CN111663125A - Chemical palladium plating solution and preparation method and application thereof - Google Patents
Chemical palladium plating solution and preparation method and application thereof Download PDFInfo
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- CN111663125A CN111663125A CN202010735737.3A CN202010735737A CN111663125A CN 111663125 A CN111663125 A CN 111663125A CN 202010735737 A CN202010735737 A CN 202010735737A CN 111663125 A CN111663125 A CN 111663125A
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- plating solution
- palladium plating
- palladium
- solution according
- electroless palladium
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 238000007747 plating Methods 0.000 title claims abstract description 99
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 77
- 239000000126 substance Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000003381 stabilizer Substances 0.000 claims abstract description 29
- 239000008139 complexing agent Substances 0.000 claims abstract description 27
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 claims abstract description 19
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 18
- 150000002940 palladium Chemical class 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims description 22
- BRWIZMBXBAOCCF-UHFFFAOYSA-N hydrazinecarbothioamide Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 claims description 22
- MATPZHBYOVDBLI-FKNRSBSYSA-N 3-[(s)-amino(carboxy)methyl]cyclopropane-1,2-dicarboxylic acid Chemical compound OC(=O)[C@@H](N)C1C(C(O)=O)C1C(O)=O MATPZHBYOVDBLI-FKNRSBSYSA-N 0.000 claims description 18
- ZQZFXEBUKQSRPZ-UHFFFAOYSA-N 5-(2-aminoethyl)thiophene-2-sulfonamide Chemical compound NCCC1=CC=C(S(N)(=O)=O)S1 ZQZFXEBUKQSRPZ-UHFFFAOYSA-N 0.000 claims description 16
- 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 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 15
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 13
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea group Chemical group NC(=S)N UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 11
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229940124530 sulfonamide Drugs 0.000 claims description 6
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- 150000003456 sulfonamides Chemical class 0.000 claims description 4
- LMYRWZFENFIFIT-UHFFFAOYSA-N toluene-4-sulfonamide Chemical compound CC1=CC=C(S(N)(=O)=O)C=C1 LMYRWZFENFIFIT-UHFFFAOYSA-N 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- DNNXAUGMZQMSEI-UHFFFAOYSA-N 1,3-bis(ethenyl)thiourea Chemical compound C=CNC(=S)NC=C DNNXAUGMZQMSEI-UHFFFAOYSA-N 0.000 claims description 3
- BFKGCGPIFIWAKG-UHFFFAOYSA-N 1-(2-azaniumylethyl)cyclopropane-1-carboxylate Chemical compound NCCC1(C(O)=O)CC1 BFKGCGPIFIWAKG-UHFFFAOYSA-N 0.000 claims description 3
- ZPCQSJYTXRPREU-UHFFFAOYSA-N 1-azaniumyl-2-(hydroxymethyl)cyclopropane-1-carboxylate Chemical compound OC(=O)C1(N)CC1CO ZPCQSJYTXRPREU-UHFFFAOYSA-N 0.000 claims description 3
- MLTGAVXHWSDGIS-UHFFFAOYSA-N 4-ethylbenzenesulfonamide Chemical compound CCC1=CC=C(S(N)(=O)=O)C=C1 MLTGAVXHWSDGIS-UHFFFAOYSA-N 0.000 claims description 3
- KHBQMWCZKVMBLN-UHFFFAOYSA-N Benzenesulfonamide Chemical compound NS(=O)(=O)C1=CC=CC=C1 KHBQMWCZKVMBLN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 3
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-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
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 claims description 3
- AEPKDRAICDFPEY-UHFFFAOYSA-L palladium(2+);dinitrite Chemical compound [Pd+2].[O-]N=O.[O-]N=O AEPKDRAICDFPEY-UHFFFAOYSA-L 0.000 claims description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 3
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 3
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- LMJXSOYPAOSIPZ-UHFFFAOYSA-N 4-sulfanylbenzoic acid Chemical compound OC(=O)C1=CC=C(S)C=C1 LMJXSOYPAOSIPZ-UHFFFAOYSA-N 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 20
- 230000007797 corrosion Effects 0.000 abstract description 20
- 230000008021 deposition Effects 0.000 abstract description 9
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 47
- XSUMSESCSPMNPN-UHFFFAOYSA-N propane-1-sulfonate;pyridin-1-ium Chemical compound C1=CC=NC=C1.CCCS(O)(=O)=O XSUMSESCSPMNPN-UHFFFAOYSA-N 0.000 description 24
- JBTLOLAWFPERSC-UHFFFAOYSA-N 1-[4-(2-hydroxypropoxy)but-2-ynoxy]propan-2-ol Chemical compound CC(O)COCC#CCOCC(C)O JBTLOLAWFPERSC-UHFFFAOYSA-N 0.000 description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 description 20
- 125000003916 ethylene diamine group Chemical group 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- QMHIMXFNBOYPND-UHFFFAOYSA-N 4MTO Natural products CC1=CSC=N1 QMHIMXFNBOYPND-UHFFFAOYSA-N 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- -1 amine compound Chemical class 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000005711 Benzoic acid Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 235000010233 benzoic acid Nutrition 0.000 description 2
- PVTGORQEZYKPDK-UHFFFAOYSA-N ethenylthiourea Chemical compound NC(=S)NC=C PVTGORQEZYKPDK-UHFFFAOYSA-N 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005844 autocatalytic reaction Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- RLWFMZKPPHHHCB-UHFFFAOYSA-N cyclopropane-1,2-dicarboxylate;hydron Chemical compound OC(=O)C1CC1C(O)=O RLWFMZKPPHHHCB-UHFFFAOYSA-N 0.000 description 1
- MATPZHBYOVDBLI-JJYYJPOSSA-N dcg-iv Chemical compound OC(=O)[C@@H](N)C1[C@@H](C(O)=O)[C@@H]1C(O)=O MATPZHBYOVDBLI-JJYYJPOSSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 150000002941 palladium compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LDHXNOAOCJXPAH-UHFFFAOYSA-M sodium;prop-2-yne-1-sulfonate Chemical group [Na+].[O-]S(=O)(=O)CC#C LDHXNOAOCJXPAH-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention belongs to the technical field of surface treatment, and particularly relates to a chemical palladium plating solution, and a preparation method and application thereof. The invention provides a chemical palladium plating solution, which comprises 0.5-2g/L of palladium salt, 10-30g/L of complexing agent, 10-20mg/L of stabilizing agent, 2-6g/L of reducing agent and 5-10mg/L of sulfonyl substances according to concentration. The chemical palladium plating solution researched by the applicant has the advantages that all components are cooperated with each other to play a role together, the deposition rate is high, the plating layer is large in thickness, the plating layer is uniform and compact, and the plating solution is good in stability and corrosion resistant.
Description
Technical Field
The invention belongs to the technical field of surface treatment, and particularly relates to a chemical palladium plating solution, and a preparation method and application thereof.
Background
The technical performance of the nickel/palladium/gold coating is obtained by carrying out chemical nickel plating, chemical palladium plating and gold immersion treatment on the surfaces of the packaging carrier plate and other printed circuit board surfaces, and the coating has excellent weldability, linearity, smoothness, oxidation resistance, heat resistance, long-term reliability and the like. Palladium and gold have different deposition hardness and melting point, but both have excellent oxidation resistance and are stable in high-temperature and high-humidity atmosphere.
Electroless palladium and palladium alloys have evolved as a more economical alternative to electroless gold plating for certain applications. Electroless palladium plating is mainly used for a two-line type package circuit and other various hybrid circuits, and is particularly often used for a package substrate on which a semiconductor bump or a semiconductor is mounted, a mobile phone substrate, and the like. The main purpose of use is to improve the corrosion resistance, solder bondability, and wire weldability of the base metal material.
CN101228293 discloses an electroless palladium plating solution containing a water-soluble palladium compound, a complexing agent which is any one of ammonia, an amine compound, an aminocarboxylic acid compound, and a carboxylic acid, and a stabilizer which is bismuth or a bismuth compound, which is excellent in corrosion resistance and solder bondability and has excellent stability to the same extent as that of a conventional plating solution using a sulfur compound as a stabilizer. These systems use hydrazine baths and have the disadvantage that the plating rate drops sharply with the consumption of hydrazine in the bath.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides an electroless palladium plating solution, which comprises 0.5-2g/L of palladium salt, 10-30g/L of complexing agent, 10-20mg/L of stabilizing agent, 2-6g/L of reducing agent and 5-10mg/L of sulfonyl substances according to concentration.
In a preferred embodiment, the palladium salt is at least one selected from tetraamminepalladium sulfate, palladium sulfate hydrate, palladium chloride and palladium nitrite.
As a preferable technical solution, the reducing agent is at least one selected from sodium hypophosphite, sodium phosphite, sodium phosphate, sodium borohydride and trimethylamine.
As a preferred technical scheme, the stabilizing agent is selected from thiourea, thiosemicarbazide, vinyl thiourea, divinyl thiourea, KI and KIO3At least one of (1).
As a preferred technical scheme, the stabilizing agent is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (A) to (B) is 1-2: 1.
as a preferable technical scheme, the sulfonamide substance is at least one selected from p-toluenesulfonamide, benzenesulfonamide, p-ethylbenzene sulfonamide, 5- (2-aminoethyl) -2-thiophenesulfonamide and p-sulfonamide benzoic acid.
As a preferred embodiment, the complexing agent includes at least one of ammonia, ethylenediamine, propylenediamine, triethanolamine, diethanolamine, ethanolamine, glycine, tryptophan, phenylalanine, malic acid, citric acid, 1- (2-aminoethyl) -cyclopropanecarboxylic acid, 1-amino-2- (hydroxymethyl) cyclopropanecarboxylic acid, and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropanedicarboxylic acid.
As a preferable technical scheme, the electroless palladium plating solution also comprises 10-20mg/L of unsaturated compounds containing polar groups.
The second aspect of the invention provides a preparation method of the electroless palladium plating solution, which comprises the following steps: the components are mixed evenly.
The third aspect of the invention provides a use method of the chemical palladium plating solution, wherein the plating condition of the chemical palladium plating solution is 40-50 ℃, and the time is 10-25 min.
Has the advantages that: the chemical palladium plating solution researched by the applicant has the advantages that all components are cooperated with each other to play a role together, the deposition rate is high, the plating layer is large in thickness, the plating layer is uniform and compact, and the plating solution is good in stability and corrosion resistant.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the problems, the invention provides chemical palladium plating solution, which comprises 0.5-2g/L of palladium salt, 10-30g/L of complexing agent, 10-20mg/L of stabilizing agent, 2-6g/L of reducing agent and 5-10mg/L of sulfonyl substances according to concentration.
Preferably, the palladium salt is at least one selected from tetraamminepalladium sulfate, palladium sulfate hydrate, palladium chloride and palladium nitrite.
The reducing agent is selected from at least one of sodium hypophosphite, sodium phosphite, sodium phosphate, sodium borohydride and trimethylamine. The reducing agent provides electrons required for reduction of palladium ions, and different reducing agents can be selected according to different requirements, for example; the plating layer obtained by adopting sodium hypophosphite, sodium phosphite and sodium phosphate is Pd-P, trimethylamine and formic acid are adopted, and the formed plating layer is pure palladium; the reducing agent is sodium hypophosphite, so that the plating solution with low price is easy to control. When the content of the sodium hypophosphite is too high, the plating layer is uneven; when the content of sodium hypophosphite is too low, the deposition rate is too slow.
The stabilizer is selected from thiourea, thiosemicarbazide, vinylthiourea, divinyl thiourea, KI and KIO3At least one of (1). Preferably, the stabilizer is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (A) to (B) is 1-2: 1.
the sulfonamide substance is at least one selected from p-toluenesulfonamide, benzenesulfonamide, p-ethylbenzene sulfonamide, 5- (2-aminoethyl) -2-thiophene sulfonamide and p-sulfonamide benzoic acid.
Like the chemical nickel plating processChemical plating palladium is also a thermodynamically unstable system, and plating solution inevitably generates tiny particles with catalytic activity in the plating process, so that autocatalytic reaction is generated, and metal palladium in the plating solution is precipitated; the applicant finds that the stability of the plating solution can be improved by adding 20-30mg/L of thiourea, but the deposition speed of palladium is inhibited by 20-30mg/L of thiourea, and the plating solution with high stability cannot be obtained by reducing the amount of thiourea; the applicant has found that the addition of a certain amount of a sulfonamide and a stabilizer of thiosemicarbazide and KIO3，KIO3The surface adsorption degree is increased, so that the dynamic process of the oxidation-reduction reaction is influenced; the speed of the obtained palladium is moderate while the stability of the plating solution is improved. Particularly, when 5- (2-aminoethyl) -2-thiophenesulfonamide is used, the bath stability is 5MTO, and the plating rate is 0.16 μm/10 min.
The complexing agent comprises at least one of ammonia water, ethylenediamine, propylenediamine, triethanolamine, diethanolamine, ethanolamine, glycine, tryptophan, phenylalanine, malic acid, citric acid, 1- (2-aminoethyl) -cyclopropanecarboxylic acid, 1-amino-2- (hydroxymethyl) cyclopropanecarboxylic acid, and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropanedicarboxylic acid. The complexing agent is complexed with palladium ions through different complexing constants; thereby improving the concentration and performance of the plating layer and shortening the working time. In the present application, the complexing agent is ethylenediamine, ammonia water, and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropanedicarboxylic acid, and the concentration ratio of ethylenediamine, ammonia water, and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropanedicarboxylic acid is 2-4: 1: 0.5-1, the obtained plating layer is relatively flat and bright.
The 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropanedicarboxylic acid, CAS number 147782-19-2.
But KIO3The addition of the S-doped silicon dioxide reduces the corrosion resistance of the plating layer, the plating layer is dark, the crystallization is compact, the surface has cracks, and the doping of S reduces the corrosion resistance of the plating layer; the Applicant has also found, surprisingly, that the complexing agents are ethylenediamine, aqueous ammonia and 3- [ (S) -aminocarboxymethyl]When the 1, 2-cyclopropane dicarboxylic acid is used, the coating is placed in a nitric acid solution for 20 minutes without corrosion; presumably the thiosemicarbazide, 3- [ (S) -aminocarboxymethyl group]The components such as-1, 2-cyclopropane dicarboxylic acid are adsorbed on the surface of the substrate and interact with each otherThe Pd atoms grow and gather among the formed molecular morphologies by forming a certain molecular morphology.
The electroless palladium plating solution also comprises 10-20mg/L of unsaturated compounds containing polar groups; the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate to the butynediol propoxylate is 1-3: 1.
the pyridinium propane sulfonate and the butynediol propoxylate in a certain proportion are adsorbed in the concave and convex parts of the unevenness in a tendency way, so that palladium is arranged in the same crystal phase, the glossiness of a palladium plating layer is improved, and the thickness of the plating layer is increased.
The preparation method of the electroless palladium plating solution is a preparation method commonly used in the field, is not particularly limited, and can be realized by uniformly mixing all the components.
The plating condition of the chemical palladium plating solution is 40-50 ℃ and the time is 10-25 min.
The chemical palladium plating solution researched by the applicant has the advantages that all components are cooperated with each other to play a role together, the deposition rate is high, the plating layer is large in thickness, the plating layer is uniform and compact, and the plating solution is good in stability and corrosion resistant.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 16mg/L of unsaturated compounds containing polar groups according to concentration.
The stabilizer is thiosemicarbazide and KIO3Said amino groupThiourea and KIO3The concentration ratio of (1.5): 1.
the sulfonyl substances are 5- (2-aminoethyl) -2-thiophene sulfonamide, CAS number: 109213-13-0.
The complexing agent is ethylenediamine, ammonia water and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid, and the concentration ratio of the ethylenediamine to the ammonia water to the 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid is 3: 1: 0.8.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 2
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 0mg/L of sulfonyl substances and 16mg/L of unsaturated compounds containing polar groups according to concentration.
The stabilizer is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (1.5): 1.
the complexing agent is ethylenediamine, ammonia water and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid, and the concentration ratio of the ethylenediamine to the ammonia water to the 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid is 3: 1: 0.8.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 3
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 16mg/L of unsaturated compounds containing polar groups according to concentration.
The stabilizer is amino sulfurUrea and KIO3The thiosemicarbazide and KIO3The concentration ratio of (1.5): 1.
the sulfonyl substance is p-toluenesulfonamide.
The complexing agent is ethylenediamine, ammonia water and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid, and the concentration ratio of the ethylenediamine to the ammonia water to the 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid is 3: 1: 0.8.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 4
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 16mg/L of unsaturated compounds containing polar groups according to concentration.
The stabilizer is KIO3。
The sulfonyl substances are 5- (2-aminoethyl) -2-thiophene sulfonamide, CAS number: 109213-13-0.
The complexing agent is ethylenediamine, ammonia water and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid, and the concentration ratio of the ethylenediamine to the ammonia water to the 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid is 3: 1: 0.8.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 5
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 16mg/L of unsaturated compounds containing polar groups according to concentration.
The stabilizer is thiosemicarbazide.
The sulfonyl substances are 5- (2-aminoethyl) -2-thiophene sulfonamide, CAS number: 109213-13-0.
The complexing agent is ethylenediamine, ammonia water and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid, and the concentration ratio of the ethylenediamine to the ammonia water to the 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid is 3: 1: 0.8.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 6
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 10-20mg/L of unsaturated compounds containing polar groups.
The stabilizer is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (1.5): 1.
the sulfonyl substances are 5- (2-aminoethyl) -2-thiophene sulfonamide, CAS number: 109213-13-0.
The complexing agent is ethylenediamine and ammonia water, and the concentration ratio of ethylenediamine to ammonia water is 3: 1.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 7
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 10-20mg/L of unsaturated compounds containing polar groups.
The stabilizer is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (1.5): 1.
the sulfonyl substances are 5- (2-aminoethyl) -2-thiophene sulfonamide, CAS number: 109213-13-0.
The complexing agent is ethylenediamine, ammonia water and citric acid, and the concentration ratio of ethylenediamine to ammonia water to citric acid is 3: 1: 0.8.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 8
The chemical palladium plating solution comprises 1.2g/L of palladium tetraammine sulfate, 16g/L of complexing agent, 14mg/L of stabilizing agent, 4.8g/L of reducing agent sodium hypophosphite, 6.2mg/L of sulfonyl substances and 10-20mg/L of unsaturated compounds containing polar groups.
The stabilizer is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (1.5): 1.
the sulfonyl substances are 5- (2-aminoethyl) -2-thiophene sulfonamide, CAS number: 109213-13-0.
The complexing agent is ethylenediamine, ammonia water and 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid, and the concentration ratio of the ethylenediamine to the ammonia water to the 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropane dicarboxylic acid is 3: 1: 3.
the polar group-containing unsaturated compound comprises pyridinium propane sulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propane sulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 2: 1.
the chemical palladium plating solution is obtained by uniformly mixing the components.
Example 9
An electroless palladium plating solution, which is similar to example 1 in specific embodiment, is different in that the polar group-containing unsaturated compound includes pyridinium propanesulfonate and butynediol propoxylate, and the ratio of the concentrations of the pyridinium propanesulfonate (CAS number: 15471-17-7) and the butynediol propoxylate is 1: 2.
example 10
An electroless palladium plating solution, which is different from example 1 in the specific embodiment, is characterized in that the polar group-containing unsaturated compound includes pyridinium propanesulfonate and butynediol propoxylate, and the concentration ratio of the pyridinium propanesulfonate (CAS number: 15471-17-7) to the butynediol propoxylate is 5: 1.
example 11
An electroless palladium plating solution, the specific embodiment of which is the same as example 1, except that pyridinium propanesulfonate is replaced with sodium propargyl sulfonate.
Performance testing
And chemically plating palladium on the PCB plated with the nickel at the plating temperature of 50 ℃ for 15 min.
And (4) testing the stability of the plating solution: the circulation experiment was conducted on the PCB plated with palladium, and in the case of a plating solution having a plating palladium concentration of 1.2g/L, the plating solution was deposited with 1.2g/L of palladium on the PCB to give 1 MTO.
Plating speed test: and measuring the thickness of the plating layer at each 3 positions of the front surface and the back surface of the PCB, and dividing the average value by the plating time. The deposition rate was evaluated as excellent at more than 0.15 μm/10min (including 0.15), the deposition rate was evaluated as medium at 0.1 to 0.15 μm/10min (including 0.1), and the deposition rate was evaluated as poor at less than 0.1 μm/10 min.
And (3) testing the corrosion of the plating layer: the palladium-plated PCB was immersed in a 20 vol% nitric acid aqueous solution for 20 minutes, then washed with water, dried, and observed with a microscope.
The appearance of the plating layer: the morphology of the plating was visualized.
And (3) testing the thickness of the plating layer: measuring the thickness of the coating by using an intelligent electrolytic thickness gauge; the thickness was evaluated as excellent at more than 1.0 μm (including 1), the thickness was evaluated as poor at less than 0.7 μm in the range of 0.7 to 1.0 μm (including 0.7).
| Stability of | Plating speed | Corrosiveness of | Morphology of the coating | Thickness of coating | |
| Example 1 | 5MTO | Superior food | No corrosion | Bright, uniform and compact | Superior food |
| Example 2 | 2MTO | Superior food | Slight corrosion | Local brightness | Superior food |
| Example 3 | 4MTO | In | Slight corrosion | Bright, uniform and compact | In |
| Example 4 | 5MTO | Difference (D) | Severe corrosion of | Dull luster | In |
| Example 5 | 5MTO | In | Slight corrosion | Dull luster | In |
| Example 6 | 4MTO | In | Severe corrosion of | Local brightness | In |
| Example 7 | 4MTO | In | Slight corrosion | Local brightness | Superior food |
| Example 8 | 3MTO | In | Slight corrosion | Local brightness | Difference (D) |
| Example 9 | 5MTO | Superior food | No corrosion | Local brightness | In |
| Example 10 | 5MTO | Superior food | No corrosion | Bright, uniform and compact | In |
| Example 11 | 4MTO | Superior food | Slight corrosion | Local brightness | In |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. The chemical palladium plating solution is characterized by comprising 0.5-2g/L of palladium salt, 10-30g/L of complexing agent, 10-20mg/L of stabilizer, 2-6g/L of reducing agent and 5-10mg/L of sulfonyl substances according to concentration.
2. The electroless palladium plating solution according to claim 1, wherein the palladium salt is at least one selected from tetraamminepalladium sulfate, palladium sulfate hydrate, palladium chloride, and palladium nitrite.
3. The electroless palladium plating solution according to claim 1, wherein the reducing agent is at least one selected from the group consisting of sodium hypophosphite, sodium phosphite, sodium phosphate, sodium borohydride, and trimethylamine.
4. The electroless palladium plating solution according to claim 1, wherein the stabilizer is selected from thiourea, thiosemicarbazide, thiovinylthiourea, divinylthiourea, KI, KIO3At least one of (1).
5. The electroless palladium plating solution according to claim 4, wherein the stabilizer is thiosemicarbazide and KIO3The thiosemicarbazide and KIO3The concentration ratio of (A) to (B) is 1-2: 1.
6. the electroless palladium plating solution according to claim 1, wherein the sulfonamide substance is at least one selected from the group consisting of p-toluenesulfonamide, benzenesulfonamide, p-ethylbenzene sulfonamide, 5- (2-aminoethyl) -2-thiophenesulfonamide, and p-sulfanylbenzoic acid.
7. The electroless palladium plating solution according to claim 1, wherein the complexing agent comprises at least one of ammonia, ethylenediamine, propylenediamine, triethanolamine, diethanolamine, ethanolamine, glycine, tryptophan, phenylalanine, malic acid, citric acid, 1- (2-aminoethyl) -cyclopropanecarboxylic acid, 1-amino-2- (hydroxymethyl) cyclopropanecarboxylic acid, 3- [ (S) -aminocarboxymethyl ] -1, 2-cyclopropanedicarboxylic acid.
8. The electroless palladium plating solution according to any one of claims 1 to 7, further comprising 10 to 20mg/L of a polar group-containing unsaturated compound.
9. The method for preparing an electroless palladium plating solution according to any one of claims 1 to 8, comprising the steps of: the components are mixed evenly.
10. The use method of the electroless palladium plating solution according to any one of claims 1 to 8, wherein the electroless palladium plating solution is applied under the condition of 40 to 50 ℃ for 10 to 25 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112301334A (en) * | 2020-10-30 | 2021-02-02 | 吉安宏达秋科技有限公司 | Chemical palladium plating solution, application thereof and chemical palladium plating method |
| CN113005439A (en) * | 2021-02-24 | 2021-06-22 | 深圳市创智成功科技有限公司 | Chemical palladium plating process for electronic packaging carrier plate |
| CN113897603A (en) * | 2021-08-31 | 2022-01-07 | 信丰正天伟电子科技有限公司 | Corrosion-resistant palladium electroless plating solution and application thereof |
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2020
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112301334A (en) * | 2020-10-30 | 2021-02-02 | 吉安宏达秋科技有限公司 | Chemical palladium plating solution, application thereof and chemical palladium plating method |
| CN113005439A (en) * | 2021-02-24 | 2021-06-22 | 深圳市创智成功科技有限公司 | Chemical palladium plating process for electronic packaging carrier plate |
| CN113897603A (en) * | 2021-08-31 | 2022-01-07 | 信丰正天伟电子科技有限公司 | Corrosion-resistant palladium electroless plating solution and application thereof |
| CN113897603B (en) * | 2021-08-31 | 2023-09-05 | 信丰正天伟电子科技有限公司 | Corrosion-resistant palladium chemical plating solution and application thereof |
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