CN116575019A - Method for electroless deposition of tin-nickel alloy on carrier-like plate - Google Patents
Method for electroless deposition of tin-nickel alloy on carrier-like plate Download PDFInfo
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- CN116575019A CN116575019A CN202310858178.9A CN202310858178A CN116575019A CN 116575019 A CN116575019 A CN 116575019A CN 202310858178 A CN202310858178 A CN 202310858178A CN 116575019 A CN116575019 A CN 116575019A
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- tin
- nickel alloy
- nickel
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- deposition
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- 229910000990 Ni alloy Inorganic materials 0.000 title claims abstract description 109
- CLDVQCMGOSGNIW-UHFFFAOYSA-N nickel tin Chemical group [Ni].[Sn] CLDVQCMGOSGNIW-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 230000008021 deposition Effects 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000000151 deposition Methods 0.000 claims abstract description 91
- 239000003814 drug Substances 0.000 claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 238000002791 soaking Methods 0.000 claims abstract description 18
- 150000002816 nickel compounds Chemical class 0.000 claims description 38
- 239000008139 complexing agent Substances 0.000 claims description 33
- 150000001875 compounds Chemical class 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000005282 brightening Methods 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 30
- 239000003638 chemical reducing agent Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 25
- 239000003381 stabilizer Substances 0.000 claims description 24
- 239000000080 wetting agent Substances 0.000 claims description 24
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 22
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 21
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 20
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 16
- XSUMSESCSPMNPN-UHFFFAOYSA-N propane-1-sulfonate;pyridin-1-ium Chemical group C1=CC=NC=C1.CCCS(O)(=O)=O XSUMSESCSPMNPN-UHFFFAOYSA-N 0.000 claims description 10
- -1 accelerator Substances 0.000 claims description 9
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 9
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 9
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 6
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical compound CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 claims description 6
- ROHFNLRQFUQHCH-UHFFFAOYSA-N Leucine Natural products CC(C)CC(N)C(O)=O ROHFNLRQFUQHCH-UHFFFAOYSA-N 0.000 claims description 6
- LXOFYPKXCSULTL-UHFFFAOYSA-N 2,4,7,9-tetramethyldec-5-yne-4,7-diol Chemical compound CC(C)CC(C)(O)C#CC(C)(O)CC(C)C LXOFYPKXCSULTL-UHFFFAOYSA-N 0.000 claims description 5
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 5
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 5
- 229930182817 methionine Natural products 0.000 claims description 5
- NACZPBOVCXPUJN-UHFFFAOYSA-N tris-decyl(methyl)azanium Chemical compound CCCCCCCCCC[N+](C)(CCCCCCCCCC)CCCCCCCCCC NACZPBOVCXPUJN-UHFFFAOYSA-N 0.000 claims description 5
- YXTDAZMTQFUZHK-ZVGUSBNCSA-L (2r,3r)-2,3-dihydroxybutanedioate;tin(2+) Chemical compound [Sn+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O YXTDAZMTQFUZHK-ZVGUSBNCSA-L 0.000 claims description 4
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 claims description 4
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 claims description 4
- VICYBMUVWHJEFT-UHFFFAOYSA-N dodecyltrimethylammonium ion Chemical compound CCCCCCCCCCCC[N+](C)(C)C VICYBMUVWHJEFT-UHFFFAOYSA-N 0.000 claims description 4
- KXUSQYGLNZFMTE-UHFFFAOYSA-N hex-2-yne-1,1-diol Chemical compound CCCC#CC(O)O KXUSQYGLNZFMTE-UHFFFAOYSA-N 0.000 claims description 4
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 4
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 4
- 229940081974 saccharin Drugs 0.000 claims description 4
- 235000019204 saccharin Nutrition 0.000 claims description 4
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 4
- 229940007163 stannous tartrate Drugs 0.000 claims description 4
- 239000004474 valine Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 106
- 239000010949 copper Substances 0.000 abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 19
- 229910052802 copper Inorganic materials 0.000 abstract description 17
- 230000007797 corrosion Effects 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 12
- 238000001556 precipitation Methods 0.000 abstract description 7
- 238000004381 surface treatment Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 41
- 238000005406 washing Methods 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 14
- 239000011148 porous material Substances 0.000 description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 7
- 238000005137 deposition process Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- 238000010992 reflux Methods 0.000 description 6
- 230000035939 shock Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000002950 deficient Effects 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002845 discoloration Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910001316 Ag alloy Inorganic materials 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 229910001297 Zn alloy Inorganic materials 0.000 description 2
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical compound [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- WDHWFGNRFMPTQS-UHFFFAOYSA-N cobalt tin Chemical compound [Co].[Sn] WDHWFGNRFMPTQS-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- JVPLOXQKFGYFMN-UHFFFAOYSA-N gold tin Chemical compound [Sn].[Au] JVPLOXQKFGYFMN-UHFFFAOYSA-N 0.000 description 2
- 239000003906 humectant Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 2
- 229910001174 tin-lead alloy Inorganic materials 0.000 description 2
- CGHIBGNXEGJPQZ-UHFFFAOYSA-N 1-hexyne Chemical compound CCCCC#C CGHIBGNXEGJPQZ-UHFFFAOYSA-N 0.000 description 1
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004846 x-ray emission Methods 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
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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)
Abstract
The invention discloses a method for electroless deposition of tin-nickel alloy on a carrier-like plate, and relates to the technical field of surface treatment of carrier-like plates. A method for electroless deposition of tin-nickel alloy on a carrier-like plate comprises the following steps: comprises a presoaking section and a depositing section; the pre-soaking section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the pre-soaking section are as follows: the temperature is 20-35 ℃ and the time is 2-12min; the deposition section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the deposition section are as follows: the temperature is 55-75deg.C, and the time is 25-45min. By the method, the similar carrier plate can achieve the effect of depositing the tin-nickel alloy on the copper base only through the pre-soaking section and the precipitation section, and the deposition effect is excellent; the deposited tin-nickel alloy has moderate thickness, compact structure, proper grain size, small internal stress and slow growth of tin whisker, can well inhibit the growth of tin whisker, and has the characteristics of brightness, wear resistance, corrosion resistance and the like.
Description
Technical Field
The invention relates to the technical field of carrier-like plate surface treatment, in particular to a method for electroless deposition of tin-nickel alloy on a carrier-like plate.
Background
In order to improve solderability of the carrier-like plate, it is often necessary to surface treat it. In the surface treatment process, the traditional hot air leveling process has the problems of poor surface leveling property, difficult fine pitch processing, easy occurrence of problems in solder paste printing, easy deformation of the plate at high temperature, easy environmental pollution caused by lead and the like.
For this, the solutions proposed are tin-gold deposition process, silver deposition process, tin deposition process, nickel-palladium-gold OSP, etc.; the tin-gold deposition process and the nickel-palladium-gold OSP process have high cost and difficult control and are limited to a certain extent; the silver deposition process has the problems of short storage period, incapability of welding for many times and the like; the pure tin layer has low cost, long storage period and easy control of the process, but has the problems of easy tin whisker generation, rough surface and the like. In addition, the existing tin precipitation liquid medicine contains thiourea, the thiourea is unstable and can decompose hydrogen sulfide gas, or thiourea residues can generate hydrogen sulfide gas under the high-temperature condition of reflux, and then black tin sulfide is generated with an oxide layer on the surface of a tin layer, so that the tin surface is blackened; meanwhile, thiourea is large in attack on solder resist ink, so that the problem that the ink falls off in the tin deposition process is extremely easy to cause defective products, the defective products need to be reworked, and even the defective products are directly disposed of when the scrapped plates are serious, so that the production cost is increased.
The pure tin layer does not contain lead, and although the pollution of lead to the environment is avoided, the pure tin layer is easier to generate tin whisker; tin whisker is a single tin crystal of an elongated shape that grows from the surface of the tin layer, which is a defect formed during deposition or is squeezed out of the substrate, and not remains on the surface of the tin; tin whisker will short circuit low voltage high resistance circuits, resulting in failure of the electrical device. Therefore, most military and aerospace devices disable pure tin plating.
For this reason, various solutions have been proposed, including reflow treatment, annealing treatment, using organic coating or other metal coating, using tin and its alloy layer, etc., which are in the subsequent treatment process, and using organic coating or other metal coating increases the manufacturing process and is too costly, so that the use of tin and its alloy layer is the focus of research.
Tin and its alloy layers are used including tin cobalt alloy layers, tin silver alloy layers, tin zinc alloy layers, and the like. Among these, tin-lead alloy layers can suppress the growth of tin whiskers better than other alloy layers, but in order to prevent contamination by lead, other solutions have been sought. The tin-cobalt alloy layer has small internal stress and can inhibit the growth of tin whisker, but has poor anti-discoloration and wear resistance; the tin-silver alloy layer is bright and compact, but the effect of inhibiting the growth of tin whisker is poor; the tin-zinc alloy layer has good corrosion resistance and brightness, but the effect of inhibiting the growth of tin whisker is poor.
Therefore, research on a surface treatment method of a carrier-like plate is urgently needed, a tin alloy layer is deposited on the carrier-like plate, the tin-lead alloy layer can be replaced, the growth of tin whisker is restrained, the cost is low, the storage period is long, the process is easy to control, meanwhile, the components do not contain thiourea, and the stability is good.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for electroless deposition of a tin-nickel alloy on a carrier-like plate, wherein the carrier-like plate can achieve the effect of depositing the tin-nickel alloy on a copper base only through a presoaking section and a precipitation section, and the deposition effect is excellent; the deposited tin-nickel alloy has moderate thickness, compact structure, proper grain size, small internal stress, slow tin whisker growth, good inhibition of tin whisker growth, bright, wear-resistant, corrosion-resistant and the like, and meanwhile, the thickness of the tin-nickel alloy deposited on the carrier-like plate is enough to ensure that the tin-nickel alloy still has the characteristics of bright, wear-resistant, corrosion-resistant and the like after being subjected to repeated reflux treatment. The method can reduce cost and is suitable for mass production.
In order to solve the problems, the invention provides the following technical scheme:
a method for electroless deposition of tin-nickel alloy on a carrier-like plate comprises the following steps:
comprises a presoaking section and a depositing section; the pre-soaking section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the pre-soaking section are as follows: the temperature is 20-35 ℃ and the time is 2-12min; the deposition section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the deposition section are as follows: the temperature is 55-75 ℃ and the time is 25-45min;
the electroless deposition tin-nickel alloy liquid medicine comprises the following components in percentage by mass:
3.0-8.0% of stannous compound; 9.0 to 25.0 percent of nickel compound; 15.0-40.0% of complexing agent; 2.0-8.0% of reducing agent; 2.0 to 6.0 percent of brightening agent; 2.0-6.0% of wetting agent; 2.0-8.0% of accelerator; 1.5 to 6.0 percent of stabilizer;
the stannous compound is one or a mixture of a plurality of stannous iso-octoate, stannous tartrate and stannous oxalate;
the nickel compound is one or a mixture of a plurality of nickel sulfate and nickel sulfamate;
the mass ratio of the stannous compound to the nickel compound is 1:3.5-5.5;
the complexing agent is a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, and the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 0.8-1.2:1;
the reducing agent is one or a mixture of more of leucine, valine and methionine;
the brightening agent is pyridinium propane sulfonate, and the mass ratio of the brightening agent to the wetting agent is 1:0.8-1.4.
Preferably, the mass ratio of the sum of the masses of the stannous compound and the nickel compound to the complexing agent is 0.8-1.5:1.
preferably, the mass ratio of the sum of the masses of the stannous compound and the nickel compound to the reducing agent is 3-6:1.
preferably, the humectant is one or more of hexynediol, saccharin, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, and mixtures thereof.
Preferably, the accelerator is one or a mixture of more of tridecyl methyl ammonium, dodecyl trimethyl ammonium and n-tetradecyl ammonium.
Preferably, the stabilizer is one or a mixture of hydroquinone and catechol.
Preferably, the concentration of the complexing agent is 15.0-35.0%.
Preferably, the concentration of the accelerator is 1.5-5.0%.
Preferably, the electroless tin-nickel alloy liquid medicine further comprises the balance of water.
Preferably, the electroless deposition tin-nickel alloy liquid medicine is prepared by stirring and mixing a stannous compound, a nickel compound, a complexing agent, a reducing agent, a brightening agent, a wetting agent, an accelerator, a stabilizer and the balance of water.
Advantageous effects
(1) The invention provides a method for electroless deposition of a tin-nickel alloy on a similar carrier plate, which can achieve the effect of depositing the tin-nickel alloy on a copper base only through a pre-soaking section and a precipitation section and has excellent deposition effect; the deposited tin-nickel alloy has moderate thickness, compact structure, proper grain size, small internal stress, slow tin whisker growth, good inhibition of tin whisker growth, bright, wear-resistant, corrosion-resistant and the like, and simultaneously, the thickness of the tin-nickel alloy deposited on the carrier plate is enough to enable the tin-nickel alloy to be subjected to multiple reflux treatment, the probability of tin whisker growth can be further reduced by the reflux treatment, and the tin-nickel alloy has the characteristics of bright, wear resistance, corrosion resistance and the like after the treatment. The method can reduce cost and is suitable for mass production.
(2) In the method, electroless deposition tin-nickel alloy liquid medicine is added into a presoaking section and a precipitation section, and the liquid medicine contains stannous compounds, nickel compounds, complexing agents, reducing agents, brightening agents, wetting agents, accelerators, stabilizing agents and other effective components. Wherein the stannous compound is reaction Sn 2+ +Cu→Sn+Cu 2+ Providing Sn element to enable tin to be deposited on copper; the nickel compound is reaction Ni 2+ +Cu→Ni+Cu 2+ Providing Ni element to enable nickel to be deposited on copper; the complexing agent and copper form a stable complex, the potential of the copper is reduced, the potential of the copper is negatively moved, the electron required by the replacement reaction is provided by the reducing agent, the reaction is pushed to move right, the replacement reaction can occur, and if any one of the complexing agent and the reducing agent is not added, the reaction cannot be performed; by adjusting the proportion of tin and nickel, the stress in the alloy layer is small, thereby inhibiting the growth of tin whisker, and simultaneously, the tin and nickel alloy layer has good corrosion resistance, wear resistance and discoloration resistance and stable structure. The wetting agent and the brightening agent cooperate to enable a tin precipitation peak to move right, the horizontal growth speed of a crystal nucleus is larger than the vertical growth speed, and the generation of tin whisker is inhibited to a certain extent; the promoter can reduce the resistivity of the solvent, and can improve the conductivity after being adsorbed on the copper surface through displacement reaction, thereby improving the deposition rate of the liquid medicine; the stabilizer can maintain the chemical properties between the componentsBalance, prevent light, thermal decomposition or oxidative decomposition, etc., thereby improving stability of the liquid medicine, and improving uniformity of alloy layer.
Drawings
In order to more clearly illustrate the technical solutions of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of a thermally shocked tin whisker test of a carrier-like plate treated with an electroless tin-nickel alloy of example 1;
fig. 2 is a microscopic schematic diagram of a thermally shocked tin whisker test of a carrier-like plate treated with the electroless tin-nickel alloy of comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
A method for electroless deposition of tin-nickel alloy on a carrier-like plate,
the method comprises the following steps:
comprises a presoaking section and a depositing section; the pre-soaking section adopts electroless deposition of tin-nickel alloy liquid medicine, and the technological parameters of the pre-soaking section are as follows: the temperature is 20-35 ℃ and the time is 2-12min; the deposition section adopts electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the deposition section are as follows: the temperature is 55-75deg.C, and the time is 25-45min.
The electroless deposition tin-nickel alloy liquid medicine comprises the following components in percentage by mass:
3.0-8.0% of stannous compound; 9.0 to 25.0 percent of nickel compound; 15.0-40.0% of complexing agent; 2.0-8.0% of reducing agent; 2.0 to 6.0 percent of brightening agent; 2.0-6.0% of wetting agent; 2.0-8.0% of accelerator; 1.5 to 6.0 percent of stabilizer;
the stannous compound is one or more of stannous isooctanoate, stannous tartrate and stannous oxalate; the nickel compound is one or a mixture of a plurality of nickel sulfate and nickel sulfamate; the mass ratio of the stannous compound to the nickel compound is 1:3.5-5.5;
the mass ratio of the stannous compound to the nickel compound is regulated, so that the proportion of tin and nickel in the tin-nickel alloy layer is regulated, and the tin-nickel alloy layer obtained by deposition has a stable and uniform structure and is bright light blue and black; the stress in the alloy layer is small, the growth of tin whisker can be inhibited, and meanwhile, the tin-nickel alloy layer has good corrosion resistance, wear resistance and discoloration resistance.
The complexing agent is a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate; preferably, the concentration of complexing agent is 15.0-35.0%. Dipotassium hydrogen phosphate and disodium hydrogen phosphate can be used as metal chelating agents for chelating copper ions, and meanwhile, phosphate chemical conversion films can be formed, so that the compactness and corrosion resistance of the tin-nickel alloy layer are enhanced; specifically, when the mass ratio of the tin-nickel alloy layer to the tin-nickel alloy layer is 0.8-1.2:1, the thickness and the corrosion resistance of the tin-nickel alloy layer are optimal.
Preferably, the mass ratio of the sum of the masses of the stannous compound and the nickel compound to the complexing agent is 0.8-1.5:1.
the reducing agent is one or more of leucine, valine and methionine; the mass ratio of the sum of the masses of the stannous compound and the nickel compound to the reducing agent is 3-6:1.
stannous Compound as reaction Sn 2+ +Cu→Sn+Cu 2+ Providing Sn element to enable tin to be deposited on copper; the nickel compound is reaction Ni 2+ +Cu→Ni+Cu 2+ Providing Ni element to enable nickel to be deposited on copper; the complexing agent and copper form a stable complex, the potential of the copper is reduced, the potential of the copper is shifted negatively, the electron required by the replacement reaction is provided by the reducing agent, the reaction is pushed to shift right, the replacement reaction can occur, if the complexing agent is not added, the reaction can not be performed, and if the reducing agent is not added, the reaction speed is low or even can not be performed.
The promoter is one or more of tridecyl methyl ammonium, dodecyl trimethyl ammonium and n-tetradecyl ammonium. Preferably, the concentration of the accelerator is 1.5-5.0%.
The promoter can reduce the resistivity of the solvent, and can improve the conductivity after being adsorbed on the copper surface through displacement reaction, thereby improving the deposition rate of the liquid medicine; the content of the accelerator is too low, and the deposition rate is slow; if the content of the accelerator is too low, the structure of the tin-nickel alloy layer can be influenced, so that the internal stress of the tin-nickel alloy layer is increased, and tin whisker can be produced more easily.
The brightening agent is pyridinium propane sulfonate, and the mass ratio of the brightening agent to the wetting agent is 1:0.8-1.4.
The wetting agent is one or more of hexyne glycol, saccharin, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol.
The wetting agent and the brightening agent cooperate to enable the tin precipitation peak to move right, the horizontal growth speed of the crystal nucleus is larger than the vertical growth speed, and the generation of tin whisker is inhibited to a certain extent.
The stabilizer is one or more of hydroquinone and catechol. The stabilizer can maintain chemical balance among the components, prevent the components from light, heat or oxidation decomposition, and the like, so that the stability of the liquid medicine can be improved, and meanwhile, the stabilizer has the effects of refining grains and improving the uniformity of an alloy layer.
The electroless tin-nickel alloy liquid medicine also comprises the balance of water.
The preparation method of the electroless deposition tin-nickel alloy liquid medicine comprises the following steps,
mixing stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and balance water.
Example 1, specifically:
sequentially weighing stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and the balance of water according to the following formula, adding into a reaction kettle, stirring and mixing for 30 minutes at normal temperature to obtain electroless deposition tin-nickel alloy liquid medicine, and sealing and storing the liquid medicine for later use.
Stannous compound 4.0%, specifically stannous iso-octoate;
22.0% of nickel compound, in particular nickel sulfate;
20.0% of complexing agent, specifically a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, wherein the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 1:1;
6.5% of a reducing agent, specifically leucine;
6.0% of brightening agent, specifically pyridinium propane sulfonate;
4.8% of a wetting agent, in particular hexynediol;
5.0% of a promoter, specifically tridecyl methyl ammonium;
4.0% of stabilizer, specifically hydroquinone;
the balance being water.
Example 2, specifically:
sequentially weighing stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and the balance of water according to the following formula, adding into a reaction kettle, stirring and mixing for 30 minutes at normal temperature to obtain electroless deposition tin-nickel alloy liquid medicine, and sealing and storing the liquid medicine for later use.
3.0% of stannous compound, specifically stannous tartrate;
10.5% of nickel compound, in particular nickel sulfamate;
16.0% of complexing agent, specifically a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, wherein the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 0.8:1;
4.5% of a reducing agent, specifically valine;
2.0% of brightening agent, specifically pyridinium propane sulfonate;
2.8% of a wetting agent, specifically saccharin;
2.0% of accelerator, specifically dodecyltrimethylammonium;
1.5% of stabilizer, specifically a mixture of catechol and hydroquinone, wherein the mass ratio of the catechol to the hydroquinone is 1:1;
the balance being water.
Example 3, specifically:
sequentially weighing stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and the balance of water according to the following formula, adding into a reaction kettle, stirring and mixing for 30 minutes at normal temperature to obtain electroless deposition tin-nickel alloy liquid medicine, and sealing and storing the liquid medicine for later use.
Stannous compound 5.0%, specifically stannous oxalate;
25.0% of nickel compound, in particular nickel sulfate;
30.0% of complexing agent, specifically a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, wherein the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 1.2:1;
5.0% of a reducing agent, specifically methionine;
5.0% of brightening agent, specifically pyridinium propane sulfonate;
a humectant 6.0%, specifically 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol;
8.0% of a promoter, specifically n-tetradecylammonium;
6.0% of stabilizer, specifically a mixture of catechol and hydroquinone, wherein the mass ratio of the catechol to the hydroquinone is 1:2;
the balance being water.
Example 4, specifically:
sequentially weighing stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and the balance of water according to the following formula, adding into a reaction kettle, stirring and mixing for 30 minutes at normal temperature to obtain electroless deposition tin-nickel alloy liquid medicine, and sealing and storing the liquid medicine for later use.
7.0% of stannous compound, specifically stannous oxalate;
24.5% of nickel compound, in particular nickel sulfate;
35.0% of complexing agent, specifically a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, wherein the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 1:1;
8.0% of a reducing agent, specifically methionine;
4.0% of brightening agent, specifically pyridinium propane sulfonate;
4.0% of a wetting agent, in particular 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol;
4.0% of a promoter, specifically n-tetradecylammonium;
3.0% of a stabilizer, specifically catechol;
the balance being water.
Example 5, specifically:
sequentially weighing stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and the balance of water according to the following formula, adding into a reaction kettle, stirring and mixing for 30 minutes at normal temperature to obtain electroless deposition tin-nickel alloy liquid medicine, and sealing and storing the liquid medicine for later use.
6.0% of stannous compound, specifically stannous oxalate;
24.0% of nickel compound, specifically nickel sulfate;
20.0% of complexing agent, specifically a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, wherein the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 1:1;
6.0% of a reducing agent, specifically leucine;
5.0% of brightening agent, specifically pyridinium propane sulfonate;
4.0% of a wetting agent, in particular hexynediol;
5.0% of a promoter, specifically tridecyl methyl ammonium;
4.0% of stabilizer, specifically hydroquinone;
the balance being water.
Meanwhile, the following comparative examples were set according to example 1, and the differences between the comparative examples and example 1 are shown in table 1 below.
Table 1 comparative example differs from example 1 in the table (/ mass fraction)
| Differences from example 1 | |
| Comparative example 1 | The only differences are: the composition being free of nickel compounds |
| Comparative example 2 | The only differences are: the content of nickel sulfate is 8.0% |
| Comparative example 3 | The only differences are: the content of nickel sulfate is 26.0% |
| Comparative example 4 | The only differences are: the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 0.6:1 |
| Comparative example 5 | The only differences are: the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 1.5:1 |
| Comparative example 6 | The only differences are: the content of the mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate is 12.0 percent |
| Comparative example 7 | The only differences are: dipotassium hydrogen phosphate and hydrogen phosphateThe content of the mixture of disodium is 42.0% |
| Comparative example 8 | The only differences are: the composition contains no reducing agent |
| Comparative example 9 | The only differences are: leucine content of 9.5% |
| Comparative example 10 | The only differences are: the composition does not contain brightening agent |
| Comparative example 11 | The only differences are: the content of pyridinium propane sulfonate is 1.5% |
| Comparative example 12 | The only differences are: the content of pyridinium propane sulfonate is 8.0% |
| Comparative example 13 | The only differences are: the content of hydroquinone is 8.5% |
In the above table, less than 100% of the water was made up.
Performance test
The invention discloses a method for electroless deposition of tin-nickel alloy on a carrier-like plate,
comprises a presoaking section and a depositing section; the pre-soaking section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the pre-soaking section are as follows: the temperature is 20-35 ℃ and the time is 2-12min; the deposition section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the deposition section are as follows: the temperature is 55-75 ℃ and the time is 25-45min;
the method for electroless deposition of the tin-nickel alloy on the carrier-like plate comprises the following steps: s1, oil removal; s2, washing with water, S3 microetching; s4, washing with water, and S5, presoaking; s6, depositing; s7, hot water washing; s8, drying;
the S1 degreasing section is used for degreasing the similar carrier plate, removing grease and oxides on the copper surface, cleaning the copper surface and increasing wettability, and the degreasing section comprises the following technological parameters: the length of the oil removing section is 2.0-m, the temperature is 30-40 ℃, and the linear speed is 0.5-1.0 m/min;
the S2 washing section is used for spraying and washing the similar carrier plates passing through the S1 oil removing section with DI water, and the technological parameters of the washing section are as follows: the temperature is 20-30 ℃, and the length of the water washing section is 2.0 m; the linear velocity is 1.0-2.0 m/min, and the pressure is 1.0-2.0 kg/cm 2 ；
The S3 microetching section microetches the similar carrier plate passing through the S2 water washing section, so that oxides on the copper surface are completely removed, and the technological parameters of the microetching section are as follows: the temperature is 25-30 ℃, and the length of the microetching section is 2.0 m; the linear velocity is 0.5-1.0 m/min, and the pressure is 1.0-2.0 kg/cm 2 ；
The S4 washing section is used for washing the similar carrier plate passing through the S3 microetching section by DI water, and the technological parameters of the washing section are as follows: the temperature is 20-30 ℃, and the length of the water washing section is 2.0 m; the linear velocity is 1.0-2.0 m/min, and the pressure is 1.0-2.0 kg/cm 2 ；
The S5 pre-soaking section pre-soaking the similar carrier plate passing through the S4 water washing section by using electroless deposition tin-nickel alloy liquid medicine, so that harmful and pollutant substances are reduced to be brought into a pre-soaking groove, the service life of the liquid medicine in the pre-soaking groove is prolonged, and the technological parameters of the pre-soaking section are as follows: the ratio of electroless deposition tin-nickel alloy liquid medicine in the presoaking groove is 100%, the temperature is 20-35 ℃, and the presoaking section length is 4.0 m; the linear speed is 0.5-2.0 m/min;
the S6 deposition section is to use electroless deposition tin-nickel alloy liquid medicine to perform tin-nickel deposition treatment on the similar carrier plate passing through the S5 presoaking section, and the technological parameters of the deposition section are as follows: the ratio of electroless deposition tin-nickel alloy liquid medicine in a deposition tank (tin-nickel deposition tank) is 100%, the temperature is 55-75 ℃, the deposition section length is 20m, and the linear speed is 0.4-0.8 m/min;
the S7 hot water washing section is used for washing the similar carrier plates passing through the S6 deposition section by hot DI water, and the process parameters of the hot water washing section are as follows: the temperature is 50-55 ℃, and the hot water washing section length is 2.0 m; the linear velocity is 1.0-2.0 m/min, and the pressure is 1.0-2.0 kg/cm 2 ；
The S8 drying section is used for drying the class carrier plate passing through the S7 hot water washing section, and the process parameters of the drying section are as follows: the temperature is 65-75 ℃, and the length of a drying washing section is 4.0 m; the linear velocity is 0.5-1.0 m/min.
The electroless tin-nickel alloy liquid medicine prepared in the examples and the comparative examples is used for operating the same batch of similar carrier plates by adopting the electroless tin-nickel alloy deposition method of the similar carrier plates to test the performance of the similar carrier plates prepared by the electroless tin-nickel alloy deposition method of the similar carrier plates, and the performance test results are shown in the following tables 2-4.
The performance of the electroless tin-nickel alloy liquid medicine is mainly expressed in three aspects: the first is to visually observe the appearance of the carrier-like plate; secondly, observing whether the surface of the carrier plate deposited with the tin-nickel alloy is flat or not by adopting a scanning electron microscope; thirdly, the thickness of the tin-nickel alloy is deposited, and the thickness is measured by an X-ray fluorescence spectrometry; fourthly, constant temperature tin whisker test, normal temperature storage (AS), 20-25 ℃,55+25%RH for 1000 hours, and then adopting a scanning electron microscope to observe a tin-nickel alloy layer of the similar carrier plate; and the fifth is to test the thermal shock tin whisker, the temperature impact test (TCT), the temperature of 55 ℃ (+/-5 ℃) to 125 ℃ (+/-5 ℃) and 1000 cycles, and then observe the tin-nickel alloy layer of the carrier-like plate by adopting a scanning electron microscope.
Table 2 results of performance tests of examples
| Appearance of carrier-like plate | Whether the deposited tin-nickel alloy surface is flat | Thickness of tin-nickel alloy deposited/mu m | Constant temperature tin whisker test | Thermal shock tin whisker test | |
| Example 1 | Bright bluish black | Leveling out | 1.25 | The surface is smooth, no tin whisker is generated | The surface is smooth, the pores are slightly formed, and no obvious tin whisker generation trace is generated |
| Example 2 | Bright bluish black | Leveling out | 1.12 | The surface is smooth, no tin whisker is generated | The surface is smooth, the pores are slightly formed, and no obvious tin whisker generation trace is generated |
| Example 3 | Bright bluish black | Leveling out | 1.30 | The surface is smooth, no tin whisker is generated | The surface is smooth, the pores are slightly formed, and no obvious tin whisker generation trace is generated |
| Example 4 | Bright bluish black | Leveling out | 1.34 | The surface is smooth, no tin whisker is generated | Smooth surface, slight pores and no brightnessShowing tin whisker formation trace |
| Example 5 | Bright bluish black | Leveling out | 1.27 | The surface is smooth, no tin whisker is generated | The surface is smooth, the pores are slightly formed, and no obvious tin whisker generation trace is generated |
TABLE 3 results of Performance measurements for comparative examples 1-7
| Appearance of carrier-like plate | Whether the deposited tin-nickel alloy surface is flat | Thickness of tin-nickel alloy deposited/mu m | Constant temperature tin whisker test | Thermal shock tin whisker test | |
| Comparative example 1 | Silvery white | Unevenness of the surface of the steel sheet | 1.53 | Uneven surface with obvious tin whisker formation | Uneven surface, pores and obvious tin whisker generation |
| Comparative example 2 | Bluish black | Unevenness of the surface of the steel sheet | 1.38 | Uneven surface and small amount of tin whisker | Uneven surface with voids and small amount of tin whisker |
| Comparative example 3 | Bright, deep blue-black | Leveling out | 1.13 | Uneven surface and small amount of tin whisker | Uneven surface with voids and small amount of tin whisker |
| Comparative example 4 | Bright bluish black | Leveling out | 1.22 | The surface is smooth, no tin whisker is generated | Uneven surface with voids and small amount of tin whisker |
| Comparative example 5 | Bright bluish black | Leveling out | 1.22 | The surface is smooth, no tin whisker is generated | Uneven surface with voids and small amount of tin whisker |
| Comparative example 6 | Bluish black | Unevenness of the surface of the steel sheet | 1.41 | Uneven surface and small amount of tin whisker | Uneven surface, pores and obvious tin whisker generation |
| Comparative example 7 | Bluish black | Unevenness of the surface of the steel sheet | 1.37 | Uneven surface and small amount of tin whisker | Uneven surface, pores and obvious tin whisker generation |
Table 4 results of Performance measurements of comparative examples 8 to 13
| Appearance of carrier-like plate | Whether the deposited tin-nickel alloy surface is flat | Thickness of tin-nickel alloy deposited/mu m | Constant temperature tin whisker test | Thermal shock tin whisker test | |
| Comparative example 8 | Surface tin-free nickel alloy | / | / | / | / |
| Comparative example 9 | Bright bluish black | Leveling out | 1.24 | The surface is smooth, no tin whisker is generated | The surface is smooth, the pores are slightly formed, and no obvious tin whisker generation trace is generated |
| Comparative example 10 | Bluish black | Unevenness of the surface of the steel sheet | 1.48 | Uneven surface and small amount of tin whisker | Uneven surface, pores and obvious tin whisker generation |
| Comparative example 11 | Bluish black | Unevenness of the surface of the steel sheet | 1.39 | Uneven surface and small amount of tin whisker | Uneven surface, pores and obvious tin whisker generation |
| Comparative example 12 | Bluish black | Unevenness of the surface of the steel sheet | 1.35 | Uneven surface and small amount of tin whisker | Uneven surface, pores and obvious tin whisker generation |
| Comparative example 13 | Bright, deep blue-black | Leveling out | 1.20 | Uneven surface and small amount of tin whisker | Uneven surface with voids and small amount of tin whisker |
As can be seen from the experimental data of examples 1-5 in Table 1, the electroless tin-nickel alloy deposition method for the carrier-like plate can deposit a bright tin-nickel alloy layer on the carrier-like plate, the thickness of the deposited tin-nickel alloy layer is 1.1-1.4 mu m, the deposition process requirements are met, and meanwhile, the tin-nickel alloy layer is compact, the grain size is moderate, the internal stress is small, and the generation of tin whiskers can be inhibited. Specifically, the microscopic schematic diagram (microscopic magnification 2000 times) of the thermal shock tin whisker test after the carrier-like plate is subjected to electroless tin-nickel alloy deposition treatment in example 1 is shown in fig. 1. The microscopic schematic diagram (microscopic magnification 2000 times) of the thermal shock tin whisker test after the similar carrier plate is subjected to electroless deposition tin-nickel alloy treatment in comparative example 1 is shown in fig. 2.
Comparative examples 1 to 3 differ from example 1 in whether or not the components contain nickel compounds; in the comparative example 1, no nickel compound is contained, so that only a pure tin layer is deposited on the carrier-like plate, the compactness of the pure tin layer is poor, and tin whisker is easy to appear after the tin whisker test; the nickel compound added in comparative examples 2-3 has higher nickel potential, slower electroless deposition rate and grain refinement, but the nickel compound added is too low, the tin-nickel alloy layer is uneven and the structure is loose; the addition of too high a nickel compound, too small a grain size, also results in easier tin whisker production.
In comparative examples 4 to 7, in the complexing agent, dipotassium hydrogen phosphate is increased, the tin-nickel alloy layer is thinned, and the compactness is enhanced, but excessive addition of dipotassium hydrogen phosphate can cause the tin-nickel alloy layer to be too thin, and the compactness is reduced; the disodium hydrogen phosphate is increased, the tin-nickel alloy layer is thinned, the crystal grains are reduced, and the compactness is enhanced, but the excessive addition of the disodium hydrogen phosphate can also cause the too thin tin-nickel alloy layer, the too small crystal grains and the compactness to be reduced. Therefore, the content of the complexing agent should not be too high, and the proportion of the complexing agent and the tin should be proper, otherwise, the tin-nickel alloy layer structure is poor, the compactness is insufficient, and the tin whisker is easier to generate.
In comparative examples 8-9, the reducing agent was used to provide electrons, if not added, which would result in no tin or nickel on the surface of the support-like plate; if the content is too high, the cost is increased, which is uneconomical.
In comparative examples 10 to 12, the brightening agent was used to brighten the surface of the tin-nickel alloy layer and at the same time, in cooperation with the wetting agent, to shift the heavy tin peak to the right, the horizontal growth rate of the crystal nuclei was greater than the vertical growth rate, and the generation of tin whiskers was suppressed to some extent. The horizontal growth speed of the crystal nucleus is lower than the vertical growth speed because no brightening agent is added or the brightening agent content is too low, so that the tin-nickel alloy layer is loose and tin whisker is easy to generate; and the added brightening agent is too much in content, so that the tin-nickel alloy layer is brittle and loose, and tin whisker is easy to generate.
In comparative example 13, too much stabilizer was added, which would make the crystal grains too small, resulting in easy generation of tin whisker.
In summary, the invention provides a method for electroless deposition of tin-nickel alloy on a carrier-like plate, which can achieve the effect of depositing tin-nickel alloy on a copper base by only a pre-soaking section and a depositing section, and has excellent deposition effect; the deposited tin-nickel alloy has moderate thickness, compact structure, proper grain size, small internal stress, slow tin whisker growth, good inhibition of tin whisker growth, bright, wear-resistant, corrosion-resistant and the like, and simultaneously, the thickness of the tin-nickel alloy deposited on the carrier plate is enough to enable the tin-nickel alloy to be subjected to multiple reflux treatment, the probability of tin whisker growth can be further reduced by the reflux treatment, and the tin-nickel alloy has the characteristics of bright, wear resistance, corrosion resistance and the like after the treatment. The method can reduce cost and is suitable for mass production.
In the foregoing embodiments, the descriptions of the embodiments are focused on, and for those portions of one embodiment that are not described in detail, reference may be made to the related descriptions of other embodiments.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The method for electroless deposition of the tin-nickel alloy on the carrier-like plate is characterized by comprising the following steps of:
comprises a presoaking section and a depositing section; the pre-soaking section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the pre-soaking section are as follows: the temperature is 20-35 ℃ and the time is 2-12min; the deposition section adopts the electroless deposition tin-nickel alloy liquid medicine, and the technological parameters of the deposition section are as follows: the temperature is 55-75 ℃ and the time is 25-45min;
the electroless deposition tin-nickel alloy liquid medicine comprises the following components in percentage by mass:
3.0-8.0% of stannous compound; 9.0 to 25.0 percent of nickel compound; 15.0-40.0% of complexing agent; 2.0-8.0% of reducing agent; 2.0 to 6.0 percent of brightening agent; 2.0-6.0% of wetting agent; 2.0-8.0% of accelerator; 1.5 to 6.0 percent of stabilizer;
the stannous compound is one or a mixture of a plurality of stannous iso-octoate, stannous tartrate and stannous oxalate;
the nickel compound is one or a mixture of a plurality of nickel sulfate and nickel sulfamate;
the mass ratio of the stannous compound to the nickel compound is 1:3.5-5.5;
the complexing agent is a mixture of dipotassium hydrogen phosphate and disodium hydrogen phosphate, and the mass ratio of the dipotassium hydrogen phosphate to the disodium hydrogen phosphate is 0.8-1.2:1;
the reducing agent is one or a mixture of more of leucine, valine and methionine;
the brightening agent is pyridinium propane sulfonate, and the mass ratio of the brightening agent to the wetting agent is 1:0.8-1.4.
2. The method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 1, wherein the mass ratio of the sum of stannous compound and nickel compound to complexing agent is 0.8-1.5:1.
3. the method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 2, wherein the mass ratio of the sum of stannous compound and nickel compound to the reducing agent is 3-6:1.
4. the method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 3, wherein the wetting agent is one or more of hexynediol, saccharin, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol.
5. The method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 4, wherein the accelerator is one or more of tridecyl methyl ammonium, dodecyl trimethyl ammonium, and n-tetradecyl ammonium.
6. The method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 5, wherein the stabilizer is one or more of hydroquinone and catechol.
7. The method for electroless deposition of tin-nickel alloy on a carrier-like substrate according to claim 6, wherein the complexing agent has a concentration of 15.0-35.0%.
8. The method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 7, wherein the accelerator has a concentration of 1.5-5.0%.
9. The carrier-like electroless tin-nickel alloy deposition method of claim 8, wherein the electroless tin-nickel alloy deposition bath further comprises a balance of water.
10. The method for electroless deposition of tin-nickel alloy on a carrier-like plate according to claim 9, wherein the preparation method of the electroless deposition tin-nickel alloy liquid medicine is that stannous compound, nickel compound, complexing agent, reducing agent, brightening agent, wetting agent, accelerator, stabilizer and the balance of water are stirred and mixed.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317596A (en) * | 2000-04-12 | 2001-10-17 | 林忠华 | Self-catalytic plating Ni-Sn-P alloy solution and its plated layer |
| JP2006144095A (en) * | 2004-11-24 | 2006-06-08 | Mitsubishi Paper Mills Ltd | Electroless plating method |
| CN114908342A (en) * | 2022-07-18 | 2022-08-16 | 深圳市板明科技股份有限公司 | Tin precipitation liquid medicine and circuit board tin precipitation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317596A (en) * | 2000-04-12 | 2001-10-17 | 林忠华 | Self-catalytic plating Ni-Sn-P alloy solution and its plated layer |
| JP2006144095A (en) * | 2004-11-24 | 2006-06-08 | Mitsubishi Paper Mills Ltd | Electroless plating method |
| CN114908342A (en) * | 2022-07-18 | 2022-08-16 | 深圳市板明科技股份有限公司 | Tin precipitation liquid medicine and circuit board tin precipitation method |
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