8 of solution in the agitator o'clock are promptly ended; Continue again after reaction finishes to stir 0.5 hour, carry out two layers of filtration after making it evenly by the intermediate frequency mixer.
The 3-powder cleans and put into two layers of filtration cloth bag in draining cylinder, the co-precipitation wet-milling that has filtered is poured in the cloth bag, pour the washed with de-ionized water about 70～80 ℃ then into, stir by hand and stir (also available Stainless steel basin stirs and stirs, and pours into after the cleaning again and drains in the cylinder); After treating that the moisture drop goes a bit, promptly open and drain pump, moisture content is drained, so repeated multiple times is cleaned, and makes the cleaning fluid pH value reach 6.5～7.5, and conductivity reaches≤190 μ S/cm.
4-oven dry is sieved silver carbonate and nickelous carbonate wet-milling is packed in the stainless steel disc, sabot thickness≤40mm, in Electric heat oven with 140～160 ℃ of oven dry, insulation 30-40h; Powder after the oven dry is broken off with the fingers and thumb into about 1cm left and right sides fritter with hand, reentered in the porcelain basin, put into air furnace and carry out roasting, temperature is 480～580 ℃, insulation 5～6h.After treating that nickelous carbonate is completely oxidized to black, sieve with 80 order dressing sieves; Black powder carried out pouring into after deionized water and stirring is cleaned in basin be placed with draining in the cylinder of filter cloth and drain, repeated multiple times like this will be deceived powder and be cleaned to conductivity and reach≤20 μ S/cm, and pH value is 6.5～7.5; Black wet-milling after will cleaning is again packed in the stainless steel disc, thickness≤30mm, and in Electric heat oven, with 150 ℃ of oven dry, insulation 30-40h.
The 4A-liquid waste processing with chemical powdering reaction and waste liquids such as the copper nitrate after cleaning, sulfuric acid pour in the settling box, add NaOH sheet alkali, make it reaction precipitation, the addition of NaOH reaches till 9～10 with the pH value of reaction solution; The waste residue of reaction precipitation is drained with the suction filtration machine, and handle by environmental regulations waste residue pack back.
The 5-ball mill grinding will be dried good silver-nickel by powder and be added the high-performance planetary ball mill and carry out ball milling, and rotating speed is controlled at 200-250r/min, and the ball milling time was at 2-3 hour.
6-reduction is handled silver-nickel powder that ball milling is good and reduce processing in hydrogen furnace; The reduction treatment process parameter of powder is stipulated requirement by table 1:
Table 1: silver-nickel powder reduces the treatment process parameter in hydrogen furnace
| Material | AgNi (10) powder (coprecipitation method) |
| Reduction temperature/time | 520℃/12h |
| Logical hydrogen pressure | 0.08~0.1MPa |
| Hydrogen flowing quantity | Give vent to anger intensive bubble (number of bubbles＞100/min) of emerging are arranged in the water bottle |
| Sabot thickness | ≤20mm |
Should be silver gray after silver-nickel powder reduction, otherwise need reduction again; 80 mesh sieves are crossed in AgNi (10) powder reduction back; Reduction materials disk material should adopt stainless steel, carries out pickling earlier before the charging in case of necessity; Flue work effective dimensions is Φ 400 * 450.AgNi (10) powder: Ag 〉=89.0%, Ni ± 1%, total impurities≤0.3%, mistake 80 mesh sieves.
Being pressed into the silver-nickel by powder that it is good that the powder ingot will sieve reduction in the 7-isostatic pressing machine oil is placed in being contained in the plastic sheath of sealing and is pressed into powder ingot (oil pressure is controlled at 12～14 MPas) in 200 tons of isostatic pressing machine oil.
The 8-sintering is the good silver-colored nickel ingot sintering in the nitrogen protection stove of briquetting, and sintering temperature is controlled at 800～820 ℃, is incubated 2～3 hours; With 630 tons of extruders silver-nickel ingot of calcining is carried out multiple pressure then, pressure is controlled at 12 ~ 13 MPas.
Silver-nickel ingot that 10-extruding, 11-hot wire drawing riveter nail will press again is placed in the nitrogen protection stove and is incubated 2～3 hours (temperature is controlled at 900～920 ℃) is squeezed into Φ 7.8mm silk material with 630 tons of extruders afterwards, then carrying out hot wire drawing according to corresponding electrical contact rivet specification, riveter is followed closely.
The major control point of silver-nickel electric contact producing technology of the present invention is:
(1) adds 0.4～1% rare earth element rhenium or Ce elements, to improve the useful life of electrical contact product.
(2) when the medium frequency shear-mixed is added sodium carbonate liquor, use self-control characteristic spray affair device to add, control its discharge at 0.5～0.8 liter/minute, the shower nozzle area reaches more than 0.07 square metre, makes reaction even, consistent.
(3) use the high-performance planetary ball mill during ball mill grinding, rotating speed is controlled at 200～250r/min, so that increase the adhesion between silver and the nickel and increase the particle of powder, is convenient to the subsequent thermal wire drawing and handles.
Silver-nickel electric contact producing technology of the present invention is to use the silver-colored nickel electric contact raw material powder production technology of " coprecipitated-ball-milling method " preparation.By the silver-colored nickel electric contact raw material powder of " ball milling-coprecipitation method " preparation, at auxiliary rare earth element (rhenium, cerium) and other additives that add trace down of high speed shear mulser, improve electrical contact product arc extinguishing effect simultaneously, thereby improve the electrical property of product.In addition, utilize the high frequency ball mill that the powder of method for preparing is carried out ball-milling treatment,, be convenient to the subsequent thermal wire drawing and handle with the particle of adhesion between further increase silver and the nickel and increase powder.Silver-nickel electric contact of the present invention can substitute the electrical contact product of the similar top grade of import, and selling price is than the low 250-300 of external imported product unit/kilogram simultaneously.
Claims (10)
1. silver-nickel electric contact producing technology, it is made up of powder preparing engineering and silver-nickel powder body sintering, wire drawing, the riveter nail engineering of silver-nickel material; It is characterized in that:
A. the powder preparing engineering of described silver-nickel material comprise get the raw materials ready, displacement reaction, powder are cleaned with oven dry and are sieved, liquid waste processing, ball mill grinding and reduction treatment process;
B. be added with rare earth element in the described procedure for preparation;
C. described silver-nickel powder body sintering, wire drawing, riveter nail engineering comprise that being pressed into powder ingot, sintering, multiple pressure and extruding, hot wire drawing riveter in the isostatic pressing machine oil follows closely sintering, wire drawing, riveter nail operation.
2. a kind of silver-nickel electric contact producing technology according to claim 1 is characterized in that: described interpolation rare earth element is rhenium or Ce elements.
3. a kind of silver-nickel electric contact producing technology according to claim 2 is characterized in that: the content of described interpolation rare earth element is that the interpolation mass percent is 0.4～1% rhenium or Ce elements.
4. a kind of silver-nickel electric contact producing technology according to claim 1 is characterized in that: described procedure for preparation is that the fine silver block casting by purity 〉=99.95% becomes particle or is cut into chip, and particle is less than 5mm; The pure nickel of purity 〉=99.5% is rolled into 1mm thickness sheet, be cut into 5mm～10mm does not wait piece; Its quantity is described fine silver piece 8.92kg, described pure nickel sheet 1kg, rhenium powder 0.04kg, cerium powder 0.04kg; Described fine silver piece and described pure nickel sheet are clean with the washed with de-ionized water that is heated to boiling point respectively; Industry one-level nitric acid 16L turns off electric furnace after adding deionized water 16L and salpeter solution being heated to 80 ℃; Earlier the pure nickel sheet is dissolved; Described fine silver piece is joined in the acid solution then in batches, make its whole dissolvings; After the dissolving solution is stirred half an hour in mixer, make it even; In addition 10.5Kg is analyzed pure sodium carbonate, pour in the stainless steel cask of the deionized water that fills 20L, be heated to 70～80 ℃, sodium carbonate is dissolved fully; Silver nitrate, nickel nitrate mixed solution are filtered secondary with woven dacron, add the 30L deionized water then mixed liquor is diluted; Analyzing pure sodium carbonate solution dilutes with the 15L deionized water.
5. a kind of silver-nickel electric contact producing technology according to claim 4 is characterized in that: described displacement reaction operation is that described silver nitrate, nickel nitrate mixed solution and described sodium carbonate liquor are heated to 40～60 ℃ respectively; Described silver nitrate, described nickel nitrate mixed solution are stirred in the intermediate frequency mixer, and described mixer rotating speed is 1000～1200 rev/mins; Add described rhenium, cerium powder more equably; Slowly add sodium carbonate liquor then, make its reaction back co-precipitation generate silver carbonate and nickelous carbonate; Treat that pH value to 7～8 of solution in the agitator o'clock promptly end; Continue again after described reaction finishes to stir 0.5 hour, carry out two layers of filtration after making it evenly by described intermediate frequency mixer.
6. a kind of silver-nickel electric contact producing technology according to claim 5 is characterized in that: described sodium carbonate liquor adds its discharge of control at 0.5～0.8 liter/minute, and the shower nozzle area reaches more than 0.07 square metre.
7. a kind of silver-nickel electric contact producing technology according to claim 1 is characterized in that: described ball mill grinding operation is that silver-nickel by powder that described oven dry is good carries out ball milling with ball mill, and described drum's speed of rotation is controlled at
200～250r/min, the described ball milling time is 2～3 hours.
8. a kind of silver-nickel electric contact producing technology according to claim 1 is characterized in that: described reduction treatment process is that described silver-nickel powder that ball milling is good reduces processing in hydrogen furnace; Reduction temperature is 520 ℃; Recovery time is 12 hours; Logical hydrogen pressure is 0.08～0.1 MPa in the described hydrogen furnace.
9. a kind of silver-nickel electric contact producing technology according to claim 1, it is characterized in that: be pressed into powder ingot operation in the described isostatic pressing machine oil and be the good silver-nickel by powder that sieves reduction is contained in to be placed in the plastic sheath of sealing and be pressed into the powder ingot in 200 tons of isostatic pressing machine oil, described oil pressure is controlled to be the 12-14 MPa.
10. a kind of silver-nickel electric contact producing technology according to claim 1 is characterized in that: described sintering circuit is that sintering temperature is controlled at 600～620 ℃, is incubated 2～3 hours the silver-colored nickel ingot sintering in the nitrogen protection stove that presses; With 630 tons of extruders silver-nickel ingot of calcining is carried out multiple pressure then, pressure is controlled at 12～13 MPas.
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| CNB2006100499195A CN100452259C (en) | 2006-03-17 | 2006-03-17 | Silver-nickel electric contact producing technology |
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| CN102737863B (en) * | 2012-07-03 | 2015-01-28 | 扬州乐银合金科技有限公司 | Silver nickel graphite composite contact terminal material and processing method thereof |
| CN104451185B (en) * | 2014-12-19 | 2016-05-04 | 桂林电器科学研究院有限公司 | From silver-colored nickel leftover pieces, silver-colored method is reclaimed in melting |
| CN104439249A (en) * | 2014-12-30 | 2015-03-25 | 桂林电器科学研究院有限公司 | Method for processing sheet silver nickel electric contact material |
| CN107633960B (en) * | 2017-09-11 | 2019-12-03 | 大连大学 | A kind of sheet iron reticulates the Ag-based electrical contact material and preparation method thereof of distribution reinforcing |
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| CN1848323A (en) | 2006-10-18 |
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