CN118237578A - 一种添加镍过渡层镀银铜粉的制备方法 - Google Patents
一种添加镍过渡层镀银铜粉的制备方法 Download PDFInfo
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- CN118237578A CN118237578A CN202410196827.8A CN202410196827A CN118237578A CN 118237578 A CN118237578 A CN 118237578A CN 202410196827 A CN202410196827 A CN 202410196827A CN 118237578 A CN118237578 A CN 118237578A
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- copper powder
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 138
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 17
- 230000007704 transition Effects 0.000 title claims abstract description 16
- 238000007747 plating Methods 0.000 claims abstract description 26
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052709 silver Inorganic materials 0.000 claims abstract description 22
- 239000004332 silver Substances 0.000 claims abstract description 22
- 230000004913 activation Effects 0.000 claims abstract description 21
- 238000011282 treatment Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 7
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 7
- 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 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000001119 stannous chloride Substances 0.000 claims description 6
- 235000011150 stannous chloride Nutrition 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 150000002815 nickel Chemical class 0.000 claims description 4
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 3
- XXSPKSHUSWQAIZ-UHFFFAOYSA-L 36026-88-7 Chemical compound [Ni+2].[O-]P=O.[O-]P=O XXSPKSHUSWQAIZ-UHFFFAOYSA-L 0.000 claims description 3
- 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 3
- 239000001263 FEMA 3042 Substances 0.000 claims description 3
- 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 claims description 3
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 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 claims description 3
- 235000011083 sodium citrates Nutrition 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 3
- 229940033123 tannic acid Drugs 0.000 claims description 3
- 235000015523 tannic acid Nutrition 0.000 claims description 3
- 229920002258 tannic acid Polymers 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 235000010338 boric acid Nutrition 0.000 claims description 2
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 2
- 239000001384 succinic acid Substances 0.000 claims description 2
- 235000011044 succinic acid Nutrition 0.000 claims description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 6
- 230000003213 activating effect Effects 0.000 claims 4
- 238000005406 washing Methods 0.000 claims 3
- 235000019441 ethanol Nutrition 0.000 claims 2
- 238000001914 filtration Methods 0.000 claims 2
- GSYUXYXARXLYDO-UHFFFAOYSA-N butanedioic acid;2-hydroxybenzoic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)C1=CC=CC=C1O GSYUXYXARXLYDO-UHFFFAOYSA-N 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 125000003396 thiol group Chemical class [H]S* 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 10
- 229910052802 copper Inorganic materials 0.000 abstract description 8
- 239000010949 copper Substances 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000005307 ferromagnetism Effects 0.000 abstract description 2
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910017770 Cu—Ag Inorganic materials 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1689—After-treatment
- C23C18/1692—Heat-treatment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Powder Metallurgy (AREA)
Abstract
本发明属于新材料技术领域，具体涉及一种添加镍过渡层镀银铜粉的制备方法，包括如下步骤：（1）前处理与活化处理、（2）制备镍包铜粉、（3）表面有机修饰、（4）表面镀银、（5）镀后处理；本发明通过在银包铜粉中间添加过渡层镍，并在保护气氛下进行热处理，通过铜、镍、银之间的扩散形成金属间化合物，形成金属间共价键结合，从而提高镀层的结合力。同时采用镍作为中间层，一方面可以提高铜层包覆的致密性，提高其高温抗氧化能力，另一方面，由于镍具有良好的导磁性，在提高铜粉的抗氧化性同时也增加了粉体的铁磁性，实现低频下的磁屏蔽，使所制得的粉体可以在更宽的频段范围内实现电磁屏蔽。
Description
技术领域
本发明属于新材料技术领域，具体涉及一种添加镍过渡层镀银铜粉的制备方法。
背景技术
金属铜粉因其优异的导电性而被广泛用于导电填料和电磁屏蔽领域，然而铜粉活性较高，在空气中极易氧化，从而使其导电性迅速降低。为解决这一问题，目前主要采用包覆法，即在铜粉表面包覆一层致密的有机薄膜或惰性金属，以隔绝氧气，避免铜粉氧化。但是有机物包覆薄膜在高温下容易分解限制了其使用。惰性金属包覆法不仅可提高粉末的常温抗氧化能力，而且使铜粉具有十分理想的高温抗氧化性。金属银是优异的导体，其化学性质也十分稳定。因此，以银包覆铜粉是解决铜粉氧化问题的最佳方案。
目前，银包铜粉大多采用置换、化学还原或者二者结合的方法，如中国专利CN102773475B一种导电浆料用抗氧化铜银复合粉及其制备方法，采用置换反应在铜粉表面包覆一层银，然后利用还原剂还原硝酸银使银层更加致密。中国专利CN100467169C一种Cu-Ag核壳复合金属粉末的制备工艺，该工艺包括预镀、两次还原处理和两次气氛炉致密化处理，工艺复杂，成本高。
因此，现有的银包铜粉存在生产工艺复杂，镀层均匀性差，包覆效果差，不耐高温等问题，使其应用领域受到限制。
发明内容
本发明在于解决上述问题，提供了一种添加镍过渡层镀银铜粉的制备方法，用于解决现有银包铜粉存在的抗氧化性差及镀层结合力不佳的问题。此外，通过添加镍过渡层，还进一步提高了粉体在低频频段的屏蔽性能，制备的粉体具有宽屏屏蔽的效果。
本发明是通过如下技术方案实现的：一种添加镍过渡层镀银铜粉的制备方法，其特征在于，步骤如下：
（1）前处理与活化处理
前处理：将铜粉在5%氢氧化钠溶液中清洗30-60min进行表面除油后用去离子水清洗干净；再用5%稀硫酸清洗30-60min除去表面的氧化层后用去离子水清洗干净；
配置活化液：氯化钯0.5-2g/L，37%盐酸100-500mL/L，氯化亚锡20-80g/L，温度18-30℃，活化时间1-3min；
活化处理：将铜粉置于活化液中活化，或是在铜粉镀镍开始时在镀液中添加活性金属活化；
（2）制备镍包铜粉
配置镀镍液：主盐：10-50g/L，还原剂：20-80 g/L，络合剂20-60 g/L，稳定剂：5-30mg/L，温度60-90℃，超声功率40-50w；
将活化处理过的铜粉在超声搅拌条件下加入配置好的镀镍液中反应30-60min，然后过滤洗涤、干燥，得到镍包铜粉；
（3）表面有机修饰
将镍包铜粉置于水与乙醇的混合溶液中，水浴加热搅拌，时间为5-10min，水与乙醇的体积比为1:1-1:3，水浴温度为60-80℃；加入镍包铜粉质量的0.5%-10%表面修饰剂，搅拌均匀，保持溶液温度60-80℃，搅拌时间为0.5-4h，随后抽滤，用无水乙醇清洗1-2遍，干燥，得到表面修饰的镍包铜粉；
（4）表面镀银
将有机修饰过的镍包铜粉加入0.05-5g/LPVP去离子水中超声搅拌下分散，同时滴入银氨溶液和还原剂，室温反应30-60min后过滤洗涤、干燥，得到以镍为中间层的银包铜粉；
（5）镀后处理
将步骤（4）所得的复合粉体在保护气氛下热处理1-4h，热处理温度为100—400℃，随炉冷却取出，即得到含有镍中间层的银包铜粉。
进一步地，步骤（1）还可以由如下方案替换：用质量分数37％的盐酸对铜粉进行酸化处理，然后将酸化后的铜粉加入到含5g/L的氯化亚锡的盐酸溶液中浸泡5-20min活化；
或用质量分数37％的盐酸对铜粉进行酸化处理15-30min后清洗，再用质量分数37％的盐酸对铜粉进行活化处理15-30min后清洗。
进一步地，步骤（2）配置镀镍液时，所述主盐采用硫酸镍、乙酸镍或次磷酸镍中的任意一种；所述还原剂采用水合肼、次亚磷酸钠或硼氢化钠中的任意一种；所述络合剂采用柠檬酸钠、硫酸铵、乳酸、苹果酸、硼酸、琥珀酸、丁二酸活水杨酸中的任意一种；所述稳定剂采用不饱和脂肪酸、马来酸或硫脲中的任意一种。
进一步地，步骤（3）中表面修饰剂采用含巯基的硅烷偶联剂、单宁酸或盐酸多巴胺的任意一种，其中干燥温度为100-150℃，干燥时间为1-24h。
进一步地，步骤（4）中的还原剂采用为葡萄糖、酒石酸钾钠或甲醛，浓度为4-20g/L；银氨溶液浓度为10-50g/L。
本发明的有益效果是：本发明通过在银包铜粉中间添加过渡层镍，并在保护气氛下进行热处理，通过铜、镍、银之间的扩散形成金属间化合物，形成金属间共价键结合，从而提高镀层的结合力。同时采用镍作为中间层，一方面可以提高铜层包覆的致密性，提高其高温抗氧化能力，另一方面，由于镍具有良好的导磁性，在提高铜粉的抗氧化性同时也增加了粉体的铁磁性，实现低频下的磁屏蔽，使所制得的粉体可以在更宽的频段范围内实现电磁屏蔽。
具体实施方式
为了使本发明的目的、技术方案及有益效果更加清楚明白，下面结合实施例对本发明中的技术方案进一步说明。
实施例1：
一种添加镍过渡层镀银铜粉的制备方法，包括下述步骤：
（1）前处理
将铜粉在5%氢氧化钠溶液中清洗30min，除油后，再用5%稀硫酸清洗30min除去表面的氧化层后用去离子水清洗干净。
（2）活化处理
因铜在化学镀镍过程中没有自催化作用，要在铜粉表面沉积镍-磷合金，通常是采用接触活化或电化学的方法对铜进行活化。本发明铜粉活化处理工艺可采用如下方案：将铜粉置于活化液中活化，配置活化液：氯化钯0.5g/L，37%盐酸100mL/L，氯化亚锡20g/L，温度20℃，活化时间2min；
（3）配置镀镍液
硫酸镍10g/L，水合肼20g/L，柠檬酸钠20g/L，马来酸5mg/L，温度60℃，超声功率40w。
（4）制备镍包铜粉
将活化处理过的铜粉在超声搅拌条件下加入步骤（3）的镀镍液中，反应30min后过滤洗涤、干燥即得到镍包铜粉。
（5）镍包铜粉表面有机修饰
加入铜粉质量的1%的KH550硅烷偶联剂，超声搅拌均匀，保持溶液温度为72℃，搅拌时间为1h，随后抽滤，用乙醇清洗一遍，在120℃干燥箱中干燥5h；
（6）镍包铜粉包覆银
将步骤（5）制得的镍包铜粉加入0.05g/LPVP去离子水中超声搅拌下分散，同时滴入30g/L银氨溶液和10g/L葡萄糖溶液，室温反应30min后过滤洗涤、干燥即得到以镍为中间层的镀银铜粉。
（7）镀后处理
将步骤（6）所得的复合粉体在保护气氛下热处理2h，随炉冷却取出，即得到含有镍中间层的银包铜粉。
实施例2：
一种添加镍过渡层镀银铜粉的制备方法，包括下述步骤：
（1）前处理与活化处理
用质量分数37％的盐酸对铜粉进行酸化处理，然后将酸化后的铜粉加入到含5g/L的氯化亚锡的盐酸溶液中浸泡5-20 min。
（2）配置镀镍液
乙酸镍30g/L，次磷酸钠30g/L，乳酸30g/L，硫脲10mg/L，温度70℃，超声功率40w。
（3）制备镍包铜粉
将活化处理过的铜粉在超声搅拌条件下加入步骤（2）的镀镍液中，反应40min后过滤洗涤、干燥即得到镍包铜粉。
（4）镍包铜粉表面有机修饰
加入铜粉质量的10%的A189硅烷偶联剂，超声搅拌均匀，保持溶液温度为75℃，搅拌时间为0.5h，随后抽滤，用无水乙醇清洗两遍，在120℃干燥箱中干燥3h；
（5）镍包铜粉表面包覆银
将步骤（4）制得的镍包铜粉加入1g/LPVP去离子水中超声搅拌下分散，同时滴入25g/L银氨溶液和50g/L酒石酸钾钠溶液，室温反应40min后过滤洗涤、干燥即得到镀银铜粉。
（6）镀后处理
将步骤（5）所得的复合粉体在保护气氛下热处理3h，随炉冷却取出，即得到含有镍中间层的银包铜粉。
实施例3：
一种添加镍过渡层镀银铜粉的制备方法，包括下述步骤：
（1）前处理与活化处理
采用质量分数37％的盐酸对铜粉进行酸化处理30min后清洗，再用质量分数37％的盐酸对铜粉进行活化处理30min后清洗；
（2）配置镀镍液
次磷酸镍50g/L，硼氢化钠60g/L，苹果酸60g/L，硫脲20mg/L，温度90℃，超声功率50w。
（3）制备镍包铜粉
将活化处理过的铜粉在超声搅拌条件下加入步骤（2）的镀镍液中，反应60min后过滤洗涤、干燥即得到镍包铜粉。
（4）镍包铜粉表面有机修饰
加入铜粉质量的5%的单宁酸，超声搅拌均匀，保持溶液温度为75℃，搅拌时间为1h，随后抽滤，用无水乙醇清洗两遍，在120℃干燥箱中干燥2.5h；
（5）镍包铜粉包覆银
将步骤（4）制得的镍包铜粉加入3g/LPVP去离子水中超声搅拌下分散，同时滴入50g/L银氨溶液和30g/L酒石酸钾钠溶液，室温反应60min后过滤洗涤、干燥即得到镀银铜粉。
（6）镀后处理
将步骤（5）所得的复合粉体在保护气氛下热处理4h，随炉冷却取出，即得到含有镍中间层的银包铜粉。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。除说明书所述技术特征外，其余技术特征均为本领域技术人员已知技术。
Claims (5)
1.一种添加镍过渡层镀银铜粉的制备方法，其特征在于，步骤如下：
（1）前处理与活化处理
前处理：将铜粉在5%氢氧化钠溶液中清洗30-60min进行表面除油后用去离子水清洗干净；再用5%稀硫酸清洗30-60min除去表面的氧化层后用去离子水清洗干净；
配置活化液：氯化钯0.5-2g/L，37%盐酸100-500mL/L，氯化亚锡20-80g/L，温度18-30℃，活化时间1-3min；
活化处理：将铜粉置于活化液中活化，或是在铜粉镀镍开始时在镀液中添加活性金属活化；
（2）制备镍包铜粉
配置镀镍液：主盐：10-50g/L，还原剂：20-80 g/L，络合剂20-60 g/L，稳定剂：5-30 mg/L，温度60-90℃，超声功率40-50w；
将活化处理过的铜粉在超声搅拌条件下加入配置好的镀镍液中反应30-60min，然后过滤洗涤、干燥，得到镍包铜粉；
（3）表面有机修饰
将镍包铜粉置于水与乙醇的混合溶液中，水浴加热搅拌，时间为5-10min，水与乙醇的体积比为1:1-1:3，水浴温度为60-80℃；加入镍包铜粉质量的0.5%-10%表面修饰剂，搅拌均匀，保持溶液温度60-80℃，搅拌时间为0.5-4h，随后抽滤，用无水乙醇清洗1-2遍，干燥，得到表面修饰的镍包铜粉；
（4）表面镀银
将有机修饰过的镍包铜粉加入0.05-5g/LPVP去离子水中超声搅拌下分散，同时滴入银氨溶液和还原剂，室温反应30-60min后过滤洗涤、干燥，得到以镍为中间层的银包铜粉；
（5）镀后处理
将步骤（4）所得的复合粉体在保护气氛下热处理1-4h，热处理温度为100—400℃，随炉冷却取出，即得到含有镍中间层的银包铜粉。
2.根据权利要求1所述的一种添加镍过渡层镀银铜粉的制备方法，其特征在于，步骤（1）还可以由如下方案替换：用质量分数37％的盐酸对铜粉进行酸化处理，然后将酸化后的铜粉加入到含5g/L的氯化亚锡的盐酸溶液中浸泡5-20min活化；
或用质量分数37％的盐酸对铜粉进行酸化处理15-30min后清洗，再用质量分数37％的盐酸对铜粉进行活化处理15-30min后清洗。
3.根据权利要求1所述的一种添加镍过渡层镀银铜粉的制备方法，其特征在于，步骤（2）配置镀镍液时，所述主盐采用硫酸镍、乙酸镍或次磷酸镍中的任意一种；所述还原剂采用水合肼、次亚磷酸钠或硼氢化钠中的任意一种；所述络合剂采用柠檬酸钠、硫酸铵、乳酸、苹果酸、硼酸、琥珀酸、丁二酸活水杨酸中的任意一种；所述稳定剂采用不饱和脂肪酸、马来酸或硫脲中的任意一种。
4.根据权利要求1所述的一种添加镍过渡层镀银铜粉的制备方法，其特征在于，步骤（3）中表面修饰剂采用含巯基的硅烷偶联剂、单宁酸或盐酸多巴胺的任意一种，其中干燥温度为100-150℃，干燥时间为1-24h。
5.根据权利要求1所述的一种添加镍过渡层镀银铜粉的制备方法，其特征在于，步骤（4）中的还原剂采用为葡萄糖、酒石酸钾钠或甲醛，浓度为4-20g/L；银氨溶液浓度为10-50g/L。
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