CN111876797A - High-corrosion-resistance neutral nickel plating solution and neutral nickel priming process - Google Patents
High-corrosion-resistance neutral nickel plating solution and neutral nickel priming process Download PDFInfo
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- CN111876797A CN111876797A CN202010649644.9A CN202010649644A CN111876797A CN 111876797 A CN111876797 A CN 111876797A CN 202010649644 A CN202010649644 A CN 202010649644A CN 111876797 A CN111876797 A CN 111876797A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 254
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 127
- 238000007747 plating Methods 0.000 title claims abstract description 124
- 230000007935 neutral effect Effects 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 45
- 230000008569 process Effects 0.000 title claims abstract description 40
- 230000037452 priming Effects 0.000 title claims abstract description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 134
- 239000000243 solution Substances 0.000 claims abstract description 114
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 81
- 229910052742 iron Inorganic materials 0.000 claims abstract description 68
- 150000003839 salts Chemical class 0.000 claims abstract description 53
- 238000009713 electroplating Methods 0.000 claims abstract description 51
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 21
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 21
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 21
- 229960002635 potassium citrate Drugs 0.000 claims abstract description 20
- 239000001508 potassium citrate Substances 0.000 claims abstract description 20
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims abstract description 20
- 235000011082 potassium citrates Nutrition 0.000 claims abstract description 20
- 230000007797 corrosion Effects 0.000 claims abstract description 19
- 238000005260 corrosion Methods 0.000 claims abstract description 19
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- DETXZQGDWUJKMO-UHFFFAOYSA-N 2-hydroxymethanesulfonic acid Chemical compound OCS(O)(=O)=O DETXZQGDWUJKMO-UHFFFAOYSA-N 0.000 claims abstract description 9
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 7
- URWIWRCHIPAGBL-UHFFFAOYSA-N OCC1OP(=O)OP(=O)O1 Chemical compound OCC1OP(=O)OP(=O)O1 URWIWRCHIPAGBL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 239000003792 electrolyte Substances 0.000 claims description 21
- 238000005238 degreasing Methods 0.000 claims description 20
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 claims description 20
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 10
- RQNVGUOKYSZUJN-UHFFFAOYSA-N [K].P1(=O)OC(CO)OP(O1)=O Chemical compound [K].P1(=O)OC(CO)OP(O1)=O RQNVGUOKYSZUJN-UHFFFAOYSA-N 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 9
- 229910052714 tellurium Inorganic materials 0.000 claims description 8
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 6
- -1 rare earth metal salt Chemical class 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- 230000008021 deposition Effects 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 9
- 229910001453 nickel ion Inorganic materials 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000004506 ultrasonic cleaning Methods 0.000 description 8
- 238000006073 displacement reaction Methods 0.000 description 7
- PHZLMBHDXVLRIX-UHFFFAOYSA-M potassium lactate Chemical compound [K+].CC(O)C([O-])=O PHZLMBHDXVLRIX-UHFFFAOYSA-M 0.000 description 6
- 239000001521 potassium lactate Substances 0.000 description 6
- 235000011085 potassium lactate Nutrition 0.000 description 6
- 229960001304 potassium lactate Drugs 0.000 description 6
- YYKGYTHEGCZRRI-UHFFFAOYSA-M potassium;hydroxymethanesulfonate Chemical compound [K+].OCS([O-])(=O)=O YYKGYTHEGCZRRI-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000008139 complexing agent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- INJHMDMDOFJODH-UHFFFAOYSA-N O.O.[Ni].[Ni] Chemical compound O.O.[Ni].[Ni] INJHMDMDOFJODH-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method 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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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 invention discloses a high-corrosion-resistance neutral nickel plating solution and a neutral nickel priming process, wherein the high-corrosion-resistance neutral nickel plating solution comprises the following components in parts by weight: 90-110 g/L of nickel sulfate, 16-24 g/L of nickel chloride, 110-130 g/L of conductive salt, 25-35 ml/L of agent A and 25-35 ml/L of agent B, wherein the conductive salt comprises hydroxymethyl sulfonate, citrate and lactate, the agent A comprises potassium citrate and hydroxyethylidene diphosphonate, and the agent B is a rare earth metal salt solution. The neutral nickel priming process comprises the steps of oil and rust removal treatment of an iron-based workpiece and electroplating of a bottom nickel layer. The high-corrosion-resistance neutral nickel plating solution and the neutral nickel priming process provided by the invention can form a thicker and more compact plating layer on the surface of the iron base under the condition of higher current density, the plating layer can better protect the iron base workpiece, prevent the iron base workpiece from generating a replacement reaction in the subsequent electroplating process, and have higher corrosion resistance.
Description
Technical Field
The invention relates to the technical field of electroplating processing, in particular to a high-corrosion-resistance neutral nickel plating solution and a neutral nickel priming process.
Background
Electroplating is a very common surface treatment process, and is a method for attaching a layer of metal on the surface of a conductor by using the principle of electrolysis. In the electroplating process, the plated base metal is used as cathode and is placed in salt solution containing preplating metal, and the cation of preplating metal in the plating solution is deposited on the surface of base metal by means of electrolysis to form a plating layer. The plating layer on the surface of the substrate can play a role in preventing corrosion, improving wear resistance, conductivity and light reflection, enhancing the appearance and the like. Iron-based workpieces tend to have their surfaces treated due to the tendency to rust, wherein a surface plated metal layer is a common method for surface treatment of iron-based materials, and the existing plated metal layer is usually plated in an acidic plating solution. However, according to the metal activity sequence table, the metal sequences of iron, zinc, aluminum and magnesium are arranged in front of hydrogen and are more active than hydrogen, so that when the iron base containing the metals is electroplated in an acidic system, the iron, the zinc, the aluminum and the magnesium can generate a displacement reaction with acid at the first time, so that impurities are brought into a plating solution during electroplating, the low region cannot be well moved due to the generation of the impurities in the plating solution, the bonding force of the plating layer is reduced, and the defective rate is extremely high; in addition, once plating solution impurities are generated, the consumption of raw materials is increased, the plating cost is increased, the subsequent treatment of the plating solution is complicated, and the wastewater treatment cost is increased. In order to prevent the iron base from generating a displacement reaction during electroplating in an acidic system and inhibit iron ions or zinc, aluminum and magnesium ions from being brought into a plating solution, a surface pretreatment is carried out in the prior art by adopting a copper-based priming method, however, the prior copper-based priming adopts a cyanide plating solution, so that the pollution is large, the wastewater treatment is troublesome, the additive variety of the copper-based plating solution is complicated, and the deep hole electroplating capability is poor. It is seen that improvements and enhancements to the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a high-corrosion-resistance neutral nickel plating solution and a neutral nickel priming process, and aims to overcome the defect that iron base generates a displacement reaction in the plating solution of an acid system and generates micro corrosion in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a highly corrosion resistant neutral nickel plating solution, wherein the plating solution comprises: 90-110 g/L of nickel sulfate, 16-24 g/L of nickel chloride, 110-130 g/L of conductive salt, 25-35 ml/L of agent A and 25-35 ml/L of agent B, wherein the conductive salt comprises hydroxymethyl sulfonate, citrate and lactate, the agent A comprises potassium citrate and hydroxyethylidene diphosphonate (HEDP. Kx), and the agent B is a rare earth metal salt solution.
In the high-corrosion-resistance neutral nickel plating solution, the weight ratio of the hydroxymethyl sulfonate, the citrate and the lactate in the conductive salt is 1:3: 1.
In the high-corrosion-resistance neutral nickel plating solution, the weight ratio of potassium citrate to potassium hydroxyethylidene diphosphonate in the agent A is 4: 1.
In the high-corrosion-resistance neutral nickel plating solution, the rare earth metal salt comprises one of strontium sulfate and tellurium sulfate.
In the high-corrosion-resistance neutral nickel plating solution, the preparation method of the plating solution comprises the following steps: accurately weighing each component according to the proportion, and dissolving nickel sulfate, nickel chloride and conductive salt with deionized water to obtain a main salt solution; dissolving the agent A with deionized water, stirring uniformly, and adding the agent B into the agent A to obtain a mixed solution of the agent A and the agent B; and adding the mixed solution of the agent A and the agent B into the main salt solution, adding the rest deionized water, uniformly stirring, and adjusting the pH value to 7 by using sodium hydroxide or ammonia water to obtain the high-corrosion-resistance neutral nickel plating solution.
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: carrying out oil removal and water washing on the iron-based workpiece twice, carrying out acid washing and rust removal, and then carrying out water washing twice;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after oil and rust removal is placed in the high-corrosion-resistance neutral nickel plating solution to be electroplated with a bottom nickel layer, wherein the current density is 9-11A/dm2The voltage is 8-10V, and the electroplating time is 3-5 min.
In the novel high corrosion resistance neutral nickel priming process, in step S2, the high corrosion resistance neutral nickel plating solution is: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of neutral conductive salt, 30ml/L of agent A and 30ml/L of agent B.
In the novel high-corrosion-resistance neutral nickel priming process, in the step S1, the oil removal includes one of electrolytic oil removal or ultrasonic oil removal.
In the novel high-corrosion-resistance neutral nickel priming process, the electrolytic oil removal comprises the following specific steps: putting an iron-based workpiece into electrolyte for electrolytic degreasing for 1-2min, wherein the electrolyte comprises 5-8 g/L of NaOH and NaHCO310-20 g/L, the temperature of the electrolyte is 40-60 ℃, and the current density is 2-4A/dm2。
In the novel high-corrosion-resistance neutral nickel priming process, the ultrasonic oil removal comprises the following specific steps: iron-based workpieceUltrasonic degreasing is carried out for 20-30 min in alkaline cleaning solution, wherein the alkaline cleaning solution comprises 1-3 g/L of NaOH and NaHCO35-8 g/L, the water bath temperature is 50-60 ℃, and the ultrasonic frequency is 20-40 Hz.
Has the advantages that:
the invention provides a high-corrosion-resistance neutral nickel plating solution and a neutral nickel priming process, wherein the high-corrosion-resistance neutral nickel plating solution is a neutral system, metal impurity ions cannot generate a displacement reaction in the electroplating process, and an agent A and an agent B which are added can form a stable complex with the nickel ions and reduce the polarization potential of a cathode, so that a thicker and denser plating layer can be formed on the surface of an iron base under the condition of higher current density, an iron-base workpiece is effectively protected from the displacement reaction in the subsequent electroplating process, and the high-corrosion-resistance neutral nickel plating solution has higher corrosion resistance. The novel high-corrosion-resistance neutral nickel priming process is simple to operate and good in priming effect, the obtained priming nickel layer is firmly combined with the iron-based workpiece, and the binding force of a subsequent coating can be improved.
Detailed Description
The invention provides a high-corrosion-resistance neutral nickel plating solution and a neutral nickel priming process, and in order to make the purpose, technical scheme and effect of the invention clearer and more clear, the invention is further described in detail by the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A highly corrosion resistant neutral nickel plating solution, wherein the plating solution comprises: 90-110 g/L of nickel sulfate, 16-24 g/L of nickel chloride, 110-130 g/L of conductive salt, 25-35 ml/L of agent A and 25-35 ml/L of agent B, wherein the conductive salt comprises hydroxymethyl sulfonate, citrate and lactate, the agent A comprises potassium citrate and hydroxy ethylidene diphosphonate (HEDP. Kx) solution, and the agent B is rare earth metal salt solution. The high-corrosion-resistance neutral nickel plating solution is used for priming treatment before plating nickel, nickel barrel plating, common nickel plating or zinc barrel plating on an iron-based workpiece, a thick bottom nickel layer can be formed on the surface of the iron-based workpiece by adopting the plating solution for plating, the iron-based workpiece can be prevented from generating a replacement reaction in a plating seed of an acid system, iron ions or other metal ions are prevented from being brought into the plating solution, the function of preventing a base part from being corroded slightly is achieved, the corrosion resistance of the iron-based workpiece is improved, in addition, the bottom nickel can also strengthen the binding force between a subsequent plating layer and the iron base, the plating time of the subsequent process is shortened, the raw material cost is saved, the yield of products is improved, and. The high-corrosion-resistance neutral nickel plating solution does not contain cyanide, is safe to use and low in cost, and can recycle nickel as a raw material by using the nickel-nickel dihydrate, so that the utilization rate of nickel is improved.
Specifically, the nickel sulfate and the nickel chloride are main salts and can provide nickel ions for electroplating, and the total concentration of the nickel sulfate and the nickel chloride directly influences the dispersibility of the plating solution, the deposition speed of the nickel ions and the particle size of the crystal of the plating layer. In the conventional electroplating process, the phenomenon that the deposition speed is high and the crystal particles of a coating are large easily occurs when the concentration of the main salt is too high, the concentration dispersibility is poor, the uniform plating force is poor, and the defect of low deposition speed exists when the concentration of the main salt is low. In the invention, the A agent, the B agent and the conductive salt are added, so that the concentration of the main salt can be greatly improved, the uniformity and the fineness of the plating layer can be improved, even if the concentration of nickel sulfate in the main salt is 90-110 g/L and the concentration of nickel chloride is 16-24 g/L, the good dispersibility and the moderate deposition speed are still achieved, and the obtained plating layer crystal is fine and uniform.
Specifically, the conductive salt is hydroxymethyl sulfonate, citrate and lactate, and can improve the conductivity of the plating solution, improve the deep plating capability and the dispersibility of the main salt and ensure that the low region has good displacement. Meanwhile, the conductive salt also has a buffering effect, so that the pH value of the system is kept at about 7, the active metal impurities are prevented from being subjected to a displacement reaction, and pinholes on the surface of the plating layer are avoided. It should be noted that the concentration of the conductive salt is not too high, which tends to precipitate other salts and affect the performance of the plating solution. When the total concentration of the conductive salt is 110-130 g/L, the plating solution has better conductivity, better dispersibility and deep plating capability of the main salt, and better solubility of each component in the plating solution. Preferably, when the total concentration of the conductive salt is 120g/L and the weight ratio of the hydroxymethyl sulfonate, the citrate and the lactate is 1:3:1, the conductivity of the plating solution and the solubility of other salts in the plating solution are better. More preferably, when the hydroxymethyl sulfonate, the citrate and the lactate are all potassium salts, the conductivity, the solubility and the dispersibility of the plating solution are optimal.
Specifically, the agent A is a complexing agent which can be complexed with metal ions in the main salt to form a stable complex. The complexing agent is a composite complexing agent and comprises potassium citrate and hydroxyethylidene diphosphonate, wherein citrate and hydroxyethylidene diphosphonate (HEDP) and nickel ions can form a stable complex, the equilibrium potential of nickel is reduced, nickel is more easily precipitated on a cathode, the nickel deposition speed is accelerated, and meanwhile, a plating layer crystal is finer. Preferably, when the weight ratio of the potassium citrate to the potassium hydroxyethylidene diphosphonate in the agent A is 4:1, the formed nickel complex is more stable.
Specifically, the rare earth metal salt comprises one of strontium sulfate and tellurium sulfate. The strontium sulfate and the tellurium sulfate have a promoting effect on nickel deposition, can catalyze and accelerate electroplating deposition of main salt, and have a certain chemical balance because the strontium sulfate and the tellurium sulfate are both metal salts which are difficult to dissolve, are easy to precipitate and separate out when the temperature is changed, and the chemical balance is changed when sulfate ions in the plating solution are changed, so that the strontium sulfate and the tellurium sulfate move towards the ionization direction, thereby improving the concentration of the sulfate ions in the plating solution, further improving the dispersibility and the uniform plating capacity of the plating solution, and simultaneously improving the depth capacity of the plating solution.
The preparation method of the high-corrosion-resistance neutral nickel plating solution comprises the following steps: accurately weighing each component according to the proportion, and dissolving nickel sulfate, nickel chloride and conductive salt by using partial deionized water to obtain a main salt solution; dissolving the agent A with partial deionized water, stirring uniformly, and adding the agent B into the agent A to obtain mixed solution of the agent A and the agent B; and adding the mixed solution of the agent A and the agent B into the main salt solution, adding the rest deionized water, uniformly stirring, and finally adjusting the pH value to 7 by using sodium hydroxide or ammonia water to obtain the high-corrosion-resistance neutral nickel plating solution.
According to the high-corrosion-resistance neutral nickel plating solution, the conductive salt, the agent A and the agent B can jointly act on the electroplating deposition of the main salt to influence the deposition of nickel ions on a cathode from multiple aspects, wherein the conductive salt can improve the conductivity of the plating solution and improve the deep plating capability and the dispersibility of the main salt, the agent A can be complexed with the nickel ions to improve the concentration of the main salt and reduce the balance potential of nickel, so that the balance potential of the nickel ions is more negative, the obtained plating layer is thicker and finer in crystal, the agent B can promote the deep hole deposition of the nickel ions, the high-low potential thickness difference of the plating layer is small, the plating layer is more uniform, and the antirust force of the plating layer is improved.
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: removing oil from an iron-based workpiece by using alkaline solution, then passing through deionized water twice, then immersing into 5% hydrochloric acid solution for 1-2min, removing metal oxides on the surface, and then cleaning twice by using deionized water;
s2, electroplating a bottom nickel layer: under the condition of room temperature, placing the iron-based workpiece after pretreatment in the high-corrosion-resistance neutral nickel plating solution to electroplate a bottom nickel layer, wherein the current density is 9-11A/dm2The voltage is 8-10V, and the electroplating time is 3-5 min. In the process of electroplating bottom nickel, the current density is the key for influencing cathode polarization, the thicker the current density is, the coarser the obtained coating crystal is, in the invention, although the larger current density is adopted, the citrate and HEDP in the agent A can promote the dispersion of nickel ions, so that the polarization effect of the cathode is large, and thus, fine and compact coating crystals can be obtained. The conductive salt and the agent B can promote the electroplating deposition speed of the main salt, so that the electroplating time is only 3-5min, and the electroplating is very efficient and rapid.
Preferably, in the novel high corrosion resistance neutral nickel priming process, in step S2, the high corrosion resistance neutral nickel plating solution is: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of neutral conductive salt, 30ml/L of A agent and 30ml/L of B agent, and the effects of thicker plating layer, finer and tighter plating layer crystal and more uniform high and low potential plating layers can be obtained.
Specifically, in the novel high corrosion resistance neutral nickel priming process, in step S1, the oil removal includes one of electrolytic oil removal or ultrasonic oil removal. The purpose of oil removal is to remove oil stains on the surface of the iron-based workpiece and improve the adhesive force of a plating layer. The oil stain can be removed more thoroughly by adopting electrolytic oil removal or ultrasonic oil removal.
Specifically, the electrolytic degreasing specifically comprises the following steps: putting an iron-based workpiece into electrolyte for electrolytic degreasing for 1-2min, wherein the electrolyte comprises 5-8 g/L of NaOH and NaHCO310-20 g/L, the temperature of the electrolyte is 40-60 ℃, and the current density is 2-4A/dm2. The electrolytic degreasing has the characteristics of high speed and high efficiency.
Specifically, the ultrasonic oil removal method comprises the following specific steps: putting an iron-based workpiece into an alkaline cleaning solution to remove oil for 20-30 min by ultrasonic treatment, wherein the alkaline cleaning solution comprises 1-3 g/L of NaOH and NaHCO35-8 g/L, the water bath temperature is 50-60 ℃, and the ultrasonic frequency is 20-40 Hz. The ultrasonic degreasing effect is more thorough, but the time consumption is longer.
The present invention will be further described with reference to the following examples.
Example 1
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, an iron-based workpiece is placed in electrolyte for electrolytic degreasing for 1min, wherein the electrolyte comprises NaOH 5g/L and NaHCO310g/L, the temperature of the electrolyte is 60 ℃, and the current density is 4A/dm2After electrolytic degreasing, the surface of the iron-based workpiece is cleaned by deionized water twice, then the iron-based workpiece is immersed in a 5% hydrochloric acid solution for 1min, and then the iron-based workpiece is cleaned twice by deionized water;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in high-corrosion-resistance neutral nickel plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 9A/dm2The voltage is 8V, the electroplating time is 3min, and the high-corrosion-resistance neutral nickel plating solution comprises: 110g/L of nickel sulfate, 24g/L of nickel chloride, 130g/L of conductive salt, 35ml/L of agent A and 35ml/L of agent B, and the pH value of the plating solution is 7. The conductive salt comprises potassium hydroxymethyl sulfonate, potassium citrate and potassium lactate in a weight ratio of 1:3:1, the agent A comprises potassium citrate and potassium hydroxyethylidene diphosphonate in a weight ratio of 4:1, and the agent B is a strontium sulfate solution.
Example 2
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, an iron-based workpiece is placed in electrolyte for electrolytic degreasing for 2min, wherein the electrolyte comprises 8g/L NaOH and NaHCO320g/L, the temperature of the electrolyte is 40 ℃, and the current density is 2A/dm2After electrolytic degreasing, the surface of the iron-based workpiece is cleaned by deionized water twice, then the iron-based workpiece is immersed in a 5% hydrochloric acid solution for 2min, and then the iron-based workpiece is cleaned twice by deionized water;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in high-corrosion-resistance neutral nickel plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 11A/dm2The voltage is 10V, the electroplating time is 5min, and the high-corrosion-resistance neutral nickel plating solution comprises: 90g/L of nickel sulfate, 16g/L of nickel chloride, 110g/L of conductive salt, 25ml/L of agent A and 25ml/L of agent B, and the pH value of the plating solution is 7. The conductive salt comprises potassium hydroxymethyl sulfonate, potassium citrate and potassium lactate in a weight ratio of 1:3:1, the agent A comprises potassium citrate and potassium hydroxyethylidene diphosphonate in a weight ratio of 4:1, and the agent B is a tellurium sulfate solution.
Example 3
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, an iron-based workpiece is placed in electrolyte for electrolytic degreasing for 2min, wherein the electrolyte comprises NaOH 7g/L and NaHCO315g/L, the temperature of the electrolyte is 50 ℃, and the current density is 3A/dm2After electrolytic degreasing, the surface of the iron-based workpiece is cleaned by deionized water twice, then the iron-based workpiece is immersed in a 5% hydrochloric acid solution for 2min, and then the iron-based workpiece is cleaned twice by deionized water;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in high-corrosion-resistance neutral nickel plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 10A/dm2The voltage is 9V, the electroplating time is 4min, and the high-corrosion-resistance neutral nickel plating solution comprises: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of conductive salt, 30ml/L of agent A, 30ml/L of agent B, and the pH value of the plating solution is 7. The electric conductionThe salt comprises potassium hydroxymethyl sulfonate, potassium citrate and potassium lactate in a weight ratio of 1:3:1, the agent A comprises potassium citrate and potassium hydroxyethylidene diphosphonate in a weight ratio of 4:1, and the agent B is a strontium sulfate solution.
Example 4
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, placing an iron-based workpiece in an ultrasonic cleaning tank for ultrasonic oil removal, wherein a tank liquor in the ultrasonic cleaning tank comprises 1g/L of NaOH and 35 g/L of NaHCO, the temperature of the tank liquor is 60 ℃, the ultrasonic frequency is 40Hz, ultrasonic oil removal is carried out for 30min, then deionized water is carried out twice, then the iron-based workpiece is immersed in a 5% hydrochloric acid solution for 2min, and then the iron-based workpiece is cleaned twice by the deionized water;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in high-corrosion-resistance neutral nickel plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 9A/dm2The voltage is 8V, the electroplating time is 5min, and the high-corrosion-resistance neutral nickel plating solution comprises: 90g/L of nickel sulfate, 16g/L of nickel chloride, 110g/L of conductive salt, 25ml/L of agent A and 25ml/L of agent B, and the pH value of the plating solution is 7. The conductive salt comprises potassium hydroxymethyl sulfonate, potassium citrate and potassium lactate in a weight ratio of 1:3:1, the agent A comprises potassium citrate and potassium hydroxyethylidene diphosphonate in a weight ratio of 4:1, and the agent B is a strontium sulfate solution.
Example 5
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, an iron-based workpiece is placed in an ultrasonic cleaning tank for ultrasonic oil removal, and tank liquor in the ultrasonic cleaning tank comprises NaOH 3g/L and NaHCO38g/L, the temperature of bath solution is 50 ℃, the ultrasonic frequency is 20Hz, ultrasonic oil removal is carried out for 20min, then deionized water is carried out twice, then the iron-based workpiece is immersed into 5% hydrochloric acid solution for 2min, and then deionized water is used for cleaning twice;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after pretreatment is used as a cathode and is placed in a high-voltage-resistant stateElectroplating bottom nickel layer in neutral nickel plating solution with nickel block as anode and current density of 11A/dm2The voltage is 10V, the electroplating time is 3min, and the high-corrosion-resistance neutral nickel plating solution comprises: 110g/L of nickel sulfate, 24g/L of nickel chloride, 130g/L of conductive salt, 35ml/L of agent A and 35ml/L of agent B, and the pH value of the plating solution is 7. The conductive salt comprises potassium hydroxymethyl sulfonate, potassium citrate and potassium lactate in a weight ratio of 1:3:1, the agent A comprises potassium citrate and potassium hydroxyethylidene diphosphonate in a weight ratio of 4:1, and the agent B is a tellurium sulfate solution.
Example 6
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, placing an iron-based workpiece in an ultrasonic cleaning tank for ultrasonic oil removal, wherein a tank liquor in the ultrasonic cleaning tank comprises 2g/L of NaOH and 36 g/L of NaHCO, the temperature of the tank liquor is 55 ℃, the ultrasonic frequency is 30Hz, ultrasonic oil removal is carried out for 25min, then deionized water is carried out twice, then the iron-based workpiece is immersed in a 5% hydrochloric acid solution for 2min, and then the iron-based workpiece is cleaned twice by the deionized water;
s2, electroplating a bottom nickel layer: under the condition of room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in high-corrosion-resistance neutral nickel plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 10A/dm2The voltage is 9V, the electroplating time is 4min, and the high-corrosion-resistance neutral nickel plating solution comprises: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of conductive salt, 30ml/L of agent A, 30ml/L of agent B, and the pH value of the plating solution is 7. The conductive salt comprises potassium hydroxymethyl sulfonate, potassium citrate and potassium lactate in a weight ratio of 1:3:1, the agent A comprises potassium citrate and potassium hydroxyethylidene diphosphonate in a weight ratio of 4:1, and the agent B is a strontium sulfate solution.
Comparative example 1
An electronickelling bottoming process, the process comprising the steps of:
s1, oil and rust removal: firstly, an iron-based workpiece is placed in electrolyte for electrolytic degreasing for 2min, wherein the electrolyte comprises NaOH 7g/L and NaHCO315g/L, the temperature of the electrolyte is 50 ℃, and the current density is 3A/dm2Electrolytic removerAfter oiling, deionized water is used for two times to clean the surface of the iron-based workpiece, then the iron-based workpiece is immersed into 5% hydrochloric acid solution for 2min, and then the iron-based workpiece is washed twice by the deionized water;
s2, electroplating a bottom nickel layer: at room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in a nickel-containing plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 10A/dm2Voltage 9V, electroplating time 4min, and plating solution comprising: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of sodium citrate and 25g/L of boric acid, and the pH value of the plating solution is 7.
Comparative example 2
A novel high-corrosion-resistance neutral nickel priming process comprises the following steps:
s1, oil and rust removal: firstly, an iron-based workpiece is placed in an ultrasonic cleaning tank for ultrasonic oil removal, and tank liquor in the ultrasonic cleaning tank comprises 2g/L of NaOH and 2g/L of NaHCO36g/L, the temperature of bath solution is 55 ℃, the ultrasonic frequency is 30Hz, ultrasonic degreasing is carried out for 25min, then deionized water is carried out twice, then the iron-based workpiece is immersed into 5% hydrochloric acid solution for 2min, and then deionized water is used for cleaning twice;
s2, electroplating a bottom nickel layer: at room temperature, the iron-based workpiece after the previous treatment is taken as a cathode and placed in a nickel-containing plating solution, and a nickel block is taken as an anode to carry out electroplating on a bottom nickel layer, wherein the current density is 10A/dm2Voltage 9V, electroplating time 4min, and plating solution comprising: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of sodium citrate and 25g/L of boric acid, and the pH value of the plating solution is 7.
The iron-based workpieces of examples 1 to 6 and comparative examples 1 to 2 were subjected to surface plating thickness tests, and thickness measurements were performed at 4 positions on each workpiece surface using an X-ray thickness gauge, wherein 2.5CM X1.5 CM on the front surface was a high potential region, 2.5CM X5.0 CM on the front surface was a medium potential region, 2.5CM X8.5 CM on the front surface was a low potential region, and 2.5CM X5.0 CM on the back surface was a deep hole position, and the measurement results at each position in each example are shown in table 1.
As can be seen from Table 1, the thicknesses of the high potential region and the low potential region of examples 1 to 6 are thicker than those of comparative examples 1 to 2, which shows that the novel nickel plating solution has better electroplating deposition effect and better corrosion prevention effect on the electroplated workpiece, the thickness of the electroplated layer on the back surface of the workpiece in examples 1 to 6 is more than 0.1 μm, and the back surfaces of the workpieces in comparative examples 1 and 2 have no electroplated layer, so that the novel nickel plating solution has strong deep hole electroplating capability and can be used for electroplating and bottoming of pipe fittings.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (10)
1. A high corrosion resistance neutral nickel plating solution is characterized by comprising the following components: 90-110 g/L of nickel sulfate, 16-24 g/L of nickel chloride, 110-130 g/L of conductive salt, 25-35 ml/L of agent A and 25-35 ml/L of agent B, wherein the conductive salt comprises hydroxymethyl sulfonate, citrate and lactate, the agent A comprises potassium citrate and hydroxyethylidene diphosphonate, and the agent B is a rare earth metal salt solution.
2. The highly corrosion-resistant neutral nickel plating solution as recited in claim 1, wherein the weight ratio of the hydroxymethylsulfonate, the citrate, and the lactate in the conductive salt is 1:3: 1.
3. The highly anticorrosive neutral nickel plating solution according to claim 1, wherein the weight ratio of potassium citrate to potassium hydroxyethylidene diphosphonate in the agent a is 4: 1.
4. The highly corrosion-resistant neutral nickel plating solution of claim 1 wherein the rare earth metal salt comprises one of strontium sulfate and tellurium sulfate.
5. The highly corrosion-resistant neutral nickel plating solution according to claim 1, wherein the plating solution is prepared by the following method: accurately weighing each component according to the proportion, and dissolving nickel sulfate, nickel chloride and conductive salt with deionized water to obtain a main salt solution; dissolving the agent A with deionized water, stirring uniformly, and adding the agent B into the agent A to obtain a mixed solution of the agent A and the agent B; and adding the mixed solution of the agent A and the agent B into the main salt solution, adding the rest deionized water, uniformly stirring, and adjusting the pH value to 7 by using sodium hydroxide or ammonia water to obtain the high-corrosion-resistance neutral nickel plating solution.
6. A novel high-corrosion-resistance neutral nickel priming process is characterized by comprising the following steps:
s1, oil and rust removal: carrying out oil removal and water washing on the iron-based workpiece twice, carrying out acid washing and rust removal, and then carrying out water washing twice;
s2, electroplating a bottom nickel layer: placing the deoiled and derusted iron-based workpiece into the high-corrosion-resistance neutral nickel plating solution according to any one of claims 1 to 5 at room temperature to carry out electroplating on a bottom nickel layer, wherein the current density is 9-11A/dm2The voltage is 8-10V, and the electroplating time is 3-5 min.
7. The novel high corrosion resistance neutral nickel priming process according to claim 6, wherein in the step S2, the high corrosion resistance neutral nickel plating solution is: 100g/L of nickel sulfate, 20g/L of nickel chloride, 120g/L of neutral conductive salt, 30ml/L of agent A and 30ml/L of agent B.
8. The novel high corrosion resistance neutral nickel priming process according to claim 6, wherein in step S1, the degreasing comprises one of electrolytic degreasing or ultrasonic degreasing.
9. The novel high-corrosion-resistance neutral nickel priming process according to claim 8, wherein the electrolytic degreasing comprises the following specific steps: putting an iron-based workpiece into electrolyte for electrolytic degreasing for 1-2min, wherein the electrolyte comprises 5-8 g/L of NaOH and NaHCO310-20 g/L, the temperature of the electrolyte is 40-60 ℃, and the current density is 2-4A/dm2。
10. The novel high-corrosion-resistance neutral nickel priming process according to claim 8, wherein the ultrasonic degreasing comprises the following specific steps: putting an iron-based workpiece into an alkaline cleaning solution to remove oil for 20-30 min by ultrasonic treatment, wherein the alkaline cleaning solution comprises 1-3 g/L of NaOH and NaHCO35-8 g/L, the water bath temperature is 50-60 ℃, and the ultrasonic frequency is 20-40 Hz.
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