CN111850623A - Electroplating solution and electroplating process for obtaining suede nickel layer - Google Patents
Electroplating solution and electroplating process for obtaining suede nickel layer Download PDFInfo
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- CN111850623A CN111850623A CN202010381878.XA CN202010381878A CN111850623A CN 111850623 A CN111850623 A CN 111850623A CN 202010381878 A CN202010381878 A CN 202010381878A CN 111850623 A CN111850623 A CN 111850623A
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- electroplating
- dimethyl benzyl
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- chloride
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 53
- 238000009713 electroplating Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 10
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000002563 ionic surfactant Substances 0.000 claims abstract description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 10
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 7
- HPKFFZSXDWPVLX-UHFFFAOYSA-N 2-[(2-pyridin-1-ium-1-ylacetyl)amino]ethyl dodecanoate;chloride Chemical compound [Cl-].CCCCCCCCCCCC(=O)OCCNC(=O)C[N+]1=CC=CC=C1 HPKFFZSXDWPVLX-UHFFFAOYSA-N 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 3
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 claims description 2
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 claims description 2
- VZWMKHUMEIECPK-UHFFFAOYSA-M benzyl-dimethyl-octadecylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 VZWMKHUMEIECPK-UHFFFAOYSA-M 0.000 claims description 2
- CSNHNGDROQRZKT-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 CSNHNGDROQRZKT-UHFFFAOYSA-M 0.000 claims description 2
- OCBHHZMJRVXXQK-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 OCBHHZMJRVXXQK-UHFFFAOYSA-M 0.000 claims description 2
- DLNWMWYCSOQYSQ-UHFFFAOYSA-M benzyl-hexadecyl-dimethylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 DLNWMWYCSOQYSQ-UHFFFAOYSA-M 0.000 claims description 2
- SXPWTBGAZSPLHA-UHFFFAOYSA-M cetalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SXPWTBGAZSPLHA-UHFFFAOYSA-M 0.000 claims description 2
- 229960000228 cetalkonium chloride Drugs 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- SFVFIFLLYFPGHH-UHFFFAOYSA-M stearalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SFVFIFLLYFPGHH-UHFFFAOYSA-M 0.000 claims description 2
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 2
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 claims description 2
- -1 (p-isooctyl phenoxy ethoxy) (benzyl) (dimethyl) ammonium chloride Chemical compound 0.000 claims 2
- YOBWBLFILQYRFY-UHFFFAOYSA-N 2-hexadecylpyridine;hydrochloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCC1=CC=CC=[NH+]1 YOBWBLFILQYRFY-UHFFFAOYSA-N 0.000 claims 1
- MBTSFCHFGWXUGT-UHFFFAOYSA-M benzyl-butyl-dimethylazanium;bromide Chemical compound [Br-].CCCC[N+](C)(C)CC1=CC=CC=C1 MBTSFCHFGWXUGT-UHFFFAOYSA-M 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 abstract description 8
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 8
- 239000004327 boric acid Substances 0.000 abstract description 8
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract description 8
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 abstract description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 abstract 1
- 229940085605 saccharin sodium Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 238000007747 plating Methods 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- 239000002736 nonionic surfactant Substances 0.000 description 9
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000012224 working solution Substances 0.000 description 6
- 238000000635 electron micrograph Methods 0.000 description 5
- 239000003995 emulsifying agent Substances 0.000 description 5
- 239000011324 bead Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- VZRMFQSVPDJJHZ-UHFFFAOYSA-M benzyl-dimethyl-[2-[2-[4-(6-methylheptyl)phenoxy]ethoxy]ethyl]azanium;chloride Chemical compound [Cl-].C1=CC(CCCCCC(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 VZRMFQSVPDJJHZ-UHFFFAOYSA-M 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 206010027146 Melanoderma Diseases 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses an electroplating solution and an electroplating process for obtaining a suede nickel layer, and mainly relates to the field of metal decorative surface treatment. The electroplating solution comprises the following raw materials: 430-520 g/L of nickel sulfate; 30-50 g/L of nickel chloride; 30-50 g/L of boric acid; 2-5 g/L of saccharin sodium; 0.5-3 g/L of sodium allylsulfonate; 0.01-6 mg/L of polyethylene glycol type ionic surfactant; 0.5-10 mg/L of quaternary ammonium salt cationic surfactant, and the process comprises using the electroplating solution, wherein the treatment temperature is 48-55 ℃, the pH value is 3.9-4.5, and the cathode current density is 3.9-4.5A/dm2The stirring mode is cathode movement and cathode rotation, and the circulation filtration is not available. The invention has the beneficial effects that: different suede effects are obtained by adjusting the composition and content of the sanding agent, so that the requirements of different customers in the market on suede nickel are met.
Description
Technical Field
The invention relates to the field of metal decorative surface treatment, in particular to electroplating solution and an electroplating process for obtaining a suede nickel layer.
Background
The suede nickel is an important process in decorative surface treatment, has the characteristics of beautiful appearance, fine and soft color, low internal stress and good corrosion resistance, can be directly used as a protective decorative outer layer, and can also be coated with other metals such as chromium, gold, silver and the like to obtain more excellent protective decorative effects. At present, suede nickel is widely applied in the industries of automobile decoration, electronic products, daily hardware, cultural goods and the like.
The earliest textured nickel was produced by mechanical means, and the products obtained by this method were rough in surface, matt, and labor intensive, and were essentially eliminated. Currently, there are two general methods for obtaining textured nickel: a composite electrodeposition method and an emulsifier method. The composite electrodeposition method is that the dispersed phase comprising metal compound is added into the working liquid and suspended in the working liquid to form uneven nickel layer through co-deposition with nickel ion. The suede nickel surface formed by the technology has unsatisfactory glossiness, and the working solution is not easy to maintain and is limited in application. The emulsifier method is characterized in that a sanding emulsifier is introduced into the Watt nickel working solution, the sanding emulsifier generally consists of one or two nonionic surfactants, the nonionic surfactants have abnormal insolubility performance, the solubility of the nonionic surfactants is reduced along with the temperature rise, and when the temperature rises to a cloud point, the nonionic surfactants have association with water, ether bonds can be unhooked, and the solution is separated out to be turbid. When the diameter of the small liquid beads formed by precipitation reaches 5-30nm, the liquid beads are in a powered state, nickel ions do not deposit on the adsorbed small liquid beads during discharge deposition, and after the liquid beads are desorbed, tiny pits are formed at the original adsorption points, so that an uneven surface can be formed by repeating the steps. The synergistic effect of the nonionic surfactant and the cationic surfactant can obtain a more uniform and beautiful suede nickel layer. The micro surface of the suede nickel prepared by the method has countless overlapped pits, and shows a soft pearl effect on the macro scale.
The emulsifier method is generally adopted in the industry nowadays to obtain the required suede nickel. However, in the current commercial products, the sanding is unstable, and after 3-4 hours, the sand is disturbed, even black spots and bright spots appear on the surface, so that the stability of the matte effect cannot be realized, the activated carbon needs to be frequently added for filtration and adsorption, and then the adjustment is carried out again, so that the maintenance is extremely difficult, the stable and continuous production cannot be realized, the efficiency is low, the matte effect is single, and the appearance requirements of different customers on the matte nickel cannot be met. Therefore, the development of a long-acting matte nickel process which can obtain different matte effects by adjusting the composition of the working solution is urgently needed to meet the requirements of different customers.
Disclosure of Invention
The invention aims to provide an electroplating solution and an electroplating process for obtaining a nickel layer on a suede surface, which can obtain different suede surface effects by adjusting the composition and content of a sanding agent so as to meet the requirements of different customers on the nickel on the suede surface in the market.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an electroplating solution for obtaining a textured nickel layer comprises the following raw materials:
preferably, the raw materials comprise:
further preferably, the raw materials comprise:
n- { [ N- (2-lauroyloxyethyl) carbamoyl ] methyl } pyridinium chloride 9 mg/L.
The polyethylene glycol type ionic surfactant comprises one or more of polyethylene glycol, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty acid polyoxyethylene ether and fatty amine polyoxyethylene ether.
The polyethylene glycol type ionic surfactant is polyethylene glycol with the molecular weight of 5000-.
The quaternary ammonium salt cationic surfactant comprises dodecyl dimethyl benzyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium bromide, hexadecyl dimethyl benzyl ammonium chloride, hexadecyl dimethyl benzyl ammonium bromide, octadecyl dimethyl benzyl ammonium chloride, octadecyl dimethyl benzyl ammonium bromide, dodecyl trimethyl ammonium chloride and dodecyl trimethyl ammonium bromide, tetradecyltrimethylammonium chloride, tetradecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, hexadecyltrimethylammonium bromide, octadecyltrimethylammonium chloride, octadecyltrimethylammonium bromide, hexadecylpyridinium chloride, (p-isooctylphenoxyethoxyethyl) (benzyl) (dimethyl) ammonium chloride, N- { [ N- (2-lauroyloxyethyl) carbamoyl ] methyl } pyridinium chloride.
The quaternary ammonium salt cationic surfactant is dodecyl dimethyl benzyl ammonium chloride and N- { [ N- (2-lauroyloxyethyl) carbamoyl ] methyl } pyridinium chloride.
As another aspect of the present invention, an electroplating process using the above-mentioned electroplating solution, wherein the treatment temperature of the process is 48 to 55 ℃, the pH value is 3.9 to 4.5, and the cathode current density is 3.9 to 4.5A/dm2The stirring mode is cathode movement and cathode rotation, and the circulation filtration is not available.
The treatment temperature of the process is 52 ℃, the pH value is 4.0, and the cathode current density is 4A/dm2。
Compared with the prior art, the invention has the beneficial effects that:
nickel sulfate, nickel chloride and boric acid are added into the electroplating solution as basic components, wherein the nickel sulfate mainly provides nickel ions and conductive substances, the nickel chloride mainly promotes the dissolution of the anode, and the boric acid is added into the electroplating solution as a pH value buffering agent to stabilize the pH value of the working solution to 3.9-4.5.
Sodium saccharin and sodium allylsulfonate are used as additive components and added into the electroplating solution, wherein the sodium saccharin is mainly used as a softening agent to reduce the internal stress of nickel matte and improve the flexibility of the nickel matte, and the sodium allylsulfonate is used to ensure the nickel matte to be crystallized finely and to be more uniform and fine.
The polyethylene glycol type nonionic surfactant and the quaternary ammonium salt type cationic surfactant function as a sanding agent in the working fluid. The polyethylene glycol type nonionic surfactant and the quaternary ammonium salt type cationic surfactant with different molecular weights can be used independently to obtain the nickel layer with the required suede effect, and can also be used in a matched manner, the addition amount is adjusted to obtain the suede nickel layers with different appearance effects, and various production requirements are met.
Wherein, the polyethylene glycol type nonionic surfactant mainly has the function of enabling the nickel layer to obtain the round pit suede effect. The quaternary ammonium salt cationic surfactant has obvious sanding effect. The matte nickel process has the advantages that various matte nickel with different requirements can be prepared by selecting and compounding the polyethylene glycol type nonionic surfactant and the quaternary ammonium salt type cationic surfactant with different molecular weights and adjusting the composition and the proportion of the sanding agent, the process is simple to maintain, stable in color and luster, capable of continuously working for more than 15 days without any treatment, well meets production and application, and has great economic benefits.
Drawings
FIG. 1 is an electron micrograph of example 1 of the present invention.
FIG. 2 is an electron micrograph of example 2 of the present invention.
FIG. 3 is an electron micrograph of example 3 of the present invention.
FIG. 4 is an electron micrograph of example 4 of the present invention.
FIG. 5 is an electron micrograph of example 5 of the present invention.
FIG. 6 shows a test piece of the HULL cell of example 5 of the present invention.
FIG. 7 shows the thickness distribution of the nickel layer of the test piece of the HULL cell of example 5 of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
Example 1: electroplating solution and electroplating process for obtaining suede nickel layer
Taking 1L of the plating solution as an example, the plating solution comprises the following raw materials:
Nickel sulfate: 470 g/L;
nickel chloride: 40 g/L;
boric acid: 40 g/L;
sodium saccharin: 3.8 g/L;
sodium allyl sulfonate: 1.8 g/L;
0.05mg/L of polyethylene glycol 10000;
0.1mg/L of polyethylene glycol 15000;
cetyl trimethylammonium bromide: 1 mg/L.
The electroplating solution is used for nickel plating, and the technological parameters comprise:
treatment temperature: 52 ℃;
pH value: 4.0;
cathode current density: 4A/dm2；
Stirring mode: moving and rotating the cathode;
and (3) a filtering mode: and (4) filtering in a non-circulating way.
Example 2: electroplating solution and electroplating process for obtaining suede nickel layer
Taking 1L of the plating solution as an example, the plating solution comprises the following raw materials:
nickel sulfate: 470 g/L;
nickel chloride: 40 g/L;
boric acid: 40 g/L;
sodium saccharin: 3.8 g/L;
sodium allyl sulfonate: 1.8 g/L;
0.15mg/L of lauryl alcohol polyoxyethylene ether 10;
1.5mg/L of polyethylene glycol 15000;
dodecyl dimethyl benzyl ammonium chloride: 3 mg/L.
The electroplating solution is used for nickel plating, and the technological parameters comprise:
treatment temperature: 52 ℃;
pH value: 4.0;
cathode current density: 4A/dm2；
Stirring mode: moving and rotating the cathode;
and (3) a filtering mode: and (4) filtering in a non-circulating way.
Example 3: electroplating solution and electroplating process for obtaining suede nickel layer
Taking 1L of the plating solution as an example, the plating solution comprises the following raw materials:
nickel sulfate: 470 g/L;
nickel chloride: 40 g/L;
boric acid: 40 g/L;
sodium saccharin: 3.8 g/L;
sodium allyl sulfonate: 1.8 g/L;
dodecyl dimethyl benzyl ammonium chloride: 1 mg/L;
(p-isooctylphenoxyethoxyethyl) (benzyl) (dimethyl) ammonium chloride: 3 mg/L.
The electroplating solution is used for nickel plating, and the technological parameters comprise:
treatment temperature: 52 ℃;
pH value: 4.0;
cathode current density: 4A/dm2；
Stirring mode: moving and rotating the cathode;
and (3) a filtering mode: and (4) filtering in a non-circulating way.
Example 4: electroplating solution and electroplating process for obtaining suede nickel layer
Taking 1L of the plating solution as an example, the plating solution comprises the following raw materials:
nickel sulfate: 470 g/L;
nickel chloride: 40 g/L;
boric acid: 40 g/L;
sodium saccharin: 3.8 g/L;
sodium allyl sulfonate: 1.8 g/L;
0.2g/L of nonylphenol polyoxyethylene ether 15;
(p-isooctylphenoxyethoxyethyl) (benzyl) (dimethyl) ammonium chloride: 3 mg/L;
dodecyl trimethyl ammonium bromide: 9 mg/L.
The electroplating solution is used for nickel plating, and the technological parameters comprise:
treatment temperature: 52 ℃;
pH value: 4.0;
cathode current density: 4A/dm2；
Stirring mode: moving and rotating the cathode;
And (3) a filtering mode: and (4) filtering in a non-circulating way.
Example 5: electroplating solution and electroplating process for obtaining suede nickel layer
Taking 1L of the plating solution as an example, the plating solution comprises the following raw materials:
nickel sulfate: 470 g/L;
nickel chloride: 40 g/L;
boric acid: 40 g/L;
sodium saccharin: 3.8 g/L;
sodium allyl sulfonate: 1.8 g/L;
0.15mg/L of polyethylene glycol 10000;
1.5mg/L of polyethylene glycol 15000;
dodecyl dimethyl benzyl ammonium chloride: 3 mg/L;
n- { [ N- (2-lauroyloxyethyl) carbamoyl ] methyl } pyridinium chloride: 9 mg/L.
The electroplating solution is used for nickel plating, and the technological parameters comprise:
treatment temperature: 52 ℃;
pH value: 4.0;
cathode current density: 4A/dm2；
Stirring mode: moving and rotating the cathode;
and (3) a filtering mode: and (4) filtering in a non-circulating way.
Example 6: performance testing
The test pieces obtained by electroplating treatment using the electroplating solutions and processes described in examples 1 to 5 were tested as follows:
1. electron microscope detection SEM
The results of the square groove test conducted with reference to the process parameters of examples 1, 2, 3, 4 and 5 are shown in the following figures 1, 2, 3, 4 and 5, respectively, and the results of the SEM detection of the test pieces obtained by 300X and 500X times are shown in the figures.
As can be seen from FIGS. 1,2,3,4 and 5, different combinations of different contents of the sanding agent can make the surface of the nickel layer show different microscopic effects, and the surface has larger or smaller circular pits or is sparse or dense. By adjusting the composition and content of the sanding agent in the working solution, a nickel layer with a proper suede effect required by a customer can be obtained, and the customer requirements are met.
2. HULL cell experiment
Referring to the process of example 5, a HULL bath test was conducted and test pieces were subjected to an appearance test and a nickel layer thickness distribution test. The experimental results show that: from the high zone to the low zone, the test piece surface is fine and uniform, the appearance is soft, no bright spot or black spot exists, and the test piece effect is as shown in FIG. 6. The thickness distribution of the nickel layer is good, and the thickness of the nickel layer is reduced regularly along with the difference of current density, as shown in figure 7.
3. Test of Process stability
The combination of example 5 was compounded, and 10 test pieces of the continuous HULL cell were used to observe the change of nickel layer. The experimental results show that: the 10 th test piece has basically the same effect as the first suede, has no obvious difference, and has no bright spot and black spot on the nickel layer, and is uniform and fine.
The factory uses the embodiment 5 for production, does not need to carry out large treatment and readjust the working solution for more than 15 days, is stable and can carry out continuous production, improves the production efficiency and greatly reduces the cost.
Claims (9)
1. The electroplating solution for obtaining the matte nickel layer is characterized by comprising the following raw materials:
2. the electroplating bath for obtaining textured nickel layers as claimed in claim 1, wherein the raw materials comprise:
3. the electroplating bath for obtaining textured nickel layers as claimed in claim 1, wherein the raw materials comprise:
4. the electroplating solution for obtaining the textured nickel layer according to claim 1, wherein the polyethylene glycol type ionic surfactant comprises one or more of polyethylene glycol, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty acid polyoxyethylene ether and fatty amine polyoxyethylene ether.
5. The electroplating bath for obtaining Ni-textured layer as claimed in claim 4, wherein the PEG-type ionic surfactant is PEG with molecular weight of 5000-.
6. The electroplating bath for obtaining matte nickel layers according to claim 1, wherein the quaternary ammonium salt cationic surfactant comprises dodecyl dimethyl benzyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium bromide, hexadecyl dimethyl benzyl ammonium chloride, hexadecyl dimethyl benzyl ammonium bromide, octadecyl dimethyl benzyl ammonium chloride, octadecyl dimethyl benzyl ammonium bromide, dodecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium bromide, hexadecyl pyridine chloride, (p-isooctyl phenoxy ethoxy) (benzyl) (dimethyl) ammonium chloride, n-butyl dimethyl benzyl ammonium bromide, n-butyl dimethyl benzyl, One or more of N- { [ N- (2-lauroyloxyethyl) carbamoyl ] methyl } pyridinium chloride.
7. The electroplating bath for obtaining textured nickel layers according to claim 6, wherein the quaternary ammonium salt cationic surfactants are dodecyl dimethyl benzyl ammonium chloride and N- { [ N- (2-lauroyloxyethyl) carbamoyl ] methyl } pyridinium chloride.
8. Electroplating process, characterized in that the electroplating solution for obtaining the textured nickel layer according to any one of claims 1 to 8 is used, and the process has a treatment temperature of 48 to 55 ℃, a pH value of 3.9 to 4.5 and a cathodic current density of 3.9 to 4.5A/dm2The stirring mode is cathode movement and cathode rotation, and the circulation filtration is not available.
9. An electroplating process according to claim 8, wherein the process is carried out at a temperature of 52 ℃, a pH of 4.0 and a cathodic current density of 4A/dm2。
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Cited By (1)
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| WO2023164994A1 (en) * | 2022-03-01 | 2023-09-07 | 九牧厨卫股份有限公司 | Bactericidal environmentally friendly composite coating, preparation method therefor, and bactericidal environmentally friendly product |
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