CN109881191A - A kind of preparation method for contact material silver-bearing copper diffusion coating - Google Patents
A kind of preparation method for contact material silver-bearing copper diffusion coating Download PDFInfo
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- CN109881191A CN109881191A CN201910250050.8A CN201910250050A CN109881191A CN 109881191 A CN109881191 A CN 109881191A CN 201910250050 A CN201910250050 A CN 201910250050A CN 109881191 A CN109881191 A CN 109881191A
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- silver
- copper
- contact material
- heat treatment
- coating
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- 239000010949 copper Substances 0.000 title claims abstract description 148
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 112
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 98
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000004332 silver Substances 0.000 title claims abstract description 94
- 239000000463 material Substances 0.000 title claims abstract description 79
- 238000000576 coating method Methods 0.000 title claims abstract description 54
- 239000011248 coating agent Substances 0.000 title claims abstract description 53
- 238000009792 diffusion process Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 46
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 15
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 6
- 229940045105 silver iodide Drugs 0.000 claims description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 5
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 3
- 235000011180 diphosphates Nutrition 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 abstract description 21
- 230000007797 corrosion Effects 0.000 abstract description 20
- 239000004615 ingredient Substances 0.000 abstract description 19
- 238000009826 distribution Methods 0.000 abstract description 13
- 229910045601 alloy Inorganic materials 0.000 abstract description 9
- 239000000956 alloy Substances 0.000 abstract description 9
- 238000013461 design Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 5
- 238000000151 deposition Methods 0.000 abstract description 3
- 238000004070 electrodeposition Methods 0.000 abstract description 3
- 238000005470 impregnation Methods 0.000 abstract description 3
- 230000008595 infiltration Effects 0.000 abstract description 3
- 238000001764 infiltration Methods 0.000 abstract description 3
- 230000008520 organization Effects 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 55
- 239000010944 silver (metal) Substances 0.000 description 32
- 239000000243 solution Substances 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- 230000008859 change Effects 0.000 description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 6
- 230000002829 reductive effect Effects 0.000 description 6
- 238000005728 strengthening Methods 0.000 description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000009713 electroplating Methods 0.000 description 5
- 239000008103 glucose Substances 0.000 description 5
- FEWJPZIEWOKRBE-LWMBPPNESA-N levotartaric acid Chemical compound OC(=O)[C@@H](O)[C@H](O)C(O)=O FEWJPZIEWOKRBE-LWMBPPNESA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 235000001968 nicotinic acid Nutrition 0.000 description 2
- 229960003512 nicotinic acid Drugs 0.000 description 2
- 239000011664 nicotinic acid Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000001235 sensitizing effect Effects 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000010930 yellow gold Substances 0.000 description 2
- 229910001097 yellow gold Inorganic materials 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910017770 Cu—Ag Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Electroplating Methods And Accessories (AREA)
- Contacts (AREA)
Abstract
The invention discloses a kind of preparation methods for contact material silver-bearing copper diffusion coating；Including being spaced copper facing, silver-plated in substrate, copper silver composite deposite is obtained；Wherein copper layer thickness is 1-50 μm, and silver thickness is 0.1-20 μm；The copper silver composite deposite is placed in vacuum drying oven or special atmosphere oven, 450-750 DEG C is warming up to 5-20 DEG C/min of heating rate and carries out heat treatment 6-24 hours to get the silver-bearing copper diffusion layer.The invention proposes multilayer electro-deposition assistant alloys to expand the design method that infiltration prepares silver-bearing copper contact material, expand cementation process by the arrangement and heat treatment of design depositing silver layers and layers of copper, acquisition is uniformly distributed with silver, copper ingredient respectively or the silver-bearing copper of silver-colored, copper ingredient distribution gradient typical organization expands impregnation coating, wherein component gradient distribution coating has the characteristics that corrosion potential gradient distribution, can reduce the galvanic couple accelerated corrosion risk due to caused by surface covering breakage.
Description
Technical field
The present invention relates to a kind of preparation methods for contact material silver-bearing copper diffusion coating.
Background technique
Contact material be prepare electric power, switching control and load current electric appliance in appliance circuit (as switch, relay,
Starter and instrument and meter etc.) critical material.Performance, quality and the service life of contact material are directly related to equipment operation
Reliability.
Due to work condition state and the difference of Service Environment, such as contact pressure, operating voltage, size of current, the disjunction service life, wet
More stringent requirements are proposed to existing contact material for heat, salinity etc..For synthesis, contact material need to have higher lead
The performances such as electricity and thermal conductivity, high chemical stability, low and stable contact resistance, high resistance fusion welding and high anti electric arc corrosion.It is expensive
Metal base electrical contact material has always been considered as being ideal contact material, is especially connecing on and off due to having both above-mentioned performance
Excellent comprehensive performance is shown in opening apparatus, therefore is all selected as slider material in many electrical contact application fields,
It is most widely used contact material at this stage.
The noble metal contact material of sizable application is broadly divided into four classes: Gold Base Electric Contact Materials, silver-based electric contact material,
Platinum base contact material and palladium base contact material.Wherein since metallic silver relative price is cheap, possess good resistance fusion welding,
Anti electric arc corrosion and electric conductivity have obtained preferential in noble metal contact material and have quickly developed, used extensively
In the high and low voltage electrical equipment of various commutator for light-heavy load, household electrical appliance, car electrics, aerospace electric appliance, especially breaker and contact
These electric appliance almost all for having a large capacity and a wide range of device are using silver-based electric contact material, such as AgCdO contact material, because resistance to electric arc,
Anti- melting welding, stable lower contact resistance are referred to as omnipotent slider material, but Cd is heavy metal, harmful to human body and environment,
For the demand of environmental protection, contact material must develop towards the environmentally friendly direction of replacement Cd.Other silver-based materials are such as
AgSnO2, AgZnO etc., due to the addition of second phase particles, the abrasion resistance and hardness of material can be significantly improved, but due to second
Phenomena such as phase particle causes cyrystal boundary segregation, and crystal grain is reunited is caused so that the corrosion resistance of material sharply declines to the application of material
Very big obstruction.
Additionally due to the reserves of silver are limited, and it is expensive, the novel electrical contact material for replacing silver is found, the dosage of silver is reduced
Seeming especially has application value.So people develop copper-based material again, the mechanical property and electric conductivity of copper are stored up close to silver
Amount is more relatively rich than silver, is the ideal material of substitution silver.But the resistance to corrosion of copper is poor, is easy to be oxidized mistake under working condition
Effect so improving the inoxidizability of copper, while not reducing its electric conductivity, is the emphasis of contact material research.Traditional is copper-based
The mentality of designing of contact material is still similar with silver-based electric contact material, is added using powder metallurgic method or alloy inner oxidation method
Add second phase particles.Powder metallurgic method improves the resistance fusion welding and wearability of material by the enhancing of addition second phase particles,
But ultra-fine second phase particles are easy to reunite, and ceramic phase is poor with basal body binding force, limit copper-based electrical contact material to a certain extent
The application of material.Alloy inner oxidation rule be easy to cause boundary to be segregated, so that material composition is uneven, brittleness increases.
Metallic copper possesses good electric conductivity, but the tensile strength of fine copper is low, wears no resistance, and is oxidized easily in air
Nonconducting copper oxide is formed, and makes contact failure.By the solution strengthening of alloy, the strong hardness of copper and wear-resisting can be enhanced
Property, but new atom causes distortion of lattice to increase, and increases the scattering of electronics, so that conductivity declines.Therefore solution strengthening pair
In the electric conductivity and intensity of copper be contradictory.But in various alloying elements, silver atoms are minimum to the Conductivity of copper but high
The Kufil of intensity still means that smaller crystal grain, more crystal boundaries and crystal defect, can equally destroy the symmetrical of lattice
Property, reduce its conductivity.For contact material, strong hardness, wearability and the corrosion resistance of copper-based material are improved, is reduced expensive
The dosage of metallic silver still has very big realistic meaning.In existing Kufil, silver-colored additive amount 1% hereinafter, silver
Doping can significantly improve the tensile strength of copper wire, and conductivity may remain in 90%IACS or more, be suitable for conductor material.
With increasing for silver content, the tensile strength and hardness of Kufil are significantly improved, but conductivity decline is serious, is not suitable for leading
Electric material.
The failure of contact material is often derived from surface, such as the interface of typical mobile phone, computer 3C Product, due to table
The abrasion of the silver-colored contact material of layer or corrosion failure phenomena such as easily causing electric leakage, generate heat, cause electric appliance damage even to occur quick-fried
Fried and fire.Contact corrosion damp and hot, under salt time-sharing environment, abrasion etc. have become the failure of contact material and aging effects
The emphasis of such contact material research.
Summary of the invention
For contact corrosion of the above-mentioned existing silver-based electric contact material under the environment such as damp and hot, salinity, Abrasion properties differences
Technological deficiency, the object of the present invention is to provide a kind of preparation methods for contact material silver-bearing copper diffusion coating.It is different from existing
There are silver-based or copper-based electric contact material preparation method, prepares silver-bearing copper electricity the invention proposes multilayer electro-deposition assistant alloy expansion infiltration and connect
The design method for touching material spreads the erosion corrosion performance strengthened and improve existing electrical contact plug connector by surface alloy, simultaneously
Have both excellent conductive, thermally conductive and wear-resisting property.Silver-bearing copper designed by the present invention expands impregnation coating, can be by designing depositing silver layers
And layers of copper arrangement and heat treatment expand cementation process, respectively obtain have silver, copper ingredient be uniformly distributed or silver, copper at
Divide the typical organization of distribution gradient, wherein component gradient distribution coating has the characteristics that corrosion potential gradient distribution, can
To reduce the galvanic couple accelerated corrosion risk due to caused by surface covering breakage.Processing relative to existing whole contact material
For preparation method, the dosage of metallic silver is can be significantly reduced in the method for alloying coating, reduces material cost.
The purpose of the present invention is what is be achieved through the following technical solutions:
The present invention relates to a kind of preparation methods for contact material silver-bearing copper diffusion layer, and the method includes walking as follows
It is rapid:
S1, it be spaced copper facing in substrate, is silver-plated, or being spaced silver-plated, copper facing, obtaining copper silver composite deposite；The copper silver is multiple
Closing copper layer thickness in coating is 1-50 μm, and silver thickness is 0.1-20 μm；
S2, the copper silver composite deposite is placed in vacuum drying oven or special atmosphere oven, with 5-20 DEG C/min of heating rate
It is warming up to 450-800 DEG C and carries out heat treatment 6-24 hours to get the silver-bearing copper diffusion layer.
Diffusion layer copper silver concentration gradient distribution in the present invention, potential gradient reduce, and outer layer richness silver layer can provide good
Anti-corrosion capability is spread through Overheating Treatment, can also improve coating hardness, wearability.In this way, can not only reduce electricity
Silver-colored dosage in contact material can also improve the wearability and anticorrosive property of copper product.
Preferably, the copper silver composite deposite is the spaced bilayer or multilayer coating of Cu/Ag, or is the interval Ag/Cu
The bilayer or multilayer coating of setting.
Preferably, the copper silver composite deposite is the double-deck coating of Cu/Ag, and wherein copper layer thickness is 5-50 μm, and silver layer is thick
Degree is 2-20 μm；The heat treatment temperature is 550-800 DEG C, and heat treatment time is 12-24 hours.
Preferably, the copper layer thickness is 10-35 μm, and silver thickness is 5-15 μm；The heat treatment temperature is 600-750
℃。
Preferably, the copper silver composite deposite is three layers of coating of Ag/Cu/Ag, and wherein copper layer thickness is 2-10 μm, silver layer
With a thickness of 0.1-2 μm, heat treatment temperature is 500-650 DEG C, and heat treatment time is 6-24 hours.
Preferably, the copper silver composite deposite is Ag/Cu/Ag/Cu/Ag/Cu/Ag/Cu/Ag/Cu/Ag coating, wherein copper
For layer with a thickness of 1-5 μm, silver thickness is 0.1-1 μm, and heat treatment temperature is 550-650 DEG C, and heat treatment time is 6-24 hours.
Preferably, the copper facing is using sodium hypophosphite chemical plating, the plating of aldehydes organic-matter chemical, acidiccopper plating or burnt phosphorus
Hydrochlorate copper facing.
Preferably, described silver-plated silver-plated using ethylenediamine chemical silvering or silver iodide plating.
Preferably, the substrate is Copper substrate.It is thermally treated by plating copper silvering on Copper substrate, it can be obvious
The corrosion resistance of material, wearability and hardness are improved, and significantly reduces material conductivity.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, the coating crystal grain that present invention plating obtains is tiny, and internal stress is larger, by heat treatment, can eliminate internal stress,
Meanwhile silver-bearing copper counterdiffusion at high temperature, the Kufil of one layer of copper silver concentration change of gradient is formed on the surface of the material.
2, by solution strengthening, the intensity of material is increased；For common metal, the solution strengthening of alloy makes material
Material internal flaw increases, electric conductivity decline, but adding silver in copper is to itself Conductivity minimum, through the invention
On the other hand the Cu-Ag film of method preparation also possesses good lead on the one hand since solution strengthening possesses good strong hardness
Electrically.
3, by exposure in air being the face Fu Yin, silver has good oxidation resistance, and the anti-corruption of material can be improved
Corrosion, while surface layer copper silver concentration gradient distribution also reduce so that potential difference gradient declines since surface fracture causes galvanic couple
The risk of corrosion is the ideal material for contact material.
4, the present invention by design silver layer and arrangement, thickness and the heat treatment process parameter of layers of copper etc., obtain have silver,
Copper ingredient is uniformly distributed or silver, copper ingredient distribution gradient electrical contact coating material；Electricity designed by the present invention
Contacting coating material has silver-bearing copper ingredient controllable, the programmable feature of corrosive nature, is realizing the same of electrical surface contact performance
When, it can largely save precious metal material.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the structural schematic diagram of the coating obtained with copper silver concentration change of gradient of embodiment 1；
Fig. 2 is the structural schematic diagram of the coating obtained with copper silver concentration change of gradient of embodiment 2；
Fig. 3 is the structural schematic diagram for the Kufil that composite deposite made from embodiment 3 and silver layer are spread completely.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention
Protection scope.
The present invention provides the technical methods that a kind of surface covering assists heat-treatment alloying diffusion:
The preparation of composite coating can be carried out by way of plating or chemical plating, and wherein copper coating can be by secondary
The mode or traditional acidiccopper plating or pyrophosphate copper plating of sodium phosphite chemical plating or the plating of aldehydes organic-matter chemical
Etc. modes obtained, it is silver-plated silver-plated system to be electroplated using ethylenediamine chemical silvering system or silver iodide.Pass through control
Plating time and plating current density control thickness of coating.Then it carries out heat treatment to be diffused, obtains copper silver lamellar composite
Coating.Pass through the arrangement of control copper silver layer and the thickness of coating and time, the temperature of regulation heat treatment, available difference
The coating of component distributing.By the number of plies of the thickness of coating and coating of control layers of copper and silver layer, can regulation appropriate it is hot at
Temperature and heat treatment time are managed, the coating number of plies is more, and coating is thinner, and the temperature of heat treatment is lower, and heat treatment time is shorter.Such as
Coating can be designed as the mode of Cu/Ag or Ag/Cu/Ag/Cu ... alternating deposit.For the double-deck coating of Cu/Ag, thickness is set
It is calculated as layers of copper (5-50 μm, preferably 10-30 μm), silver layer (2-20 μm, preferably 5-10 μm), heat treatment temperature is (550-750
DEG C, preferably 600-700 DEG C), the time (12-24 hours), the coating of available silver concentration change of gradient, outermost layer Fu Yin
Layer, silver concentration successively decrease to material internal gradient, can form the silver-bearing copper diffusion coating with a thickness of (10-40 μm) on surface,
Or the equally distributed silver-bearing copper diffusion layer of silver-bearing copper ingredient, wherein yellow gold ingredient can be copper (94wt%-98wt%), silver
(6wt%-2wt%).Heat treatment time is reduced to improve diffuser efficiency for three layers of coating with Ag/Cu/Ag, designs allusion quotation
The copper layer thickness of type is (2-10 μm), and silver thickness is (0.1-2 μm), and heat treatment temperature is (500-650 DEG C, preferably 550-
600 DEG C), time (6-24 hours), available silver content is the uniform yellow gold coating of (3wt%-6wt%), this processing
The mode of method is equally applicable to Ag/Cu/Ag/Cu ... alternating deposit, details are not described herein.
After heat treatment be formed by silver-bearing copper concentration gradient distribution alloy coat, hardness be apparently higher than simple metallic copper with
Metallic silver, hardness is up to 188HV0.05, wear-resisting property is obviously improved；Simultaneously because graded elemental is distributed, potential difference gradient is reduced,
The galvanic corrosion risk due to caused by coating damage can be reduced, the corrosion resistance of coating, the outer surface of this external coating are improved
Rich silver layer and internal copper layer possess good electric conductivity.
This method includes step in detail below:
Step 1, oil removing cleaning
Alkaline degreasing solution is used in oil removing cleaning, ingredient is 30g/L sodium carbonate, 35g/L sodium phosphate, 40g/L hydroxide
Sodium, 75 DEG C after oil removing 15 minutes, clear water rinses.
Step 2, acid etch
It is impregnated 30 seconds in acid etch using 10% dilute sulfuric acid, clear water rinses.
Step 3, plating
Copper facing and silver plating solution can use copper electroplating solution and electrosilvering or electroless copper and chemical silvering solution, or
Person selects their combination of two to implement.
Copper plating solution in the step 3 can use typical sulfate electro-coppering system, and ingredient is 200g/L copper sulphate,
50g/L sulfuric acid, 0.1g/L lauryl sodium sulfate；Pyrophosphate method of electro-plating system, ingredient are as follows: 32g/L coke phosphorus can also be used
Sour copper, 120g/L potassium pyrophosphate, 12g/L tartaric acid,；Electroless copper system can also be used, if ingredient is 8g/L copper sulphate,
20g/L sodium citrate, 30g/L boric acid, 40g/L sodium hypophosphite, 0.8g/L nickel sulfate.(specific technological parameter such as electric current is close
Degree, temperature, pH value illustrate in embodiment)
Silver plating solution in the step 3 can use iodide plating silver solution, and ingredient is 12g/L silver iodide, 330g/
L potassium iodide, 0.1g/L neopelex, 1g/L tartaric acid.Glucose chemical silvering, ingredient can also be used are as follows:
3.5g/L silver nitrate, 2.5g/L sodium hydroxide, 4.5g/L glucose, 0.4g/L tartaric acid, 10g/L dehydrated alcohol, appropriate ammonium hydroxide.
Ethylenediamine chemical silvering solution can also be used: silver salt solution group becomes 10g/L silver nitrate, 50mL/L ammonium hydroxide, 20mL/L second two
Amine, 5g/L potassium hydroxide；Reducing agent solution group becomes 10g/L glucose, 2.5g/L sodium potassium tartrate tetrahydrate, 30mL/L ethyl alcohol, 50mg/
L polyethylene glycol.
Plating process in the step 3 can use the mode of Cu/Ag, Cu/Ag/Cu, Ag/Cu/Ag/Cu ... alternating deposit
It carries out；
Step 4, heat treatment
Plating obtained is placed in vacuum drying oven or special atmosphere oven to prevent surface oxidation, can choose 5-20
DEG C/heating rate of min, and preferably 5-10 DEG C/min, optimally 10 DEG C/min；Heat treatment temperature is maintained at 450-700 DEG C；It protects
Warm time 12-24 hours；Furnace cooling.
Concrete application is shown in following embodiment:
Embodiment 1
System is electroplated using sulfate in copper plating solution, and ingredient is 200g/L cupric sulfate pentahydrate, 50g/L sulfuric acid, 0.1g/L
Surfactant.Wherein surfactant is lauryl sodium sulfate, and temperature is 25 DEG C, electroplating current density 1-4A/dm2,
Preferably 2-4A/dm2.It is silver-plated using silver iodide be electroplated system, solution composition be 12g/L silver iodide, 330g/L potassium iodide,
0.1g/L neopelex, tank liquor temperature are 60 DEG C, adjust PH to 2.0, current density 0.5-1.0A/ with sulfuric acid
dm2。
It is 35 μm that control electroplating time, which obtains Cu layers, the Cu/Ag composite deposite that silver layer is 15 μm, and heat treatment heating rate is
10 DEG C/min, holding temperature is 700 DEG C, and soaking time is 24 hours.Obtained coating as shown in Figure 1, outermost layer is fine silver layer,
The copper sliver diffusion layer with a thickness of 15 μm is obtained in copper silver layer interface, wherein silver layer accounts for 10 μm, and layers of copper accounts for 5 μm.Outermost layer silver layer
Hardness is 88HV0.05, conductivity 97%IACS, inner layer since copper silver solution strengthening, hardness gradually rise, conductivity by
Gradually decline, at silver-colored 18 μm of the surface layer of distance, hardness highest is 179HV0.05, it is seen then that the present embodiment floating coat after heat treatment obtains
The certain change of gradient of diffusion layer copper silver concentration arrived, also changes in gradient so as to cause hardness and electric conductivity；By material grinding and polishing
After 18 μm, conductivity 55%IACS, copper silver content is copper 96wt%, silver-colored 4wt%.
Embodiment 2
Copper facing uses sodium hypophosphite electroless copper system, solution composition are as follows: 8g/L cupric sulfate pentahydrate, 20g/L lemon
Sour sodium, 30g/L boric acid, 40g/L sodium hypophosphite, 0.8g/L nickel sulfate.PH to 9.5 is adjusted with sodium hydroxide, tank liquor temperature is
75℃.It is silver-plated to use glucose chemical silvering system, plating solution composition are as follows: 3.5g/L silver nitrate, 2.5g/L sodium hydroxide,
4.5g/L glucose, 0.4g/L tartaric acid, 10g/L dehydrated alcohol, appropriate ammonium hydroxide, adjust PH to 10.5,60 DEG C of tank liquor temperature.Its
Sensitization activation processing, sensitizing solution ingredient are carried out before middle electroless copper are as follows: 10g/L stannous chloride, 40ml/L hydrochloric acid, sensitizing temperature
It is 30 DEG C, time 3-5 minute.Activating solution are as follows: 0.5g/L palladium chloride, 20ml/L hydrochloric acid, 40 DEG C of temperature, time 3-5 minute.
Control plating time obtains the Ag/Cu/Ag composite deposite that silver layer is respectively 2 μm, 6 μ m-thick of layers of copper, heat treatment heating
Rate is 10 DEG C/min, and holding temperature is 600 DEG C, and soaking time is 24 hours, obtains the coating of copper silver concentration change of gradient, such as
Shown in Fig. 2.Two sides are the faces Fu Yin, silver content 93wt%, copper 7wt%, and inner layer silver concentration gradient is successively decreased, copper content gradient
It is incremented by, is respectively formed 3 μm of copper sliver diffusion layer in two sides, coating surface hardness is 135HV0.05, conductivity 82%IACS.
Embodiment 3
Copper facing is electroplated using ethylenediamine system, plating solution composition are as follows: 100g/L cupric sulfate pentahydrate, 12g/L tartaric acid, 60g/
L ethylenediamine, 4g/L potassium nitrate adjust PH to 8-9 with potassium hydroxide solution, and tank liquor temperature is 60 DEG C, current density 2-4A/dm2。
It is silver-plated to be electroplated using niacin system, ingredient are as follows: 40g/L silver nitrate, 77g/L ammonium acetate, 32ml/L ammonium hydroxide, 50g/L hydroxide
Potassium, 90g/L niacin, 75g/L potassium carbonate, with nitric acid adjust PH to 9.0,20 DEG C of tank liquor temperature, current density 0.1-0.8A/dm2。
Current density and electroplating time are adjusted, obtains that silver layer is respectively 0.1 μm, layers of copper is respectively 1 μm of silver layer and layers of copper
Ag/Cu/Ag/Cu/Ag/Cu/Ag/Cu/Ag/Cu/Ag composite deposite；As shown in the upper figure of Fig. 3.Handle heating rate be 10 DEG C/
Min, holding temperature are 600 DEG C, and soaking time is 12 hours, obtain Kufil material that silver layer is spread completely (under such as Fig. 3
Figure), silver atoms are spread completely in layers of copper, form the Kufil material that silver content is 3.4wt%, and hardness can reach
188HV0.05, surface conductivity 65%IACS.This also illustrates the thickness of coating and the time of heat treatment and temperature all can
Directly affect heat treatment after as a result, coating is thinner, heat treatment temperature is higher, and the time is longer, spread it is more thorough.
In conclusion the invention proposes multilayer electro-deposition assistant alloys to expand the design side that infiltration prepares silver-bearing copper contact material
Method expands cementation process by the arrangement and heat treatment of design depositing silver layers and layers of copper, and obtain has silver, copper ingredient uniform respectively
The silver-bearing copper of distribution or silver-colored, copper ingredient distribution gradient typical organization expands impregnation coating, and wherein component gradient is distributed
Coating has the characteristics that corrosion potential gradient distribution, can reduce the galvanic couple accelerated corrosion wind due to caused by surface covering breakage
Danger.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (9)
1. a kind of preparation method for contact material silver-bearing copper diffusion layer, which is characterized in that described method includes following steps:
S1, it be spaced copper facing in substrate, is silver-plated, or being spaced silver-plated, copper facing, obtaining copper silver composite deposite；The copper silver Composite Coatings
Copper layer thickness is 1-50 μm in layer, and silver thickness is 0.1-20 μm；
S2, the copper silver composite deposite are placed in vacuum drying oven or special atmosphere oven, are warming up to 5-20 DEG C/min of heating rate
450-800 DEG C carries out heat treatment 6-24 hours to get the silver-bearing copper diffusion layer.
2. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that the copper silver
Composite deposite is the spaced bilayer or multilayer coating of Cu/Ag, or is the spaced bilayer or multilayer coating of Ag/Cu.
3. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that the copper silver
Composite deposite is the double-deck coating of Cu/Ag, and wherein copper layer thickness is 5-50 μm, and silver thickness is 2-20 μm,；The heat treatment temperature
Degree is 550-800 DEG C, and heat treatment time is 12-24 hours.
4. being used for the preparation method of contact material silver-bearing copper diffusion layer as claimed in claim 3, which is characterized in that the layers of copper
With a thickness of 10-35 μm, silver thickness is 5-15 μm；The heat treatment temperature is 600-750 DEG C.
5. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that the copper silver
Composite deposite is three layers of coating of Ag/Cu/Ag, and wherein copper layer thickness is 2-10 μm, and each silver thickness is 0.1-2 μm, at heat
Managing temperature is 500-650 DEG C, and heat treatment time is 6-24 hours.
6. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that the copper silver
Composite deposite is Ag/Cu/Ag/Cu/Ag/Cu/Ag/Cu/Ag/Cu/Ag coating, wherein each copper layer thickness is 1-5 μm, each
Silver thickness is 0.1-1 μm, and heat treatment temperature is 550-650 DEG C, and heat treatment time is 6-24 hours.
7. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that the copper facing
Using sodium hypophosphite chemical plating, the plating of aldehydes organic-matter chemical, acidiccopper plating or pyrophosphate copper plating.
8. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that described silver-plated
It is silver-plated using ethylenediamine chemical silvering or silver iodide plating.
9. being used for the preparation method of contact material silver-bearing copper diffusion layer as described in claim 1, which is characterized in that the substrate
For Copper substrate.
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