CN114808048B - Electroless nickel plating solution and plating process thereof - Google Patents
Electroless nickel plating solution and plating process thereof Download PDFInfo
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- CN114808048B CN114808048B CN202110598956.6A CN202110598956A CN114808048B CN 114808048 B CN114808048 B CN 114808048B CN 202110598956 A CN202110598956 A CN 202110598956A CN 114808048 B CN114808048 B CN 114808048B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 190
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 95
- 238000007747 plating Methods 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 35
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 57
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000009713 electroplating Methods 0.000 claims description 29
- 150000007524 organic acids Chemical class 0.000 claims description 20
- 239000004408 titanium dioxide Substances 0.000 claims description 20
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 19
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 19
- 239000001630 malic acid Substances 0.000 claims description 19
- 235000011090 malic acid Nutrition 0.000 claims description 19
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 15
- 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 15
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 15
- -1 alkyl phosphate Chemical compound 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003945 anionic surfactant Substances 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 239000003381 stabilizer Substances 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 7
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 6
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 4
- 150000002898 organic sulfur compounds Chemical class 0.000 claims description 4
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229910000085 borane Inorganic materials 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 45
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 8
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical group FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 6
- 239000013538 functional additive Substances 0.000 description 6
- 239000003607 modifier Substances 0.000 description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 5
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 4
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000005711 Benzoic acid Substances 0.000 description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 235000010233 benzoic acid Nutrition 0.000 description 2
- 238000005282 brightening Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000174 gluconic acid Substances 0.000 description 2
- 235000012208 gluconic acid Nutrition 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 229960004889 salicylic acid Drugs 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- QCQCHGYLTSGIGX-GHXANHINSA-N 4-[[(3ar,5ar,5br,7ar,9s,11ar,11br,13as)-5a,5b,8,8,11a-pentamethyl-3a-[(5-methylpyridine-3-carbonyl)amino]-2-oxo-1-propan-2-yl-4,5,6,7,7a,9,10,11,11b,12,13,13a-dodecahydro-3h-cyclopenta[a]chrysen-9-yl]oxy]-2,2-dimethyl-4-oxobutanoic acid Chemical compound N([C@@]12CC[C@@]3(C)[C@]4(C)CC[C@H]5C(C)(C)[C@@H](OC(=O)CC(C)(C)C(O)=O)CC[C@]5(C)[C@H]4CC[C@@H]3C1=C(C(C2)=O)C(C)C)C(=O)C1=CN=CC(C)=C1 QCQCHGYLTSGIGX-GHXANHINSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- AMNPXXIGUOKIPP-UHFFFAOYSA-N [4-(carbamothioylamino)phenyl]thiourea Chemical compound NC(=S)NC1=CC=C(NC(N)=S)C=C1 AMNPXXIGUOKIPP-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JIRRNZWTWJGJCT-UHFFFAOYSA-N carbamothioylthiourea Chemical compound NC(=S)NC(N)=S JIRRNZWTWJGJCT-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 description 1
- KBAFDSIZQYCDPK-UHFFFAOYSA-M sodium;octadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCS([O-])(=O)=O KBAFDSIZQYCDPK-UHFFFAOYSA-M 0.000 description 1
- AYFACLKQYVTXNS-UHFFFAOYSA-M sodium;tetradecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCS([O-])(=O)=O AYFACLKQYVTXNS-UHFFFAOYSA-M 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004846 x-ray emission 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
-
- 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)
- Chemically Coating (AREA)
Abstract
The invention discloses a chemical nickel plating solution and a plating process thereof. The invention improves the stability of the chemical nickel plating solution by the combined action of the components in the chemical nickel plating solution, so that the obtained plating layer shows good flatness, compactness and adhesiveness.
Description
Technical Field
The invention relates to the field of electroplating technology, in particular to electroless nickel plating solution and an electroplating technology thereof.
Background
Nickel plating is a key process in the pretreatment process of electroplating, and the quality of the performance of a nickel plating layer is directly related to whether the subsequent electroplating process can be successfully carried out or not and whether the performance of the finally obtained plated piece meets the requirement or not. Electroless nickel plating is one of the fast developing nickel plating processes and has also been studied extensively. The electroless nickel plating is to deposit free nickel ions on the surface of a substrate by applying an electric current to the nickel plating solution to form a smooth, corrosion-resistant and high-hardness nickel layer. However, the nature of the chemical nickel solution in the chemical nickel plating, particularly the stability of the chemical nickel solution, has great influence on the nickel plating process, and can reduce the compactness of the plating layer and the flatness of the plating layer. Based on the above, the invention provides an electroless nickel plating solution and a plating process thereof.
Disclosure of Invention
In a first aspect, the present invention provides an electroless nickel plating solution, comprising: nickel sulfate, nickel sulfamate, anionic surfactant, functional additive and deionized water.
Preferably, the anionic surfactant is at least one selected from alkyl sulfate, alkyl sulfonate, alkylphenol sulfate, and alkyl phosphate.
Preferably, the functional additive comprises at least one of a reducing agent, a stabilizing agent, an organic acid and a brightening agent.
Preferably, the functional additive further comprises titanium dioxide.
Preferably, the mass ratio of the nickel sulfate to the nickel sulfamate is (2-5): 1.
Preferably, the reducing agent is at least one selected from boric acid, borohydride, hypophosphite, hydroquinone, amine borane, hydrazine.
Preferably, the stabilizer is at least one selected from rare earth salts, rare earth oxides and organic sulfur compounds.
Preferably, the organic acid is at least one selected from the group consisting of gluconic acid, benzoic acid, salicylic acid, malic acid, citric acid, and glycolic acid.
Preferably, the raw materials comprise the following components in percentage by mass: 8-30% of nickel sulfate, 4-10% of nickel sulfamate, 2-5% of reducing agent, 0.5-1.5% of stabilizer, 2-5% of organic acid, 0.001-0.01% of anionic surfactant, 0.05-0.5% of titanium dioxide and the balance of deionized water.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.0-6.0 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 30-50 ℃, the electroplating current is 80-100A, and the electroplating time is 10-40min.
Compared with the prior art, the invention has the beneficial effects that:
1. In the system, the obtained coating shows good flatness under the interaction of citric acid and malic acid with nickel sulfate and nickel sulfamate with specific proportions.
2. In the system, under the combined action of titanium dioxide with specific particle size, specific nickel source, hypophosphite, specific organic acid and the like, the prepared plating solution shows good stability, and the compactness of the obtained plating layer can be further improved.
3. In the system, the plating layer and the substrate show excellent adhesion performance under the combined action of thiourea with a specific content and sodium dodecyl sulfonate with a specific content.
4. The electroless nickel plating solution prepared by the invention is suitable for plating nickel layers on the surfaces of aluminum alloy plates, steel products, ironworks and the like.
Detailed Description
In a first aspect, the present invention provides an electroless nickel plating solution, comprising: nickel sulfate, nickel sulfamate, anionic surfactant, functional additive and deionized water.
Preferably, the anionic surfactant is at least one selected from alkyl sulfate, alkyl sulfonate, alkylphenol sulfate, and alkyl phosphate.
Preferably, the alkyl sulfonate is at least one selected from sodium dodecyl sulfonate, sodium tetradecyl sulfonate, sodium hexadecyl sulfonate and sodium octadecyl sulfonate.
Preferably, the anionic surfactant is sodium dodecyl sulfonate.
Preferably, the functional additive comprises at least one of a reducing agent, a stabilizing agent, an organic acid and a brightening agent.
Preferably, the functional additive further comprises titanium dioxide.
Preferably, the average particle size of the titanium dioxide is 30nm, and the titanium dioxide is purchased from Xuan Chengjing Rui New materials Co., ltd, and has the model number of: VK-T30D.
In the system, titanium dioxide with specific particle size can show good dispersibility among various raw material molecules and ions of the system, so that the probability of occurrence of the phenomenon of overlarge local current in the electroplating process is reduced, the probability of occurrence of active crystal cores in the plating solution in the electroplating process is also reduced, the stability of the plating solution is improved, and the compactness of the plating layer is further improved.
Preferably, the mass ratio of the nickel sulfate to the nickel sulfamate is (2-5): 1.
Preferably, the reducing agent is at least one selected from boric acid, borohydride, hypophosphite, hydroquinone, amine borane, hydrazine.
Preferably, the reducing agent is sodium hypophosphite.
Preferably, the stabilizer is at least one selected from rare earth salts, rare earth oxides and organic sulfur compounds.
Preferably, the rare earth salt is at least one selected from rare earth sulfate salt, rare earth hydrochloride salt and rare earth phosphate salt.
Preferably, the organic sulfur compound is selected from at least one of thiourea, 2, 4-dithiobiuret, 1, 4-phenylene bis (thiourea).
Preferably, the stabilizer is thiourea.
Preferably, the organic acid is at least one selected from the group consisting of gluconic acid, benzoic acid, salicylic acid, malic acid, citric acid, and glycolic acid.
Preferably, the organic acid is a mixture of malic acid and citric acid.
Preferably, the mass ratio of the malic acid to the citric acid is 1: (3-5).
In the system, under the interaction of citric acid and malic acid in specific proportion, nickel sulfate in specific proportion and nickel sulfamate in specific proportion, active groups contained in the malic acid and the citric acid complex free nickel ions in the system, and the deposition speed of the nickel ions is stabilized, so that the plating layer shows good flatness.
Preferably, the raw materials comprise the following components in percentage by mass: 8-30% of nickel sulfate, 4-10% of nickel sulfamate, 2-5% of reducing agent, 0.5-1.5% of stabilizer, 2-5% of organic acid, 0.001-0.01% of anionic surfactant, 0.05-0.5% of titanium dioxide and the balance of deionized water.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.0-6.0 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 30-50 ℃, the electroplating current is 80-100A, and the electroplating time is 10-40min.
Preferably, the acid-base modifier is sulfuric acid and ammonia water.
The present invention will be specifically described below by way of examples. It is noted herein that the following examples are given solely for the purpose of further illustration and are not to be construed as limitations on the scope of the invention, as will be apparent to those skilled in the art in light of the foregoing disclosure.
Example 1
The invention provides a chemical nickel plating solution, which comprises the following raw materials in percentage by mass: the balance is made up of 20% nickel sulfate, 4% nickel sulfamate, 3% sodium hypophosphite, 1.5% thiourea, 5% organic acid, 0.01% sodium dodecyl sulfate, 0.2% titanium dioxide and deionized water.
Wherein the organic acid is malic acid and citric acid, and the mass ratio of the malic acid to the citric acid is 1:4.
The titanium dioxide has an average particle size of 30nm and is purchased from Xuan Chengjing Rui New Material Co., ltd., model number: VK-T30D.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.8 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 50 ℃, the electroplating current is 80A, and the electroplating time is 25min.
Wherein the acid-base modifier is 10wt% sodium hydroxide aqueous solution and 5wt% sulfuric acid aqueous solution.
Example 2
The invention provides a chemical nickel plating solution, which comprises the following raw materials in percentage by mass: the balance is supplemented by 25 percent of nickel sulfate, 5 percent of nickel sulfamate, 2 percent of sodium hypophosphite, 0.5 percent of thiourea, 3 percent of organic acid, 0.01 percent of sodium dodecyl sulfate, 0.5 percent of titanium dioxide and deionized water.
Wherein the organic acid is malic acid and citric acid, and the mass ratio of the malic acid to the citric acid is 1:2.
The titanium dioxide has an average particle size of 30nm and is purchased from Xuan Chengjing Rui New Material Co., ltd., model number: VK-T30D.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.8 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 50 ℃, the electroplating current is 80A, and the electroplating time is 25min.
Wherein the acid-base modifier is 10wt% sodium hydroxide aqueous solution and 5wt% sulfuric acid aqueous solution.
Example 3
The invention provides a chemical nickel plating solution, which comprises the following raw materials in percentage by mass: the balance is 3% nickel sulfate, 18% nickel sulfamate, 3% sodium hypophosphite, 1.5% thiourea, 5% organic acid, 0.01% sodium dodecyl sulfate, 0.2% titanium dioxide and deionized water.
Wherein the organic acid is malic acid and citric acid, and the mass ratio of the malic acid to the citric acid is 1:4.
The titanium dioxide has an average particle size of 30nm and is purchased from Xuan Chengjing Rui New Material Co., ltd., model number: VK-T30D.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.8 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 50 ℃, the electroplating current is 80A, and the electroplating time is 25min.
Wherein the acid-base modifier is 10wt% sodium hydroxide aqueous solution and 5wt% sulfuric acid aqueous solution.
Example 4
The invention provides a chemical nickel plating solution, which comprises the following raw materials in percentage by mass: the balance is made up of 20% nickel sulfate, 4% nickel sulfamate, 3% sodium hypophosphite, 1.5% thiourea, 5% organic acid, 0.01% sodium dodecyl sulfate, 0.2% titanium dioxide and deionized water.
Wherein the organic acid is malic acid and citric acid, and the mass ratio of the malic acid to the citric acid is 20:1.
The titanium dioxide has an average particle size of 30nm and is purchased from Xuan Chengjing Rui New Material Co., ltd., model number: VK-T30D.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.8 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 50 ℃, the electroplating current is 80A, and the electroplating time is 25min.
Wherein the acid-base modifier is 10wt% sodium hydroxide aqueous solution and 5wt% sulfuric acid aqueous solution.
Example 5
The invention provides a chemical nickel plating solution, which comprises the following raw materials in percentage by mass: the balance is made up of 20% nickel sulfate, 4% nickel sulfamate, 3% sodium hypophosphite, 1.5% thiourea, 5% organic acid, 0.01% sodium dodecyl sulfate, 0.2% titanium dioxide and deionized water.
Wherein the organic acid is malic acid and citric acid, and the mass ratio of the malic acid to the citric acid is 1:4.
The titanium dioxide has an average particle size of 150nm and is commercially available from the Biotechnology Co., inc. of Sean Ji Yue.
In a second aspect, the present invention provides an electroplating process of electroless nickel plating solution, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.8 by using an acid-base regulator.
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 50 ℃, the electroplating current is 80A, and the electroplating time is 25min.
Wherein the acid-base modifier is 10wt% sodium hydroxide aqueous solution and 5wt% sulfuric acid aqueous solution.
Performance testing
The plated article obtained in the example was subjected to tests of nickel layer thickness, nickel layer porosity, and nickel layer adhesion. The data are recorded in table 1.
1. Nickel layer thickness
The nickel layer thickness was measured by X-ray fluorescence spectroscopy.
2. Porosity of nickel layer
The nickel layer porosity test was performed with reference to GB/T12332-2008.
3. Adhesion of nickel layer
Dividing the nickel layer on the workpiece into 20 squares with the area of 1mm 2, sticking the adhesive tape, peeling the adhesive tape after 10 minutes, and recording the number of the peeled squares.
TABLE 1
Finally, it is pointed out that the foregoing examples are illustrative only and serve to explain some of the features of the method according to the invention. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the invention. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.
Claims (3)
1. The electroless nickel plating solution is characterized by comprising the following raw materials in percentage by mass: 8-30% of nickel sulfate, 4-10% of nickel sulfamate, 2-5% of reducing agent, 0.5-1.5% of stabilizer, 2-5% of organic acid, 0.001-0.01% of anionic surfactant, 0.05-0.5% of titanium dioxide and deionized water, and the balance being supplemented;
the average particle diameter of the titanium dioxide is 30nm;
the organic acid is a mixture of malic acid and citric acid, and the mass ratio of the malic acid to the citric acid is 1: (3-5);
the anionic surfactant is at least one selected from alkyl sulfate, alkyl sulfonate, alkylphenol sulfate and alkyl phosphate;
The reducing agent is at least one selected from boric acid, borohydride, hypophosphite, hydroquinone, amine borane and hydrazine;
the stabilizer is at least one selected from rare earth salts, rare earth oxides and organic sulfur compounds.
2. The electroless nickel plating solution according to claim 1, wherein the mass ratio of the nickel sulfate to the nickel sulfamate is (2-5): 1.
3. A plating process of an electroless nickel plating solution according to any one of claims 1 to 2, comprising the steps of:
(1) Preparing chemical nickel plating solution according to the chemical nickel plating solution formula, and adjusting the pH value of the chemical nickel plating solution to 4.0-6.0 by using an acid-base regulator;
(2) Nickel plating is carried out on the workpiece, the anode plate is a nickel plate, and the cathode plate is a workpiece; the temperature of the nickel plating process is 30-50 ℃, the electroplating current is 80-100A, and the electroplating time is 10-40min.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102828207A (en) * | 2012-09-13 | 2012-12-19 | 广东达志环保科技股份有限公司 | Nickel electroplating solution and electroplating method thereof |
| CN104947094A (en) * | 2014-03-27 | 2015-09-30 | 浙江德汇电子陶瓷有限公司 | Chemical nickel plating solution and application thereof in chemical nickel plating as well as circuit board |
| CN105256345A (en) * | 2015-10-10 | 2016-01-20 | 安徽长青电子机械（集团）有限公司 | Rustproof composite electroplating bath |
| CN106086832A (en) * | 2016-07-21 | 2016-11-09 | 江苏盈科汽车空调有限公司 | A kind of maintaining method of car air conditioning compressor slanting plate surface nickel phosphorus alloy special chemistry nickel plating bath |
| CN106086830A (en) * | 2016-07-21 | 2016-11-09 | 江苏盈科汽车空调有限公司 | A kind of modified model high-antiwear self-lubricating chemical nickel plating solution |
| CN106868571A (en) * | 2016-12-25 | 2017-06-20 | 句容亿格纳米材料厂 | A kind of nanometer molybdenum palladium titanium electroplate liquid and preparation method thereof |
| CN109518171A (en) * | 2018-12-24 | 2019-03-26 | 广州传福化学技术有限公司 | A kind of chemical nickel-plating liquid |
| CN109773178A (en) * | 2017-11-15 | 2019-05-21 | 青岛凯玉盈商贸有限公司 | A kind of processing method of chemical nickel-plating solution |
| CN110318044A (en) * | 2019-06-20 | 2019-10-11 | 深圳市宏达秋科技有限公司 | A kind of chemical nickel-plating liquid and preparation method thereof |
| CN112501598A (en) * | 2020-11-30 | 2021-03-16 | 南通麦特隆新材料科技有限公司 | Chemical nickel plating solution for aluminum substrate PCB circuit board and preparation method thereof |
-
2021
- 2021-05-31 CN CN202110598956.6A patent/CN114808048B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102828207A (en) * | 2012-09-13 | 2012-12-19 | 广东达志环保科技股份有限公司 | Nickel electroplating solution and electroplating method thereof |
| CN104947094A (en) * | 2014-03-27 | 2015-09-30 | 浙江德汇电子陶瓷有限公司 | Chemical nickel plating solution and application thereof in chemical nickel plating as well as circuit board |
| CN105256345A (en) * | 2015-10-10 | 2016-01-20 | 安徽长青电子机械（集团）有限公司 | Rustproof composite electroplating bath |
| CN106086832A (en) * | 2016-07-21 | 2016-11-09 | 江苏盈科汽车空调有限公司 | A kind of maintaining method of car air conditioning compressor slanting plate surface nickel phosphorus alloy special chemistry nickel plating bath |
| CN106086830A (en) * | 2016-07-21 | 2016-11-09 | 江苏盈科汽车空调有限公司 | A kind of modified model high-antiwear self-lubricating chemical nickel plating solution |
| CN106868571A (en) * | 2016-12-25 | 2017-06-20 | 句容亿格纳米材料厂 | A kind of nanometer molybdenum palladium titanium electroplate liquid and preparation method thereof |
| CN109773178A (en) * | 2017-11-15 | 2019-05-21 | 青岛凯玉盈商贸有限公司 | A kind of processing method of chemical nickel-plating solution |
| CN109518171A (en) * | 2018-12-24 | 2019-03-26 | 广州传福化学技术有限公司 | A kind of chemical nickel-plating liquid |
| CN110318044A (en) * | 2019-06-20 | 2019-10-11 | 深圳市宏达秋科技有限公司 | A kind of chemical nickel-plating liquid and preparation method thereof |
| CN112501598A (en) * | 2020-11-30 | 2021-03-16 | 南通麦特隆新材料科技有限公司 | Chemical nickel plating solution for aluminum substrate PCB circuit board and preparation method thereof |
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