CN115710701A - 一种化学镀金液和应用 - Google Patents
一种化学镀金液和应用 Download PDFInfo
- Publication number
- CN115710701A CN115710701A CN202211654207.1A CN202211654207A CN115710701A CN 115710701 A CN115710701 A CN 115710701A CN 202211654207 A CN202211654207 A CN 202211654207A CN 115710701 A CN115710701 A CN 115710701A
- Authority
- CN
- China
- Prior art keywords
- gold
- salt
- acid
- alkyl
- group
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000010931 gold Substances 0.000 title claims abstract description 124
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 124
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000007747 plating Methods 0.000 title claims abstract description 44
- 239000000126 substance Substances 0.000 title abstract description 19
- 239000008139 complexing agent Substances 0.000 claims abstract description 31
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 29
- 239000003381 stabilizer Substances 0.000 claims abstract description 23
- -1 gold ion Chemical class 0.000 claims description 57
- 150000003839 salts Chemical class 0.000 claims description 51
- 125000004400 (C1-C12) alkyl group Chemical group 0.000 claims description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 18
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 17
- 229910052700 potassium Inorganic materials 0.000 claims description 17
- 239000011591 potassium Substances 0.000 claims description 17
- 229960003975 potassium Drugs 0.000 claims description 17
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 16
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 125000003172 aldehyde group Chemical group 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 12
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 125000003277 amino group Chemical group 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 125000001424 substituent group Chemical group 0.000 claims description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052763 palladium Inorganic materials 0.000 claims description 9
- 125000000229 (C1-C4)alkoxy group Chemical group 0.000 claims description 8
- 239000004471 Glycine Substances 0.000 claims description 8
- 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 claims description 8
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 8
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- 150000001299 aldehydes Chemical class 0.000 claims description 5
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 5
- 239000001630 malic acid Substances 0.000 claims description 5
- 235000011090 malic acid Nutrition 0.000 claims description 5
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 claims description 5
- ZWZLRIBPAZENFK-UHFFFAOYSA-J sodium;gold(3+);disulfite Chemical compound [Na+].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O ZWZLRIBPAZENFK-UHFFFAOYSA-J 0.000 claims description 5
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 4
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims description 4
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 4
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 4
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 125000002252 acyl group Chemical group 0.000 claims description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 4
- 125000004093 cyano group Chemical group *C#N 0.000 claims description 4
- YMAWOPBAYDPSLA-UHFFFAOYSA-N glycylglycine Chemical compound [NH3+]CC(=O)NCC([O-])=O YMAWOPBAYDPSLA-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- SFDJOSRHYKHMOK-UHFFFAOYSA-N nitramide Chemical group N[N+]([O-])=O SFDJOSRHYKHMOK-UHFFFAOYSA-N 0.000 claims description 4
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 4
- 229960003330 pentetic acid Drugs 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims description 4
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 4
- CYQGCJQJIOARKD-UHFFFAOYSA-N 4-carboxy-TEMPO Chemical group CC1(C)CC(C(O)=O)CC(C)(C)N1[O] CYQGCJQJIOARKD-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 3
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 claims description 3
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 3
- CEGDSRUGKSIHHO-UHFFFAOYSA-N 1,2-diaminoethane-1,1,2,2-tetrol Chemical compound NC(O)(O)C(N)(O)O CEGDSRUGKSIHHO-UHFFFAOYSA-N 0.000 claims description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- XNCSCQSQSGDGES-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)C(C)CN(CC(O)=O)CC(O)=O XNCSCQSQSGDGES-UHFFFAOYSA-N 0.000 claims description 2
- IWTIBPIVCKUAHK-UHFFFAOYSA-N 3-[bis(2-carboxyethyl)amino]propanoic acid Chemical compound OC(=O)CCN(CCC(O)=O)CCC(O)=O IWTIBPIVCKUAHK-UHFFFAOYSA-N 0.000 claims description 2
- UXBLSWOMIHTQPH-UHFFFAOYSA-N 4-acetamido-TEMPO Chemical group CC(=O)NC1CC(C)(C)N([O])C(C)(C)C1 UXBLSWOMIHTQPH-UHFFFAOYSA-N 0.000 claims description 2
- XUXUHDYTLNCYQQ-UHFFFAOYSA-N 4-amino-TEMPO Chemical group CC1(C)CC(N)CC(C)(C)N1[O] XUXUHDYTLNCYQQ-UHFFFAOYSA-N 0.000 claims description 2
- BKENZAFIBRCMKD-UHFFFAOYSA-N 4-isothiocyanato-1-$l^{1}-oxidanyl-2,2,6,6-tetramethylpiperidine Chemical group CC1(C)CC(N=C=S)CC(C)(C)N1[O] BKENZAFIBRCMKD-UHFFFAOYSA-N 0.000 claims description 2
- BOTWFBJTUJHJAI-UHFFFAOYSA-J C(C(S)CC(=O)[O-])(=O)[O-].[K+].[Au+3].C(C(S)CC(=O)[O-])(=O)[O-] Chemical compound C(C(S)CC(=O)[O-])(=O)[O-].[K+].[Au+3].C(C(S)CC(=O)[O-])(=O)[O-] BOTWFBJTUJHJAI-UHFFFAOYSA-J 0.000 claims description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 108010008488 Glycylglycine Proteins 0.000 claims description 2
- FSVCELGFZIQNCK-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)glycine Chemical compound OCCN(CCO)CC(O)=O FSVCELGFZIQNCK-UHFFFAOYSA-N 0.000 claims description 2
- JYXGIOKAKDAARW-UHFFFAOYSA-N N-(2-hydroxyethyl)iminodiacetic acid Chemical compound OCCN(CC(O)=O)CC(O)=O JYXGIOKAKDAARW-UHFFFAOYSA-N 0.000 claims description 2
- QYTDEUPAUMOIOP-UHFFFAOYSA-N TEMPO Chemical group CC1(C)CCCC(C)(C)N1[O] QYTDEUPAUMOIOP-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- FYNVXASLFHXUBV-UHFFFAOYSA-K [Au+3].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[Na+] Chemical compound [Au+3].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[Na+] FYNVXASLFHXUBV-UHFFFAOYSA-K 0.000 claims description 2
- CPDKISYFHRCKRW-UHFFFAOYSA-J [K+].[Au+3].[O-]S([O-])(=O)=S.[O-]S([O-])(=O)=S Chemical compound [K+].[Au+3].[O-]S([O-])(=O)=S.[O-]S([O-])(=O)=S CPDKISYFHRCKRW-UHFFFAOYSA-J 0.000 claims description 2
- ZHSOHGDJTZDDIF-UHFFFAOYSA-N acetic acid;2-(2-aminoethylamino)ethane-1,1-diol Chemical compound CC(O)=O.CC(O)=O.NCCNCC(O)O ZHSOHGDJTZDDIF-UHFFFAOYSA-N 0.000 claims description 2
- RUSUZAGBORAKPY-UHFFFAOYSA-N acetic acid;n'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCNCCNCCN RUSUZAGBORAKPY-UHFFFAOYSA-N 0.000 claims description 2
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 claims description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 2
- YPKDXMUXIRQHAU-UHFFFAOYSA-N azane;gold;thiocyanic acid Chemical compound N.[Au].SC#N YPKDXMUXIRQHAU-UHFFFAOYSA-N 0.000 claims description 2
- AGHHWJYXGRYSLG-UHFFFAOYSA-K azanium dioxido-oxo-sulfanylidene-lambda6-sulfane gold(3+) Chemical compound [NH4+].[Au+3].[O-]S([O-])(=O)=S.[O-]S([O-])(=O)=S AGHHWJYXGRYSLG-UHFFFAOYSA-K 0.000 claims description 2
- GABPAXJCPQEORA-UHFFFAOYSA-K azanium;gold(3+);disulfite Chemical compound [NH4+].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O GABPAXJCPQEORA-UHFFFAOYSA-K 0.000 claims description 2
- WPEJSSRSFRWYJB-UHFFFAOYSA-K azanium;tetrachlorogold(1-) Chemical compound [NH4+].[Cl-].[Cl-].[Cl-].[Cl-].[Au+3] WPEJSSRSFRWYJB-UHFFFAOYSA-K 0.000 claims description 2
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 2
- 239000000174 gluconic acid Substances 0.000 claims description 2
- 235000012208 gluconic acid Nutrition 0.000 claims description 2
- 229940043257 glycylglycine Drugs 0.000 claims description 2
- 229940015045 gold sodium thiomalate Drugs 0.000 claims description 2
- 229940083577 gold sodium thiosulfate Drugs 0.000 claims description 2
- MXZVHYUSLJAVOE-UHFFFAOYSA-N gold(3+);tricyanide Chemical compound [Au+3].N#[C-].N#[C-].N#[C-] MXZVHYUSLJAVOE-UHFFFAOYSA-N 0.000 claims description 2
- PWSKHLMYTZNYKO-UHFFFAOYSA-N heptane-1,7-diamine Chemical compound NCCCCCCCN PWSKHLMYTZNYKO-UHFFFAOYSA-N 0.000 claims description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 2
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 claims description 2
- ZMBNHDLIADCPCO-UHFFFAOYSA-K potassium gold(3+) 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[K+].[Au+3] ZMBNHDLIADCPCO-UHFFFAOYSA-K 0.000 claims description 2
- WSHYKIAQCMIPTB-UHFFFAOYSA-M potassium;2-oxo-3-(3-oxo-1-phenylbutyl)chromen-4-olate Chemical compound [K+].[O-]C=1C2=CC=CC=C2OC(=O)C=1C(CC(=O)C)C1=CC=CC=C1 WSHYKIAQCMIPTB-UHFFFAOYSA-M 0.000 claims description 2
- RRDWZGMHSCBIGX-UHFFFAOYSA-J potassium;gold(3+);disulfite Chemical compound [K+].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O RRDWZGMHSCBIGX-UHFFFAOYSA-J 0.000 claims description 2
- PPAHQJUSSZLWHV-UHFFFAOYSA-J potassium;gold(3+);tetrathiocyanate Chemical compound [K+].[Au+3].[S-]C#N.[S-]C#N.[S-]C#N.[S-]C#N PPAHQJUSSZLWHV-UHFFFAOYSA-J 0.000 claims description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 2
- NUTOYZZSFLIOKI-UHFFFAOYSA-J sodium gold(3+) tetrathiocyanate Chemical compound [Na+].[Au+3].[S-]C#N.[S-]C#N.[S-]C#N.[S-]C#N NUTOYZZSFLIOKI-UHFFFAOYSA-J 0.000 claims description 2
- AGHLUVOCTHWMJV-UHFFFAOYSA-J sodium;gold(3+);2-sulfanylbutanedioate Chemical compound [Na+].[Au+3].[O-]C(=O)CC(S)C([O-])=O.[O-]C(=O)CC(S)C([O-])=O AGHLUVOCTHWMJV-UHFFFAOYSA-J 0.000 claims description 2
- 239000001384 succinic acid Substances 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 2
- KZNBHWLDPGWJMM-UHFFFAOYSA-J trisodium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane;gold(1+);dihydrate Chemical compound O.O.[Na+].[Na+].[Na+].[Au+].[O-]S([O-])(=O)=S.[O-]S([O-])(=O)=S KZNBHWLDPGWJMM-UHFFFAOYSA-J 0.000 claims description 2
- 150000002343 gold Chemical class 0.000 claims 2
- BSIDXUHWUKTRQL-UHFFFAOYSA-N nickel palladium Chemical compound [Ni].[Pd] BSIDXUHWUKTRQL-UHFFFAOYSA-N 0.000 claims 2
- OCIQOBBYJWEKSA-UHFFFAOYSA-N 1-$l^{1}-oxidanyl-2,2,6,6-tetramethylpiperidine-4-carbonitrile Chemical group CC1(C)CC(C#N)CC(C)(C)N1[O] OCIQOBBYJWEKSA-UHFFFAOYSA-N 0.000 claims 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 20
- 230000008021 deposition Effects 0.000 abstract description 6
- 239000006076 specific stabilizer Substances 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 24
- 238000010438 heat treatment Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 8
- 238000005406 washing Methods 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 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 description 5
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Landscapes
- Chemically Coating (AREA)
Abstract
本发明公开了一种化学镀金液,包括以下组分:金离子源0.1‑5g/L,络合剂5‑200 g/L,金离子还原剂1‑50 g/L,稳定剂0.01‑100mg/L;络合剂至少同时包含2种及以上不同的络合剂。本发明通过采用特定的稳定剂以及至少同时包含2种及以上不同的络合剂,使得本发明的化学镀金液具有稳定、低析出风险的优点,从而延长镀金浴的寿命,而且能够明显提升镀金时金沉积的均一性。
Description
技术领域
本发明涉及化学镀金技术领域。
背景技术
镍钯金表面处理工艺起于1990年代中期,主要作为化学镍金(ENIG)的一种改进工艺。在镍层与金层之间多一层钯层,钯层能够抑制金对镍层的过度攻击,减少镍的过度腐蚀,避免黑镍(black pad)出现。除了能正常满足传统焊接的需要外,镍钯金表面非常适于金线、铝线邦定(wire-bonding),在高端印刷电路板如IC载板(chip-carrier board)、覆晶(flip chip)以及摄像头模组等电子行业领域应用广泛。镍钯金有多种沉积路线,根据钯的不同可分为ENEP与ENIP,钯层又有纯钯与磷钯两种,但目前市场上以ENEP为主,ENIP比较少见;根据金的不同可分为ENEPIG与ENEPEG,目前市场上比较成熟的产品主要是ENEPIG。但由于置换金的反应特性,易出现甩金、镍腐蚀等问题,还原金的开发变得日渐重要。
还原型镀金的过程与置换金过程最大的不同在于金离子得到电子方式不同:还原金中金离子得到的电子来自于槽液中还原剂释放出来的电子,而置换金中的电子来自于镍层释放电子。
与置换金相比,还原金有以下优点:
(1)金层镀层均一性好,降低金盐消耗;
(2)金槽沉速快,能提升产能;
(3)表面和切片镍腐蚀表现均优秀,达到1级水平;
(4)结合力与打线性能优秀且稳定;
(5)能适配镍钯金、薄镍钯金、钯金工艺。
但是,目前市场应用并不广泛,主要是还原金的技术难度大,药水稳定性差,寿命短,药水使用成本高。目前市面上大多的做法是往金槽中额外加入氰化合物,然而氰化合物是毒性高的管制物,因此,为了能够安全地进行镀覆处理作业,需严格管理作业环境。
因此,需要提供一种镀金浴,该镀金浴即使不额外添加氰化合物也能够防止镀浴的分解,提高稳定性。
发明内容
本发明的目的在于,提供一种无需添加氰化合物的化学镀金液,具有稳定、低析出风险的优点,从而延长镀金浴的寿命。
本发明是通过以下技术方案实现的:
一种化学镀金液,包括以下组分:
金离子源 0.1-5g/L(以金浓度计),
络合剂 5-200 g/L,
金离子还原剂 1-50 g/L,
稳定剂 0.01-100mg/L;
络合剂至少同时包含2种及以上不同的络合剂;
pH值范围是4-9;
稳定剂的结构式为
其中,式(1)中,R1、R2、R3、R4分别独立地选自氢或取代的C1-C12烷基或未取代的C1-C12烷基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基;并且R1、R2、R3、R4中不超过2个基团选自氢;R5选自氢、羧基、醛基、磺酸基、硝基、氰基、异硫氰酰基、氧基、甲氧基、环氧丙基氧基、苯基、苄酰氧基、膦氧基、取代的胺基或未取代的胺基、取代的C1-C12烷基或未取代的C1-C12烷基,所述胺基的取代基是C1-C4烷基或羟基取代的C1-C4烷基或C1-C4酰基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基或氰基;R1、R2、R3、R4中不超过2个基团选自氢;
式(2)中,R6、R7、R8、R9 分别独立地选自氢或取代的C1-C12烷基或未取代的C1-C12烷基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基;R10选自氢、羧基、醛基、磺酸基、硝基、氰基、异硫氰酰基、氧基、甲氧基、环氧丙基氧基、苯基、苄酰氧基、膦氧基、取代的胺基或未取代的胺基、取代的C1-C12烷基或未取代的C1-C12烷基,所述胺基的取代基是C1-C4烷基或羟基取代的C1-C4烷基或C1-C4酰基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基或氰基;R6、R7、R8、R9中不超过2个基团选自氢。
优选的,稳定剂的含量为优选0.1-50mg/L,更优选0.5-10mg/L。
具体的,式(1)可以选自4-(2,2,6,6-四甲基-1-氧基-4-哌啶基)丁醇(CAS:88932-81-4)、1-氧基-2,2,6,6-四甲基-4-(β-氨乙基)哌啶二氯化物(CAS:74102-35-5)、2-(2,2,6,6-四甲基-1-氧基-4-哌啶基)乙醛(CAS:88932-83-6)、4-[N-(2-羟乙基)-N-甲基氨基]-2,2,6,6-四甲基哌啶氧基(CAS:42013-74-1)、
2,2,6,6-四甲基哌啶-1-氧基(CAS:2564-83-2)、4-羧基-2,2,6,6-四甲基哌啶-1-氧基(CAS:37149-18-1)、4-乙酰氨基-2,2,6,6-四甲基哌啶-1-氧基(CAS:14691-89-5)、4-环氧丙基氧-2,2,6,6-四甲基哌啶1-氧基(CAS:122413-85-8)、4-氰基-2,2,6,6-四甲基哌啶1-氧基(CAS:38078-71-6)、4-异硫氰酰基-2,2,6,6-四甲基哌啶1-氧基自由基(CAS:36410-81-8)、4-苄酰氧基-四甲基哌啶氧自由基(CAS:3225-26-1)、4-膦氧基-2,2,6,6-四甲基哌啶1-氧基(CAS:22690-04-6)、4-氧-2,2,6,6-四甲基哌啶-1-氧基(CAS:2896-70-0)、4-甲氧基-2,2,6,6-四甲基哌啶1-氧基(CAS:95407-69-5)、4-氨基-2,2,6,6-四甲基哌啶1-氧基(CAS:14691-88-4)等。
具体的,式(2)可以选自2,2-二丁基-5,5-二甲基吡咯烷-1-氧基(CAS:127898-70-8)、3-羧基-2,2,5,5-四甲基吡咯烷-1-氧基(CAS:2154-68-9)、3-(氨基甲基)-2,2,5,5-四甲基吡咯烷-1-氧基(CAS:54606-49-4)、2,2-二甲基-5-甲基吡咯烷-1-氧基(CAS 40936-05-8)、2,2-二甲基-5-乙基吡咯烷-1-氧基(CAS 40936-09-2)等。
所述的金离子源选自水溶性含氰金盐、水溶性非氰金盐中的至少一种;水溶性含氰金盐选自氰化亚金钾、氰化亚金钠、氰化亚金铵、四氰合金酸钾、四氰合金酸钠、四氰合金酸铵中的至少一种;水溶性非氰金盐选自亚硫酸金钾、亚硫酸金钠、亚硫酸金铵、硫代硫酸金钠、硫代硫酸金钾、硫代硫酸金铵、氯金酸钠、氯金酸钾、氯金酸铵、二氯金酸钠、二氯金酸钾、二氯金酸铵、硫氰酸金钠、硫氰酸金钾、硫氰酸金铵、硫代苹果酸金钠、硫代苹果酸金钾、硫代苹果酸金铵、柠檬酸金钾、柠檬酸金钠、柠檬酸金铵中的至少一种。
络合剂选自含氮羧酸类络合剂、脂肪羧酸或其盐类络合剂、硫代硫酸盐类络合剂、有机胺络合剂中的至少一种;
所述的含氮羧酸类络合剂选自乙二胺四乙酸或其盐、羟乙基乙二胺三乙酸或其盐、二羟乙基乙二胺二乙酸或其盐、丙二胺四乙酸或其盐、二亚乙基三胺五乙酸或其盐、三亚乙基四胺六乙酸或其盐、甘氨酸或其盐、甘氨酰-甘氨酸或其盐、甘氨酰-甘氨酰-甘氨酸或其盐、二羟乙基甘氨酸或其盐、亚氨基二乙酸或其盐、羟乙基亚氨基二乙酸或其盐、次氮基三乙酸或其盐、次氮基三丙酸或其盐中的至少一种;
所述的脂肪羧酸或其盐类络合剂选自柠檬酸或其盐、苹果酸或其盐、丙二酸或其盐、丁二酸或其盐、戊二酸或其盐、酒石酸或其盐、乙醇酸或其盐、乳酸葡萄糖酸或其盐、葡庚糖酸或其盐中的至少一种;
所述的硫代硫酸盐类络合剂选自硫代硫酸钠、硫代硫酸钾、硫代硫酸铵中的至少一种;
所述的有机胺络合剂选自甲胺、乙胺、丙胺、丁胺、乙二胺、丙二胺、1,3-丙二胺、丁二胺、己二胺、庚二胺、二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺、四羟基亚乙基二胺、单乙醇胺、双乙醇胺、三乙醇胺中的至少一种。
所述的金离子还原剂选自甲酸或其盐类还原剂、肼类还原剂、次亚磷酸盐还原剂、醛类还原剂、甲醛与有机胺的加成物类还原剂、亚硫酸根离子类还原剂、其它金离子还原剂中的至少一种。
甲酸或其盐类还原剂可以是甲酸的碱金属盐(如甲酸钾、甲酸钠等)、甲酸的碱土金属盐(甲酸镁、甲酸钙等)、甲酸的铵盐(一级-四级胺的胺盐)
肼类还原剂可以是碳酸肼、硫酸肼、硫酸二肼、盐酸肼等。
次/亚磷酸盐还原剂可以是次/亚磷酸钠、次/亚磷酸钾、次/亚磷酸铵等。
醛类还原剂可以是甲醛、乙醛、丙醛、正丁醛、o-甲基戊醛、β-甲基戊醛、γ-甲基戊醛或类似物的脂族饱和醛,如乙二醛、丁二醛或类似物的脂族双醛,如巴豆醛或类似物的脂族不饱和醛,如苯甲醛、邻硝基苯甲醛、间硝基苯甲醛、对硝基苯甲醛、邻甲基苯甲醛(o-tolaldehyde)、间甲基苯甲醛(m-tolaldehyde)、对甲基苯甲醛(p-tolaldehyde)、邻羟基苯甲醛、间羟基苯甲醛、对羟基苯甲醛、苯乙醛或类似物的芳香醛,或者具有醛基(-CHO)的糖类例如葡萄糖、半乳糖、甘露糖、核糖、麦芽糖、乳糖或类似物等。
甲醛与有机胺的加成物类还原剂可以是甲醛与亚硫酸氢盐加成化合物:可举出甲醛化亚硫酸氢钠、甲醛化亚硫酸氢钾、甲醛化亚硫酸氢铵等。
亚硫酸根离子类还原剂可以是任何水溶性亚硫酸盐或适用于将亚硫酸根离子释放到本发明无电镀镀金浴中的配位络合物。可选的,亚硫酸根离子源选自由以下组成的群组:亚硫酸碱,如亚硫酸锂、亚硫酸钠、亚硫酸钾、亚硫酸铵、亚硫酸等。
其它金离子还原剂可以是对苯二酚、抗坏血酸等。
本发明的化学镀金液的应用,用于镍钯金工艺、薄镍钯金工艺、钯金、镍金工艺中的至少一种。
化学镀镍钯金工艺:
(1)前处理
将基板按下述步骤进行处理:除油-水洗-微蚀-水洗-预浸-活化-水洗-沉镍-水洗-沉钯-水洗,其中的水洗是使用去离子水冲洗基板1分钟。
①除油:使用广东东硕科技有限公司产品TS-Acidclean 6189除油剂,操作温度为35℃,处理时间为5分钟。
②微蚀:微蚀剂由100g/L过硫酸钠和2%(v/v)浓硫酸组成,操作温度为30℃,处理时间是2分钟。
③预浸:采用1%硫酸处理,处理时间为2分钟。
④活化:使用广东东硕科技有限公司产品TS-Activator LA活化剂,操作温度为24℃,处理时间为1分钟。
⑤沉镍:沉镍使用广东东硕科技有限公司产品化学镀镍5183DMP系列药水,操作温度为82℃,处理时间为25分钟。
⑥沉钯:沉镍使用广东东硕科技有限公司产品化学钯5184P系列药水,操作温度为53℃,处理时间为15分钟。
(2)化学镀金
经过上述前处理后的基板浸入本发明的化学镀金液中,操作温度为65- 85℃,pH值为4-9,处理时间为10分钟。
化学镀金后,水洗吹干。
本发明具有如下有益效果:
针对目前还原型镀金浴普遍面临着药水稳定性差、金容易析出、金镀层厚度偏差较大这一问题,本发明向镀液中添加特定化学结构的稳定剂,该稳定剂具有捕获自由基、猝灭单线态氧和选择性氧化等功能。本发明利用该类分子结构具有强的吸电子效应,可以稳定镀金组合物,降低金离子析出的风险,从而延长镀液寿命,节约成本,而且能够明显提升镀金时金沉积的均一性。
具体实施方
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
本发明所用原料来源如下:
稳定剂:
稳定剂A:2,2-二丁基-5,5-二甲基吡咯烷-1-氧基(CAS:127898-70-8),市售;
稳定剂B:2-(2,2,6,6-四甲基-1-氧基-4-哌啶基)乙醛(CAS:88932-83-6),市售;
稳定剂C:4-[N-(2-羟乙基)-N-甲基氨基]-2,2,6,6-四甲基哌啶氧基(CAS:42013-74-1),市售;
稳定剂D:4-(2,2,6,6-四甲基-1-氧基-4-哌啶基)丁醇(CAS:88932-81-4),市售;
稳定剂E:1-氧基-2,2,6,6-四甲基-4-(β-氨乙基)哌啶二氯化物(CAS:74102-35-5),市售;
稳定剂F:4-羧基-2,2,6,6-四甲基哌啶-1-氧基(CAS:37149-18-1),市售;稳定剂G:4-膦氧基-2,2,6,6-四甲基哌啶1-氧基(CAS:22690-04-6),市售;
稳定剂H:3-(氨基甲基)-2,2,5,5-四甲基吡咯烷-1-氧基(CAS:54606-49-4),市售;
稳定剂I:2,2-二甲基-5-甲基吡咯烷-1-氧基(CAS 40936-05-8),市售;
稳定剂J:2,2-二甲基-5-乙基吡咯烷-1-氧基(CAS 40936-09-2),市售;
金离子源:氰化亚金钾、亚硫酸金钠来源于市售;
络合剂:柠檬酸、乙二胺四乙酸、甘氨酸、二亚乙基三胺五乙酸、次氮基三乙酸、乙二胺、羟乙基乙二胺三乙酸、三乙醇胺、苹果酸来源于市售;
还原剂:次磷酸钠、甲醛、硫酸肼、亚硫酸钠来源于市售。
pH调节剂:硫酸、氢氧化钾,市售。
各项测试方法:
(1)稳定性测试:分别取50mL的化学镀金液,在80℃水浴下持续加热,观察并记录槽液开始出现金单质沉淀的时间,对比各组合物的稳定性。
(2)金厚相对标准偏差(均一性)测试:
印制电路板规格是13.5cm*10cm,FR4材质的覆铜电路板,具有不同尺寸的焊盘(1.2mm×1.5mm ,1.5mm×1.5mm ,2mm×5mm, 3mm×3mm, 5mm×5mm, 7mm×7mm)。使用的设备为德国菲希尔FISCHERSCOPE X-RAY XDV-μ镀层测厚仪进行厚度测量。通过X射线荧光法(XRF)测量每块镀件化金10分钟后的不同尺寸焊盘的金层厚度,每个尺寸各测4个位置,共计24个测量位置,并计算所得24个数据的标准偏差和平均值。金厚相对标准偏差=标准偏差÷平均值×100%,数值越小,表示金厚均一性越好,反之则越差。
实施例和对比例化学镀金液的制备方法:先在适量纯水中加入络合剂,加入pH调整剂使pH接近目标pH值,搅拌使络合剂完全溶解后,再加入还原剂、金离子源、稳定剂混合均匀,再准确调节pH,最后定容后得到化学镀金液。
实施例1:氰化亚金钾5g/L(以金浓度计)、柠檬酸30g/L、乙二胺四乙酸10g/L、次磷酸钠15g/L、2,2-二丁基-5,5-二甲基吡咯烷-1-氧基100mg/L,pH=5.5。
实施例2:与实施例1的区别在于2,2-二丁基-5,5-二甲基吡咯烷-1-氧基浓度为0.01 mg/L,pH=5.5。
实施例3:与实施例1的区别在于2,2-二丁基-5,5-二甲基吡咯烷-1-氧基浓度为0.1 mg/L,pH=5.5。
实施例4:与实施例1的区别在于2,2-二丁基-5,5-二甲基吡咯烷-1-氧基浓度为0.5 mg/L,pH=5.5。
实施例5:与实施例1的区别在于2,2-二丁基-5,5-二甲基吡咯烷-1-氧基浓度为10mg/L,pH=5.5。
实施例6:与实施例1的区别在于2,2-二丁基-5,5-二甲基吡咯烷-1-氧基浓度为50mg/L,pH=5.5。
实施例7:亚硫酸金钠1g/L(以金浓度计)、甘氨酸20g/L、硫代硫酸钠5g/L、柠檬酸钠30g/L、亚硫酸钠10g/L 、2-(2,2,6,6-四甲基-1-氧基-4-哌啶基)乙醛10mg/L,pH=6.5。
实施例8:亚硫酸金钠2g/L(以金浓度计)、乙二胺四乙酸二钠15g/L、硫代硫酸钠5g/L、二乙烯三胺5g/L、亚硫酸钠50g/L、4-[N-(2-羟乙基)-N-甲基氨基]-2,2,6,6-四甲基哌啶氧基20mg/L,pH=7.5。
实施例9:氰化亚金钾0.1g/L(以金浓度计)、甘氨酸2g/L、二亚乙基三胺五乙酸3g/L、次磷酸钠1g/L、4-(2,2,6,6-四甲基-1-氧基-4-哌啶基)丁醇0.01mg/L,pH=4.0。
实施例10:氰化亚金钾5g/L(以金浓度计)、甘氨酸50g/L、三乙醇胺150g/L、甲醛50g/L、1-氧基-2,2,6,6-四甲基-4-(β-氨乙基)哌啶二氯化物100mg/L,pH=9.0
实施例11:氰化亚金钾2g/L(以金浓度计)、次氮基三乙酸15g/L、乙二胺30g/L、硫酸肼15g/L、4-羧基-2,2,6,6-四甲基哌啶-1-氧基5mg/L,pH=6.0。
实施例12:氰化亚金钾2g/L(以金浓度计)、苹果酸50g/L、羟乙基乙二胺三乙酸50g/L、次磷酸钠15g/L、4-膦氧基-2,2,6,6-四甲基哌啶1-氧基20mg/L,pH=4.0。
实施例13:氰化亚金钾3g/L(以金浓度计)、甘氨酸30g/L、乙二胺四乙酸20g/L、甲醛25g/L、3-(氨基甲基)-2,2,5,5-四甲基吡咯烷-1-氧基2mg/L、pH=7.5
实施例14:氰化亚金钾1g/L(以金浓度计)、甘氨酸30g/L、乙二胺20g/L、甲醛20g/L、2,2-二甲基-5-甲基吡咯烷-1-氧基1mg/L,pH=8.5。
实施例15::氰化亚金钾2g/L(以金浓度计)、苹果酸40g/L、乙二胺四乙酸20g/L、硫酸肼25g/L、2,2-二甲基-5-乙基吡咯烷-1-氧基10mg/L,pH=7.0。
对比例1:与实施例1相比,不含有稳定剂。
对比例2:与实施例2相比,不含有稳定剂。
对比例3:与实施例1相比,pH=3。
对比例4:与实施例1相比,pH=10。
表1:实施例和对比例测试结果
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | |
稳定性测试 | 加热72小时轻微金析出 | 加热72小时轻微析出 | 加热72小时轻微析出 | 加热72小时无金析出 | 加热72小时无析出 |
金厚相对标准偏差(%) | 5-7 | 5-7 | 4-6 | 3-5 | 3-5 |
续表1:
实施例6 | 实施例7 | 实施例8 | 实施例9 | 实施例10 | |
稳定性测试 | 加热72小时无金析出 | 加热72小时无金析出 | 加热72小时无金析出 | 加热72小时无金析出 | 加热72小时无金析出 |
金厚相对标准偏差(%) | 4-6 | 4-6 | 4-6 | 4-7 | 3-5 |
续表1:
实施例11 | 实施例12 | 实施例13 | 实施例14 | 实施例15 | |
稳定性测试 | 加热72小时无金析出 | 加热72小时无金析出 | 加热72小时无金析出 | 加热72小时无金析出 | 加热72小时无金析出 |
金厚相对标准偏差(%) | 4-6 | 4-6 | 3-6 | 4-6 | 4-6 |
续表1:
对比例1 | 对比例2 | 对比例3 | 对比例4 | |
稳定性测试 | 加热24小时有金析出 | 加热24小时有金析出 | 加热48小时有金析出 | 加热48小时有金析出 |
金厚相对标准偏差(%) | 15-20 | 15-20 | 10-15 | 10-15 |
由实施例与对比例可知,本发明的稳定剂不仅能够实现化学镀金液体系中金的稳定性,而且能够提升镀金时金沉积的均一性,实现镀件各部位金层厚度均一。
具体的,由实施例1-6可知,优选的稳定剂浓度范围内,镀金液稳定性更好、金层厚度更均一。
由对比例3/4可知,如pH值不在本发明范围内时,镀金液稳定性、金层厚度更均一都较差。
Claims (8)
1.一种化学镀金液,其特征在于,包括以下组分:
金离子源 0.1-5g/L,
络合剂 5-200 g/L,
金离子还原剂 1-50 g/L,
稳定剂 0.01-100mg/L;
络合剂至少同时包含2种及以上不同的络合剂;
pH值范围是4-9;
稳定剂的结构式为
其中,式(1)中,R1、R2、R3、R4分别独立地选自氢或取代的C1-C12烷基或未取代的C1-C12烷基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基;并且R1、R2、R3、R4中不超过2个基团选自氢;R5选自氢、羧基、醛基、磺酸基、硝基、氰基、异硫氰酰基、氧基、甲氧基、环氧丙基氧基、苯基、苄酰氧基、膦氧基、取代的胺基或未取代的胺基、取代的C1-C12烷基或未取代的C1-C12烷基,所述胺基的取代基是C1-C4烷基或羟基取代的C1-C4烷基或C1-C4酰基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基或氰基;R1、R2、R3、R4中不超过2个基团选自氢;
式(2)中,R6、R7、R8、R9 分别独立地选自氢或取代的C1-C12烷基或未取代的C1-C12烷基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基;R10选自氢、羧基、醛基、磺酸基、硝基、氰基、异硫氰酰基、氧基、甲氧基、环氧丙基氧基、苯基、苄酰氧基、膦氧基、取代的胺基或未取代的胺基、取代的C1-C12烷基或未取代的C1-C12烷基,所述胺基的取代基是C1-C4烷基或羟基取代的C1-C4烷基或C1-C4酰基,所述C1-C12烷基的取代基选自羟基、羧基、醛基、磺酸基、硝基、胺基、C1-C4烷氧基、C1-C4烷基取代的胺基或乙炔基或氰基;R6、R7、R8、R9中不超过2个基团选自氢。
2.根据权利要求1所述的化学镀金液,其特征在于,稳定剂的含量为优选0.1-50mg/L,更优选0.5-10mg/L。
3.根据权利要求1所述的化学镀金液,其特征在于,式(1)选自2,2,6,6-四甲基哌啶-1-氧基、4-羧基-2,2,6,6-四甲基哌啶-1-氧基、4-乙酰氨基-2,2,6,6-四甲基哌啶-1-氧基、4-环氧丙基氧-2,2,6,6-四甲基哌啶1-氧基、4-氰基-2,2,6,6-四甲基哌啶1-氧基、4-异硫氰酰基-2,2,6,6-四甲基哌啶1-氧基自由基、4-苄酰氧基-四甲基哌啶氧自由基、4-膦氧基-2,2,6,6-四甲基哌啶1-氧基、4-氧-2,2,6,6-四甲基哌啶-1-氧基、4-甲氧基-2,2,6,6-四甲基哌啶1-氧基、4-氨基-2,2,6,6-四甲基哌啶1-氧基、4-(2,2,6,6-四甲基-1-氧基-4-哌啶基)丁醇、2-(2,2,6,6-四甲基-1-氧基-4-哌啶基)乙醛、4-[N-(2-羟乙基)-N-甲基氨基]-2,2,6,6-四甲基哌啶氧基中的至少一种。
4.根据权利要求1所述的化学镀金液,其特征在于,式(2)选自2,2-二丁基-5,5-二甲基吡咯烷-1-氧基、3-羧基-2,2,5,5-四甲基吡咯烷-1-氧基、3-(氨基甲基)-2,2,5,5-四甲基吡咯烷-1-氧基、2,2-二甲基-5-甲基吡咯烷-1-氧基、2,2-二甲基-5-乙基吡咯烷-1-氧基中的至少一种。
5.根据权利要求1所述的化学镀金液,其特征在于,所述的金离子源选自水溶性含氰金盐、水溶性非氰金盐中的至少一种;水溶性含氰金盐选自氰化亚金钾、氰化亚金钠、氰化亚金铵、四氰合金酸钾、四氰合金酸钠、四氰合金酸铵中的至少一种;水溶性非氰金盐选自亚硫酸金钾、亚硫酸金钠、亚硫酸金铵、硫代硫酸金钠、硫代硫酸金钾、硫代硫酸金铵、氯金酸钠、氯金酸钾、氯金酸铵、二氯金酸钠、二氯金酸钾、二氯金酸铵、硫氰酸金钠、硫氰酸金钾、硫氰酸金铵、硫代苹果酸金钠、硫代苹果酸金钾、硫代苹果酸金铵、柠檬酸金钾、柠檬酸金钠、柠檬酸金铵中的至少一种。
6.根据权利要求1所述的化学镀金液,其特征在于,络合剂选自含氮羧酸类络合剂、脂肪羧酸或其盐类络合剂、硫代硫酸盐类络合剂、有机胺络合剂中的至少一种;
所述的含氮羧酸类络合剂选自乙二胺四乙酸或其盐、羟乙基乙二胺三乙酸或其盐、二羟乙基乙二胺二乙酸或其盐、丙二胺四乙酸或其盐、二亚乙基三胺五乙酸或其盐、三亚乙基四胺六乙酸或其盐、甘氨酸或其盐、甘氨酰-甘氨酸或其盐、甘氨酰-甘氨酰-甘氨酸或其盐、二羟乙基甘氨酸或其盐、亚氨基二乙酸或其盐、羟乙基亚氨基二乙酸或其盐、次氮基三乙酸或其盐、次氮基三丙酸或其盐中的至少一种;
所述的脂肪羧酸或其盐类络合剂选自柠檬酸或其盐、苹果酸或其盐、丙二酸或其盐、丁二酸或其盐、戊二酸或其盐、酒石酸或其盐、乙醇酸或其盐、乳酸葡萄糖酸或其盐、葡庚糖酸或其盐中的至少一种;
所述的硫代硫酸盐类络合剂选自硫代硫酸钠、硫代硫酸钾、硫代硫酸铵中的至少一种;
所述的有机胺络合剂选自甲胺、乙胺、丙胺、丁胺、乙二胺、丙二胺、1,3-丙二胺、丁二胺、己二胺、庚二胺、二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺、四羟基亚乙基二胺、单乙醇胺、双乙醇胺、三乙醇胺中的至少一种。
7.根据权利要求1所述的化学镀金液,其特征在于,所述的金离子还原剂选自甲酸或其盐类还原剂、肼类还原剂、次/亚磷酸盐还原剂、醛类还原剂、甲醛与有机胺的加成物类还原剂、亚硫酸根离子类还原剂、其它金离子还原剂中的至少一种。
8.权利要求1-7任一项所述的化学镀金液的应用,其特征在于,用于镍钯金工艺、薄镍钯金工艺、钯金工艺中的至少一种。
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