CN117051450A - Nickel plating solution and nickel plating method applied to electroplating processing - Google Patents
Nickel plating solution and nickel plating method applied to electroplating processing Download PDFInfo
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- CN117051450A CN117051450A CN202311030612.0A CN202311030612A CN117051450A CN 117051450 A CN117051450 A CN 117051450A CN 202311030612 A CN202311030612 A CN 202311030612A CN 117051450 A CN117051450 A CN 117051450A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 390
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 195
- 238000007747 plating Methods 0.000 title claims abstract description 143
- 238000009713 electroplating Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000012545 processing Methods 0.000 title claims abstract description 22
- 229930192627 Naphthoquinone Natural products 0.000 claims abstract description 27
- 150000002791 naphthoquinones Chemical class 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- RNFNDJAIBTYOQL-UHFFFAOYSA-N chloral hydrate Chemical compound OC(O)C(Cl)(Cl)Cl RNFNDJAIBTYOQL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229960002327 chloral hydrate Drugs 0.000 claims abstract description 15
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 238000005282 brightening Methods 0.000 claims abstract description 10
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 6
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- 239000000080 wetting agent Substances 0.000 claims abstract description 6
- 239000000872 buffer Substances 0.000 claims abstract description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 25
- 239000004848 polyfunctional curative Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- TZBXHAADXXYJPG-UHFFFAOYSA-N N1=CC=CC=C1.C(CC)S(=O)(=O)OO Chemical compound N1=CC=CC=C1.C(CC)S(=O)(=O)OO TZBXHAADXXYJPG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000011859 microparticle Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- WLCFKPHMRNPAFZ-UHFFFAOYSA-M didodecyl(dimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC WLCFKPHMRNPAFZ-UHFFFAOYSA-M 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- FRTIVUOKBXDGPD-UHFFFAOYSA-M sodium;3-sulfanylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCCS FRTIVUOKBXDGPD-UHFFFAOYSA-M 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 2
- 239000006172 buffering agent Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 63
- 238000000576 coating method Methods 0.000 abstract description 63
- 238000005260 corrosion Methods 0.000 abstract description 47
- 230000007797 corrosion Effects 0.000 abstract description 47
- 239000010410 layer Substances 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 16
- 230000004580 weight loss Effects 0.000 description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 229910052717 sulfur Inorganic materials 0.000 description 10
- 239000011593 sulfur Substances 0.000 description 10
- 239000000654 additive Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 239000003607 modifier Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 150000002989 phenols Chemical class 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007788 roughening Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GOLORTLGFDVFDW-UHFFFAOYSA-N 3-(1h-benzimidazol-2-yl)-7-(diethylamino)chromen-2-one Chemical compound C1=CC=C2NC(C3=CC4=CC=C(C=C4OC3=O)N(CC)CC)=NC2=C1 GOLORTLGFDVFDW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KHAZIIVSIJPRGF-UHFFFAOYSA-N [Na].CCCS Chemical compound [Na].CCCS KHAZIIVSIJPRGF-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- BPZADQUYEUZTAN-UHFFFAOYSA-N n,n-diethylprop-2-yn-1-amine;sulfuric acid Chemical compound OS(O)(=O)=O.CCN(CC)CC#C BPZADQUYEUZTAN-UHFFFAOYSA-N 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000006179 pH buffering agent Substances 0.000 description 1
- AZQWKYJCGOJGHM-UHFFFAOYSA-N para-benzoquinone Natural products O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- MRGUSFYIQDLKNZ-UHFFFAOYSA-M sodium;prop-1-yne-1-sulfonate Chemical compound [Na+].CC#CS([O-])(=O)=O MRGUSFYIQDLKNZ-UHFFFAOYSA-M 0.000 description 1
- LWLVRCRDPVJBKL-UHFFFAOYSA-M sodium;prop-2-ynoate Chemical compound [Na+].[O-]C(=O)C#C LWLVRCRDPVJBKL-UHFFFAOYSA-M 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- 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)
- Electroplating Methods And Accessories (AREA)
Abstract
The application relates to a nickel plating solution and a nickel plating method applied to electroplating processing in the field of electroplating processing, wherein the nickel plating solution comprises the following components in percentage by weight: 230g/L to 350g/L of nickel sulfate, 33g/L to 50g/L of nickel chloride, 8g/L to 12g/L of semi-gloss nickel potential difference regulator, 35g/L to 50g/L of buffer, 0.6g/L to 0.8g/L of brightening agent, 5g/L to 8g/L of semi-gloss nickel cylinder opener, 2g/L to 4g/L of wetting agent, 4g/L to 6g/L of hardening agent and the balance of ultrapure water; wherein the semi-gloss nickel potential difference regulator comprises naphthoquinone, aqueous organic solvent and chloral hydrate. The application can improve the potential difference between the semi-bright nickel coating and the bright nickel coating, thereby improving the corrosion resistance of the double coating.
Description
Technical Field
The application relates to the field of electroplating processing, in particular to a nickel plating solution and a nickel plating method applied to the electroplating processing.
Background
A process of plating a metal or some non-metal with nickel by electrolytic or chemical means is called nickel plating. Nickel plating is divided into electroplating nickel and chemical nickel plating. The nickel electroplating is to deposit a uniform and compact nickel coating on a cathode (plated piece) by direct current in an electrolyte composed of nickel salt (called as main salt), conductive salt, PH buffer and wetting agent.
Dark nickel is obtained in the nickel plating solution without the addition of the brightening agent, bright nickel is obtained from the nickel plating solution with the addition of the brightening agent, and semi-bright nickel is obtained from the nickel plating solution with the addition of the semi-bright nickel additive. The semi-bright nickel is a bottom layer, needs to have better corrosion resistance, is used as a decorative coating, and is commonly used on the semi-bright nickel coating to increase the decorative performance and corrosion resistance. The semi-gloss nickel additive generally comprises coumarin, butynediol and other additives with good leveling capability, and the semi-gloss nickel additive does not contain sulfur or has very low sulfur content, so that the formed semi-gloss nickel coating also does not contain sulfur or has very low sulfur content.
The semi-bright nickel plating layer has no sulfur or very low sulfur content, and the potential of the semi-bright nickel plating layer is positive, and the potential of the bright nickel plating layer obtained by bright nickel containing sulfur is negative, so that a certain potential difference exists between the semi-bright nickel plating layer and the bright nickel plating layer, and the corrosion resistance of the double plating layer can be improved to a certain extent. However, the potential difference between the semi-gloss nickel coating and the bright nickel coating obtained by adding the nickel plating solution of the semi-gloss nickel additive is still small and unstable, and the corrosion resistance is also poor.
Disclosure of Invention
In order to improve the potential difference between the semi-bright nickel coating and the bright nickel coating and further improve the corrosion resistance of the double coating, the application provides a nickel plating solution and a nickel plating method applied to electroplating processing.
The application provides a nickel plating solution applied to electroplating processing, which adopts the following technical scheme:
the nickel plating solution for electroplating comprises the following components in percentage by weight:
230g/L to 350g/L of nickel sulfate, 33g/L to 50g/L of nickel chloride, 8g/L to 12g/L of semi-gloss nickel potential difference regulator, 35g/L to 50g/L of buffer, 0.6g/L to 0.8g/L of brightening agent, 5g/L to 8g/L of semi-gloss nickel cylinder opener, 2g/L to 4g/L of wetting agent, 4g/L to 6g/L of hardening agent and the balance of ultrapure water;
wherein the semi-gloss nickel potential difference regulator comprises naphthoquinone, aqueous organic solvent and chloral hydrate.
By adopting the technical scheme, nickel ions in the nickel plating solution are provided by the nickel sulfate and nickel chloride. Nickel chloride is a source of chloride ions that ensures that the anode is in an activated state and dissolves normally to raise and maintain the current density in the nickel plating solution to maintain the potential of the semi-gloss nickel coating formed at the cathode. The method can improve the dispersion degree of the naphthoquinone in the nickel plating solution by using the aqueous organic solvent, wherein the naphthoquinone is used as a quinone compound, and carbonyl contained in the naphthoquinone is an active center of oxidation-reduction reaction, so that the method has good electrochemical reaction activity. The naphthoquinone has stronger oxidizing property, and the obtained hydrogen atoms are reduced into phenols, so that the naphthoquinone accelerates electron transfer through self oxidation-reduction reaction, and increases cathode polarization. Because the metal with positive potential is a cathode and the metal with negative potential is an anode in electroplating, the naphthoquinone increases cathode polarization in the electroplating process, so that the potential correction degree of the semi-gloss nickel coating is increased, the potential difference between the semi-gloss nickel coating and a bright nickel coating formed on the semi-gloss nickel coating later is further increased, the corrosion direction is further developed from longitudinal direction to transverse direction, and the corrosion resistance of the double coating is further improved. The chloral hydrate can remove active sulfur in the nickel plating solution, stabilize the potential difference of the nickel plating solution, and is matched with naphthoquinone to improve and stabilize the potential of the semi-gloss nickel plating layer. Because the naphthoquinone can be combined with hydrogen atoms to be reduced into phenols, the naphthoquinone can also reduce the permeated hydrogen in the semi-gloss nickel coating so as to reduce the escape or diffusion of the permeated hydrogen and lead the semi-gloss nickel coating to shrink or expand, so that the semi-gloss nickel coating generates compressive stress or tensile stress, the possibility of stress corrosion of the semi-gloss nickel coating is reduced, and the corrosion resistance of the double coating is further improved.
The brightening agent is used for removing greasy dirt, oxide, impurities and the like which stay on the surface of the formed coating, and keeping the coating clean, glossiness and the like. The buffer is used for keeping the pH value of the nickel plating solution stable so as to reduce the possibility of blackening and roughening a plating layer and having larger brittleness caused by unstable pH value of the nickel plating solution. The semi-gloss nickel cylinder opening agent has good filling property, ductility and dispersion performance, has leveling and dispersion effects on a coating, has extremely low sulfur content, and can promote and stabilize potential difference.
Optionally, the mass ratio of naphthoquinone, aqueous organic solvent and chloral hydrate is 1: (1-1.2): (0.7-0.9).
By adopting the technical scheme, the proportions of the naphthoquinone, the aqueous organic solvent and the chloral hydrate are compared according to the mass ratio, so that the potential of the semi-gloss nickel coating can be better improved and stabilized by the matched use of the naphthoquinone, the chloral hydrate and the naphthoquinone, and the potential difference between the semi-gloss nickel coating and the bright nickel coating can be improved.
Optionally, the hardener comprises SiC particles and MoS in a mass ratio of 9:1 2 Microparticles.
By adopting the technical scheme, the button is pressedThe mass ratio of the two particles is added into the nickel plating solution to form Ni-SiC-MoS 2 Composite plating solution, and forming Ni-SiC-MoS after electroplating 2 The composite coating is used for improving the hardness of the semi-gloss nickel coating and further improving the corrosion resistance of the coating. However, in general, the higher the hardness of the coating layer is, the higher the brittleness is, and the higher the possibility of inducing stress corrosion is, so that the content of the hardening agent needs to be strictly controlled within a certain range.
Optionally, the SiC particles and MoS 2 The purity of the particles is more than or equal to 99 percent, and the average particle diameter is 1.5-2.5 mu m.
By adopting the technical scheme, siC particles and MoS 2 The purity and particle size of the microparticles are such that Ni-SiC-MoS is formed 2 The composite coating is more compact, so that the improvement effect on the hardness of the semi-gloss nickel coating is better.
Optionally, the preparation method of the hardener comprises the following steps:
firstly, hydrochloric acid with volume fraction of 45% -55% is adopted to activate SiC particles and MoS 2 Cleaning SiC particles and MoS with a vacuum pump 2 And (3) mixing the particles until the particles are neutral, and drying to obtain the hardening agent.
By adopting the technical scheme, siC particles and MoS are removed through the corrosion of hydrochloric acid 2 Impurities and oxides on the surface of the particles increase the surface area and porosity, thereby improving the electrochemical activity.
Optionally, the buffer is selected from one of boric acid, ammonium salt, acetate and citrate.
By adopting the technical scheme, the PH value in the nickel plating solution influences the discharge potential of hydrogen, the precipitation of alkaline inclusion, the composition of complex or hydrate and the adsorption degree of additives, so the quality of the plating layer is greatly influenced. The weak acid and the weak acid salt reagent are added into the nickel plating solution, so that the acid in the salt can be gradually and practically used for keeping the pH value of the nickel plating solution, and the possibility of blackening and roughening a plating layer and high brittleness caused by unstable pH value of the nickel plating solution is reduced.
Optionally, the pH of the nickel plating solution is 3.8-4.6.
By adopting the technical scheme, the PH value range in the nickel plating solution can discharge potential of hydrogen and precipitate alkaline inclusion in the nickel plating solution, and also influence the composition of complex or hydrate and the adsorption degree of additives, so that the quality of the formed plating layer is better.
Optionally, the brightening agent comprises the following components in percentage by mass: (0.1-0.3): (0.2-0.5): (0.04-0.07) pyridinium hydroxy propane sulfonate, N-diethyl propargylamine sulfate, sodium propynylsulfonate, and sodium 3-mercaptopropane sulfonate.
By adopting the technical scheme, the content of free woolen and S032-, organic salt in the pyridinium hydroxy propane sulfonate is very small, so that abnormal phenomena such as blackening, roughness, more pinholes and the like of a plated part can be prevented, and the plated part has better leveling property; the N, N-diethyl propargylamine sulfate has better brightness and leveling property; the sodium propynylsulfonate has better brightness, leveling capability and impurity tolerance; the 3-mercaptopropane sodium sulfonate has better brightness and corrosion resistance, and the reagent is used according to the mass ratio, so that the brightness, flatness and corrosion resistance of a coating can be better improved.
Optionally, the wetting agent is at least one selected from didodecyl dimethyl ammonium chloride, polyoxyethylene alkylphenol ether and sodium dodecyl sulfate.
By adopting the technical scheme, the agent can reduce the interfacial tension between the surface tension nickel plating solution of the nickel plating solution and the plating piece, so that the nickel plating solution is easy to spread on the surface of the plating piece to improve the affinity state of the plating piece and the solution, and the flatness and uniformity of a plating layer formed by electroplating are improved.
In a second aspect, the application provides a nickel plating method of a nickel plating solution, which adopts the following technical scheme.
A nickel plating method of a nickel plating solution, comprising the steps of: the workpiece to be plated is placed as a cathode and a nickel plate as an anode in the nickel plating solution prepared according to claims 1-9 for electroplating, wherein the temperature of the nickel plating solution is 50-60 ℃ and the current density is 1-7A/square decimeter during the electroplating process.
By adopting the technical scheme, electroplating is carried out in the current sealing range and the temperature range, so that the potential difference between the semi-gloss nickel coating and the bright nickel layer can be improved and maintained while good appearance (namely better brightness) is obtained.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the naphthoquinone can increase cathode polarization through oxidation-reduction reaction of the naphthoquinone, so that the potential difference between the semi-gloss nickel coating and a bright nickel coating formed on the semi-gloss nickel coating is further increased, active sulfur in a nickel plating solution can be removed by chloral hydrate, the potential difference of the nickel plating solution is stabilized, chloral hydrate and naphthoquinone are used together to increase and stabilize the potential of the semi-gloss nickel coating, so that the potential difference between the semi-gloss nickel coating and the bright nickel coating is increased, the corrosion direction is further developed from longitudinal direction to transverse direction, and the corrosion resistance of the double-coating is further improved.
2. The naphthoquinone can be combined with hydrogen atoms to be reduced into phenols, so that the naphthoquinone can also reduce hydrogen permeated into the semi-gloss nickel coating so as to reduce the escape or diffusion of the permeated hydrogen and lead the semi-gloss nickel coating to shrink or expand, so that the possibility of compressive stress or tensile stress of the semi-gloss nickel coating is reduced, the possibility of stress corrosion of the semi-gloss nickel coating is reduced, and the corrosion resistance of the double coating is further improved;
3. the two particles are added into the nickel plating solution according to the mass ratio to form Ni-SiC-MoS 2 Composite plating solution, and forming Ni-SiC-MoS after electroplating 2 The composite coating is used for improving the hardness of the semi-gloss nickel coating and further improving the corrosion resistance of the coating.
Detailed Description
1. Examples
Example 1:
preparing 1L of nickel plating solution: 230g of nickel sulfate, 33g of nickel chloride, 8g of semi-gloss nickel potential difference regulator, 35g of boric acid, 0.6g of brightening agent, 5g of semi-gloss nickel cylinder opener, 2g of didodecyl dimethyl ammonium chloride and 5g of hardener are mixed and stirred, and then ultrapure water is added for constant volume to 1L. The pH of the nickel plating solution was 4.
Wherein the mass ratio of naphthoquinone, aqueous organic solvent and chloral hydrate in the semi-gloss nickel potential difference regulator is 1:1.1:0.8; wherein the semi-gloss nickel cylinder opening agent is ML-310 semi-gloss nickel cylinder opening agent; wherein the mass ratio of the pyridinium hydroxy propane sulfonate, the N, N-diethyl propiolate, the sodium propiolate and the sodium 3-mercaptopropane sulfonate in the brightening agent is 1:0.2:0.4:0.05.
the preparation method of the hardener comprises the following steps: firstly, hydrochloric acid with volume fraction of 50% is adopted to activate SiC particles and MoS 2 Cleaning SiC particles and MoS with a vacuum pump 2 And (5) drying the particles until the particles are neutral to obtain the hardening agent.
Electroplating a workpiece: and (3) placing the workpiece to be plated into the prepared nickel plating solution for electroplating, wherein the workpiece to be plated is 7cm multiplied by 2cm multiplied by 0.01cm in sample specification, and the workpiece to be plated is used as a cathode and the nickel plate is used as an anode, and in the electroplating process, the temperature of the nickel plating solution is 50 ℃, the current density is 4A/square decimeter, and the product A plated with the semi-gloss nickel plating layer is obtained by electroplating. And electroplating bright nickel on the product A to obtain a product B plated with double plating layers (semi-bright nickel plating layer and bright nickel plating layer).
Examples 2-3:
a nickel plating solution and a nickel plating method applied to plating processing are different from example 1 in that raw materials and their contents are shown in table 1.
TABLE 1 raw materials for examples 1-3 and parts by weight (g)
Example 4:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the content of the hardener is 4g/L.
Example 5:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the content of hardener was 6g/L.
Example 6:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the content of the semi-gloss nickel potential difference regulator is 8g/L.
Example 7:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the content of the semi-gloss nickel potential difference regulator is 12g/L.
Example 8:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the mass ratio of naphthoquinone, aqueous organic solvent and chloral hydrate in the semi-gloss nickel potential difference regulator is 1:1:0.7.
example 9:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the mass ratio of naphthoquinone, aqueous organic solvent and chloral hydrate in the semi-gloss nickel potential difference regulator is 1:1.2:0.9.
example 10:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the current density was 1A/square decimeter.
Example 11:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the current density was 7A/square decimeter.
2. Comparative example
Comparative example 1:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the semi-gloss nickel potential difference regulator is replaced with ultrapure water in equal quantity.
Comparative example 2:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the current density was 9A/square decimeter.
Comparative example 3:
a nickel plating solution and a nickel plating method applied to plating processing, which are different from example 2 in that: the content of the hardener is 8g/L.
3. Performance test
1) Potential difference test: the products B obtained in examples 1 to 11 and comparative examples 1 to 3 were passed through, respectivelyThe CMSSTEP multilayer nickel tester tests the potential difference between the semi-gloss nickel coating and the bright nickel coating.
2) Corrosion resistance test: the products B obtained in examples 1 to 11 and comparative examples 1 to 3 were placed in test chambers at a temperature of 35℃and a relative humidity of 85%, respectively, and sprayed continuously with a 5% NaCl solution by mass for 300 hours. Washing the electroplated product with a cleaning agent and distilled water before placing, then washing with wine, drying and weighing Wo. After 300 hours of continuous placement, the electroplated product is taken out, firstly washed under running water (if red rust appears on the surface, corrosion products are gently removed by a sharp-mouth camera), washed and dried, and then weighed for W1; wo-W1 is the corrosion weight loss.
3) Hardness testing: the products B obtained in examples 1 to 11 and comparative examples 1 to 3 were each tested for microhardness of the plating layer using a type HV-50 microhardness tester, with a load of 0.1kg for 10 seconds.
The above performance test results are shown in table 2:
table 2:
4. results and analysis
As can be seen from a combination of examples 1-11 and comparative examples 1-3 and Table 2, in examples 1-3, the inter-plating potential difference of example 2 was significantly higher than that of example 1, the weight loss on corrosion of example 2 was significantly lower than that of example 1, and the hardness of example 2 was higher than that of example 1, i.e., both the hardness and corrosion resistance of example 2 were superior to those of example 1. The inter-coating potential difference of example 3 was also significantly higher than that of example 2, but the corrosion weight loss quality of example 3 was slightly higher than that of example 2. This is because the hardness of example 3 is significantly higher than that of example 2, and when the hardness is higher, the brittleness of the plating layer is also increased, and the semi-gloss nickel plating layer is susceptible to stress corrosion, so that the inter-plating potential difference of example 3 is higher than that of example 2, but the corrosion resistance of example 3 is still lower than that of example 2.
From the above, the respective raw materials of example 2 and parts by weight thereof are compared with those of examples 1 and 3, and the hardness of the semi-gloss nickel plating layer is improved, and the corrosion resistance of the double plating layer obtained by electroplating is better, and the quality of the obtained electroplated product is better.
The hardener content of example 4 is lower than that of example 2, and the hardener content of example 5 is higher than that of example 2. As can be seen from Table 2, the potential differences of examples 4 to 5 are the same as those of example 2; example 4 has a lower hardness than example 2, and example 5 has a higher hardness than example 2; the corrosion weight loss mass of example 4 was the same as example 2, but that of example 5 was significantly higher than example 2. This is because, when the hardness is high, the brittleness of the plating layer also increases, and the semi-gloss nickel plating layer is liable to be subjected to stress corrosion.
And it is also known from comparative example 3 and Table 2 that too high a hardener content of comparative example 3 results in a much higher corrosion weight loss quality of comparative example 3 than that of example 2. According to the method, when the content of the hardener in the nickel plating solution is 5g/L, the semi-gloss nickel plating layer has better hardness and better corrosion resistance.
The amount of the semi-gloss nickel potential difference modifier in example 6 was lower than that in example 2, and the amount of the semi-gloss nickel potential difference modifier in example 7 was higher than that in example 2. As is clear from table 2, the potential difference of example 6 was lower than that of example 2, and the corrosion weight loss was higher than that of example 2; while example 7 has a potential difference and corrosion weight loss quality similar to example 2. From the above, the content of the semi-gloss nickel potential difference modifier in example 2 is compared with example 6, which can increase the inter-plating potential difference to increase the corrosion resistance, but the content of the semi-gloss nickel potential difference modifier in example 7 is not obvious compared with example 2.
And it can be seen from a combination of comparative example 1 and Table 2 that the semi-gloss nickel potential difference modifier in comparative example 1 was replaced with ultrapure water in equal amount, the potential difference in comparative example 1 was much lower than that in example 2, and the corrosion weight loss quality in comparative example 1 was much higher than that in example 2. The semi-gloss nickel potential difference regulator has an improvement effect on the potential difference between the semi-gloss nickel coating and the bright nickel coating, and can improve the corrosion resistance of the double coating; and when the content of the semi-gloss nickel potential difference regulator in the nickel plating solution is 10g/L, the double plating layer has better corrosion resistance on the premise of saving cost.
The mass ratios of naphthoquinone, aqueous organic solvent and chloral hydrate in the semi-gloss nickel potential difference modifiers of examples 8 to 9 were all different from those of example 2, and as can be seen from Table 2, the potential differences of examples 8 to 9 were lower than that of example 2, and the corrosion weight loss masses of examples 8 to 9 were higher than that of example 2. From the above, the mass ratio of naphthoquinone, aqueous organic solvent and chloral hydrate in the semi-gloss nickel potential difference regulator is 1:1.1: and when the corrosion resistance is 0.8, the potential difference between the semi-gloss nickel coating and the bright nickel coating is improved, and the corrosion resistance of the double coating is improved.
The current density of example 10 is lower than that of example 2, and the current density of example 11 is higher than that of example 2. As is clear from Table 2, the inter-plating potential difference in example 10 was lower than that in example 2, and the corrosion weight loss was higher than that in example 2; the inter-coating potential difference of example 11 was higher than that of example 2, but the corrosion weight loss mass of example 11 was lower than that of example 2. This is because the deposition rate of nickel ions on the workpiece to be plated is high due to the high current density, and the nickel plating solution is unstable due to the high deposition rate, so that the formation quality of the semi-gloss nickel plating layer is affected, and the corrosion resistance of the double plating layer is reduced.
Also, it can be seen in combination with comparative example 2 that when the current density is too high, the potential difference between the plating layers is increased, but the corrosion resistance of the double plating layers is adversely affected due to the excessively fast deposition rate of the semi-gloss nickel plating layer. From the above, when the current density is 4A/square decimeter, the half-gloss nickel coating obtained by electroplating can maintain a relatively fast and proper deposition rate, so that the electroplating efficiency is improved, and the corrosion resistance of the double coating is not negatively influenced.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (10)
1. The nickel plating solution for electroplating processing is characterized by comprising the following components in percentage by weight:
230g/L to 350g/L of nickel sulfate, 33g/L to 50g/L of nickel chloride, 8g/L to 12g/L of semi-gloss nickel potential difference regulator, 35g/L to 50g/L of buffer, 0.6g/L to 0.8g/L of brightening agent, 5g/L to 8g/L of semi-gloss nickel cylinder opener, 2g/L to 4g/L of wetting agent, 4g/L to 6g/L of hardening agent and the balance of ultrapure water;
wherein the semi-gloss nickel potential difference regulator comprises naphthoquinone, aqueous organic solvent and chloral hydrate.
2. The nickel plating solution for electroplating process according to claim 1, wherein: the mass ratio of the naphthoquinone to the aqueous organic solvent to the chloral hydrate is 1: (1-1.2): (0.7-0.9).
3. The nickel plating solution for electroplating process according to claim 1, wherein: the hardener comprises SiC particles and MoS in a mass ratio of 9:1 2 Microparticles.
4. A nickel plating solution for electroplating process according to claim 3, wherein: the SiC microparticles and MoS 2 The purity of the particles is more than or equal to 99 percent, and the average particle diameter is 1.5-2.5 mu m.
5. A nickel plating solution according to claim 3, wherein said hardening agent is prepared by the following steps:
firstly, hydrochloric acid with volume fraction of 45% -55% is adopted to activate SiC particles and MoS 2 Cleaning SiC particles and MoS with a vacuum pump 2 And (3) mixing the particles until the particles are neutral, and drying to obtain the hardening agent.
6. The nickel plating solution for electroplating process according to claim 1, wherein: the buffering agent is selected from one of boric acid, ammonium salt, acetate and citrate.
7. The nickel plating solution for electroplating process according to claim 1, wherein: the pH value of the nickel plating solution is 3.8-4.6.
8. The nickel plating solution for electroplating process according to claim 1, wherein: the brightening agent comprises the following components in percentage by mass: (0.1-0.3): (0.2-0.5): (0.04-0.07) pyridinium hydroxy propane sulfonate, N-diethyl propargylamine sulfate, sodium propynylsulfonate, and sodium 3-mercaptopropane sulfonate.
9. The nickel plating solution for electroplating process according to claim 1, wherein: the wetting agent is at least one selected from didodecyl dimethyl ammonium chloride, polyoxyethylene alkylphenol ether and sodium dodecyl sulfate.
10. The nickel plating method applied to electroplating processing is characterized by comprising the following steps of: the workpiece to be plated is placed as a cathode and a nickel plate as an anode in the nickel plating solution prepared according to claims 1-9 for electroplating, wherein the temperature of the nickel plating solution is 50-60 ℃ and the current density is 1-7A/square decimeter during the electroplating process.
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| CN118186383B (en) * | 2024-05-14 | 2024-07-12 | 广州传福化学技术有限公司 | Chemical nickel plating solution and nickel plating method thereof |
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