CN110965053A - Acidic chemical nickel plating method and solution - Google Patents

Acidic chemical nickel plating method and solution Download PDF

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Publication number
CN110965053A
CN110965053A CN201911158608.6A CN201911158608A CN110965053A CN 110965053 A CN110965053 A CN 110965053A CN 201911158608 A CN201911158608 A CN 201911158608A CN 110965053 A CN110965053 A CN 110965053A
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nickel plating
post
solution
chemical nickel
concentration
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裴玉汝
任可真
张立
刘贵峰
王涛
左倩
刘静
陈巧军
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AECC Aero Engine Xian Power Control Technology Co Ltd
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AECC Aero Engine Xian Power Control Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/48Coating with alloys
    • C23C18/50Coating with alloys with alloys based on iron, cobalt or nickel
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1689After-treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00Electrolytic cleaning, degreasing, pickling or descaling

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Chemically Coating (AREA)

Abstract

The invention belongs to the technical field of chemical nickel plating, and relates to an acidic chemical nickel plating method and solution. The method comprises the steps of preparing a test piece, hanging, electrolytically degreasing, washing with water for the first time, soaking, washing with water for the second time and chemically plating nickel, wherein the acidic chemical nickel plating method further comprises washing with water for the third time and post-treatment after the chemical nickel plating; the post-treatment is to place the test piece after the chemical nickel plating and the third water cleaning in a post-treatment solution for 10 to 25 minutes, wherein the post-treatment solution comprises 23 to 25g/L of sodium dichromate and 5.5 to 7g/L of ammonium heptamolybdate; the temperature of the post-treatment solution is 48 ℃ to 55 ℃, and the pH of the post-treatment solution is 5.0 to 6.0. The invention provides an acidic chemical nickel plating method and solution capable of improving the corrosion resistance of a chemical nickel plating layer.

Description

Acidic chemical nickel plating method and solution
Technical Field
The invention belongs to the technical field of chemical nickel plating, relates to a chemical nickel plating process, and particularly relates to an acidic chemical nickel plating method and solution.
Prior Art
Chemical plating, also known as electroless plating, and autocatalytic plating, is widely used because of its advantages: 1) the plating uniformity and the deep plating capability are good, a plating layer with uniform thickness can be generated on a complex surface, no corner effect exists, and the shape of the substrate is almost copied, so that the method is particularly suitable for plating inner walls of workpieces with complex shapes, cavity parts, deep hole parts, blind hole parts and the like. 2) The chemical plating is started by the autocatalysis activity of the base material, and the plating layer has fine and compact grains, low porosity and excellent surface performance. 3) Low working temperature, high bonding strength between the coating and the substrate and controllable coating thickness. 4) The equipment is simple and the operation is easy. Other non-metallic surfaces besides metals may be plated. 5) The coating has special mechanical, physical and chemical properties. The chemical nickel plating alloy layer has fine crystallization, no hole, semi-bright or mirror luster, good chemical stability, high hardness and wear resistance.
Because the chemical nickel-phosphorus alloy plating layer belongs to the cathode covering layer, the incompleteness or the existence of extremely fine pores of the plating layer can cause the formation of a large cathode and small anode type corrosion galvanic cell between the base metal and the covering layer, so that the base metal is subjected to more serious local corrosion. In order to better exert the corrosion resistance of the nickel-phosphorus plating layer, in addition to the good pretreatment of the substrate and the strict chemical plating process, the post-treatment after the chemical plating is also very necessary. The method searches journal magazines at home and abroad, and has no relevant data specially aiming at the process method for improving the corrosion resistance of the acid chemical nickel plating.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides an acidic chemical nickel plating method and solution capable of improving the corrosion resistance of a chemical nickel plating layer.
In order to achieve the purpose, the invention adopts the following technical scheme:
an acid chemical nickel plating method comprises the steps of preparing a test piece, hanging, electrolyzing and deoiling, washing with water for the first time, soaking and polishing, washing with water for the second time and chemical nickel plating, and is characterized in that: the acid chemical nickel plating method also comprises a third time of water cleaning and post-treatment after chemical nickel plating; the post-treatment is to place the test piece after the chemical nickel plating and the third water cleaning in a post-treatment solution for 10 to 25 minutes, wherein the post-treatment solution comprises 23 to 25g/L of sodium dichromate and 5.5 to 7g/L of ammonium heptamolybdate; the temperature of the post-treatment solution is 48 ℃ to 55 ℃, and the pH of the post-treatment solution is 5.0 to 6.0.
The post-treatment solution also comprises sodium chloride with the concentration of 6.5-8 g/L.
The post-treatment solution also comprises glycol amine with the concentration of 2-3 ml/L.
The post-treatment solution is sodium dichromate with a concentration of 23.8g/L, ammonium heptamolybdate with a concentration of 6.4g/L, sodium chloride with a concentration of 6.8g/L and glycol amine with a concentration of 2.8ml/L, the temperature of the post-treatment solution is 49-51 ℃, and the post-treatment time is 15-20 minutes.
The chemical nickel plating is to place the test piece cleaned by the second water in the chemical nickel plating solution for 4 to 4.5 hours; the chemical nickel plating solution comprises 21.5-23.5g/L nickel sulfate, 23-25g/L sodium hypophosphite, 29-31ml lactic acid and 2.0-2.4ml/L propionic acid; the temperature of the chemical nickel plating solution is 85-92 ℃, and the pH of the chemical nickel plating solution is 4-4.5.
The chemical nickel plating solution also comprises 0.15-0.3mg/L of lead acetate.
The chemical nickel plating solution also comprises 0.4-0.6g/L of sodium fluoride.
The electroless nickel plating solution comprises nickel sulfate with the concentration of 22.5g/L, sodium hypophosphite with the concentration of 24g/L, lactic acid with the concentration of 30ml/L, propionic acid with the concentration of 2.2ml/L, sodium fluoride with the concentration of 0.5g/L and lead acetate with the concentration of 0.2mg/L, wherein the temperature of the electroless nickel plating solution is 86-88 ℃, and the pH value of the electroless nickel plating solution is 4.2-4.3.
A post-treatment solution for use in an acidic electroless nickel plating process, characterized by: the post-treatment solution comprises sodium dichromate in a concentration of 23-25g/L and ammonium heptamolybdate in a concentration of 5.5-7 g/L.
The post-treatment solution also comprises sodium chloride with the concentration of 6.5-8g/L and glycol amine with the concentration of 2-3 ml/L.
The invention has the advantages that:
the invention provides an acid chemical nickel plating method and a solution, the nickel plating method comprises a conventional chemical nickel plating process and is additionally provided with a post-treatment process after the chemical nickel plating, a very thin, compact and good-covering-performance chromate three-dimensional solid product film exists on the surface of a passivated metal after the metal is soaked by chromate, the plated metal or a base metal is oxidized in the chromate solution, metal ions enter the solution and release hydrogen, and the released hydrogen enables Cr to be oxidized6+Reduction to Cr3+Whereby the dissolution of the metal causes the pH at the interface between the metal and the solution to rise, causing Cr to form3+Possibly precipitated as colloidal chromium hydroxide, while Cr is in solution6+And metal ions are adsorbed in the colloid to participate in film formation; ammonium heptamolybdate as a complexing agent can make the release rate of chromium ions more uniform, and simultaneously has the function of controlling the pH of the solution, and controls the dissolution, coordination and dissociation reaction rate of metal in the sealing process together with sodium dichromate, so that a sealing thin layer formed on a coating is more uniform and compact, sodium chloride as a strong electrolyte has the function of accelerating the film formation, and ethylene glycol amine as a corrosion inhibitor forms an ethanolamine-molybdate system which is easy to combine with a nickel atom in a chemical nickel plating layer to form a coordination structure, thereby strengthening the passivation film formation function. Meanwhile, the solution adopted in the conventional chemical nickel plating is also adaptively adjusted, nickel sulfate is used as main salt, in the acidic nickel plating solution, when the concentration of nickel salt is lower than 10g/L, the deposition rate is increased along with the increase of the concentration of nickel salt, but when the concentration of nickel salt is too high (higher than 30g/L), the concentration of nickel salt is continuously increased, and the deposition rate is reduced on the contrary; sodium hypophosphite is a reducing agent, the deposition speed is high when the content is high, but the stability of the plating solution is poor, lactic acid is a complexing agent, and nickel ions (Ni)2+) Form stable complex, inhibit precipitation of nickel phosphite, and ensure stability of solutionSex; lead acetate is used as stabilizer, and adsorbs catalytically active particles or colloidal particles in the solution to prevent reduction of nickel on the particles, thereby effectively controlling nickel ions (Ni)2+) The reduction and the reduction reaction of (2) are carried out only on the plated surface; sodium fluoride is used as an accelerator to activate hypophosphite ions and improve the deposition rate; propionic acid is used as buffering agent, and hydrogen ions (H) in the solution are generated in the chemical nickel plating process+) The concentration is increased and the pH value is gradually reduced, and a certain amount of buffer is required to ensure the stability of the solution. The invention uses hypophosphite as a reducing agent, propionic acid as a buffering agent, lactic acid as a complexing agent, and main salt-nickel salt are added at the same time to deposit a chemical nickel-phosphorus alloy plating layer, and the sample after chemical nickel plating is subjected to post-treatment, so that the corrosion resistance of a chemical nickel plating layer is improved. The existing domestic process generally refers to HB/Z5071 chemical nickel plating process and quality inspection, and the neutral salt spray test for 48 hours is required.
Drawings
FIG. 1 is a graph showing the appearance of a test piece after a salt spray test for 500 hours by using the acid electroless nickel plating method provided by the present invention;
fig. 2 is a salt spray test report for fig. 1.
Detailed Description
The invention mainly aims at a post-treatment process method for improving the corrosion resistance of the acidic chemical nickel plating, the corrosion resistance of the acidic chemical nickel plating process is improved, the neutral salt spray test reaches 500 hours according to the requirements of ASTMB117, and the surface of a base metal is not corroded.
1 preparation of the test
1.1) test materials: the test piece material used in the test is low carbon steel 4130.
1.2) components and working conditions of the acidic chemical nickel plating solution:
21.5-23.5g/L of nickel sulfate (NiSO)4·7H2O); 23-25g/L sodium hypophosphite (NaH)2PO2·H2O); lactic acid (CH) of 29-31 ml/l3CHOHCOOH); 2.0-2.4ml/L propionic acid (CH)3CH2COOH); 0.4-0.6g/L sodium fluoride (NaF); 0.15-0.3mg/L lead acetate ((CH)3COO)2Pb·3H2O), temperature: 85-92 ℃, pH: 4-4.5, the time depends on the thickness.
1.3) composition of post-treatment solution and working conditions: 23-25g/L sodium dichromate (Na)2Cr2O7) (ii) a 5.5-7g/L ammonium heptamolybdate ((NH)4)6Mo7O24·4H2O); 6.5-8g/L sodium chloride (NaCl); 2-3ml/L glycol amine; temperature: 48-55 ℃, time: 10-25 minutes, pH: 5.0-6.0 (adjusted with ammonia).
2 analysis of mechanism
2.1) electroless nickel plating mechanism: chemical nickel plating with sodium hypophosphite as a reducing agent, and the obtained plating layer is a nickel-phosphorus alloy, and various theories about chemically depositing a Ni-P alloy plating layer exist, but the catalysis theory of C.Cutzeit is accepted by most people. This theory can be described by several procedures below.
(1) By the catalytic action of the metal, nascent atomic hydrogen is released:
H2PO2 -→PO2 -+2(H)
PO2 -+H2O→HPO3 2-+H+
or H2PO2 -+H2O→HPO3 2-+H++2[H]
(2) The nascent atomic hydrogen is adsorbed on the catalytic metal surface to activate it, reducing the nickel cations in the plating solution, depositing metallic nickel on the catalytic metal surface:
Ni2++2[H]→Ni0+2H-
(3) reduction of hypophosphite to phosphorus by nascent atomic hydrogen on the catalytic metal surface; at the same time, the hypophosphite is decomposed by the catalytic action, forming phosphorous acid and molecular hydrogen:
H2PO2 -+[H]→H2O+OH-+P0
H2PO2 -+H2O→H[HPO2]-+H2
thus, the nickel salt is reduced, the hypophosphite is oxidized, and the total reaction formula is as follows:
Ni2++H2PO2 -+H2O→HPO3 2-+3H++Ni0
(4) the nickel atoms and the phosphorus atoms co-deposit and form a nickel-phosphorus alloy layer.
Ni + P → Ni-P alloy (solid solution or amorphous)
In the acidic nickel plating solution, when the nickel salt is lower than 10g/L, the deposition rate is increased along with the increase of the nickel salt concentration, but when the nickel salt is too high (more than 30g/L), the nickel salt concentration is continuously increased, and the deposition rate is reduced; sodium hypophosphite is a reducing agent, the deposition speed is high when the content is high, but the stability of the plating solution is poor, lactic acid is a complexing agent, and nickel ions (Ni)2+) A stable complex is formed, the precipitation of the nickel phosphite is inhibited, and the stability of the solution is ensured; lead acetate is used as stabilizer, and adsorbs catalytically active particles or colloidal particles in the solution to prevent reduction of nickel on the particles, thereby effectively controlling nickel ions (Ni)2+) The reduction and the reduction reaction of (2) are carried out only on the plated surface; sodium fluoride is used as an accelerator to activate hypophosphite ions and improve the deposition rate; propionic acid is used as buffering agent, and hydrogen ions (H) in the solution are generated in the chemical nickel plating process+) The concentration is increased and the pH value is gradually reduced, and a certain amount of buffer is required to ensure the stability of the solution.
2.2) analysis of the mechanism of the aftertreatment solution
After the metal is soaked by chromate, a layer of very thin and compact chromate three-dimensional solid product film with good covering performance exists on the surface of the passivated metal. The coating metal or base metal is oxidized in chromate solution, the metal ions enter the solution and release hydrogen, the released hydrogen reacts Cr6+Reduction to Cr3+Whereby the dissolution of the metal causes the pH at the interface between the metal and the solution to rise, causing Cr to form3+Possibly precipitated as colloidal chromium hydroxide, while Cr is in solution6+And metal ions are adsorbed in the colloid to participate in film formation. Ammonium heptamolybdate as a complexing agent can release chromium ions at a more uniform rateThe solution is uniform, the pH value of the solution is controlled, the solution and sodium dichromate jointly control the dissolution, coordination and dissociation reaction rate of metal in the sealing process, so that a sealing thin layer formed on a coating is more uniform and compact, sodium chloride has the function of accelerating the film formation by being used as a strong electrolyte, ethylene glycol amine is used as a corrosion inhibitor to form an ethanolamine-molybdate system, and the ethanolamine-molybdate system is easy to combine with a nickel atom in a chemical nickel coating to form a coordination structure, so that the passivation film formation function is enhanced.
3 test procedure
3.1) protocol:
the experiment is carried out by adopting an acid chemical nickel plating method, the chemical reagent is an analytically pure reagent produced by Tianjin Chengyuan chemical Limited company, and the components and the process conditions are as follows: 22.5g/L of nickel sulfate, 24g/L of sodium hypophosphite, 30ml/L of lactic acid, 2.2ml/L of propionic acid, 0.5g/L of sodium fluoride, 0.2mg/L of lead acetate, and water for preparation: deionized water, temperature: 86-88 ℃, pH: 4.2-4.3, and the time is 4-5 hours. In the test, the chemical nickel plating is carried out in a plastic barrel, and a water bath heating method is used for ensuring that the solution cannot be locally overheated unevenly when heated.
The post-treatment solution comprises the following components and process conditions: 23.8g/L of sodium dichromate, 6.4g/L of ammonium heptamolybdate, 6.8g/L of sodium chloride, 2.8ml/L of glycol amine, temperature: 49-51 ℃, time: 15-20 minutes.
The neutral salt spray test was carried out according to astm b 117: CZ-200B type salt fog box, 50g/L sodium chloride (NaCl), pH 6.5-7.2; air pressure 10.0N/cm2The spraying amount is 1.0-2.0mL/(80 cm)2·h-1) The salt spray temperature is (35 +/-1) DEG C, and the test temperature is (35 +/-1) DEG C; and taking out the sample when the first rust spot appears on the surface of the sample, and recording the corrosion time.
3.2) process flow:
1) and (4) acceptance: the surface of the test piece should have no defects such as rust, burr, dirt, oil stain, metal chip and mechanical damage (pressure injury, bruise and scratch), and if the test piece has serious defects, the test piece should be returned and taken again, and the sharp edge of the test piece should have no burr.
2) Mounting and hanging: the test piece is hung by a copper wire, and the surface of the test piece is not scratched or bruised during hanging.
3) Electrolytic degreasing: solutionThe components and the process conditions of the liquid are as follows: 20-40g/L of sodium hydroxide; 20-40g/L of sodium carbonate; 20-40g/L of sodium phosphate; 3-5g/L of sodium silicate; the temperature is 70-90 ℃, the time is 10-30 minutes, and the current density is 3-10A/dm2
4) Cleaning: cleaning in hot water of 50 deg.C or lower for 0.3-3 min, cleaning in flowing cold water for 0.3-3 min, checking whether the water film is continuous for 30 s, and if so, continuing the next procedure, and if not, cleaning to remove oil again until the water film is continuous. ("Water film continuous" is defined as a continuous water film surface that remains at least 30 seconds after being sprayed or rinsed with fresh water at a temperature of less than 100 ℉ (38 deg.C)
5) Soaking and polishing: the components and the process conditions of the solution are as follows: 500-600g/L hydrochloric acid; the temperature is room temperature; the time is 1-3 minutes.
6) Cleaning: washing in flowing cold water for 0.3-3 min. And checking whether the water film is continuous for 30 seconds, if so, continuing the following steps, and if not, re-performing oil removal cleaning until the water film is continuous.
7) Chemical nickel plating: the solution components and the process conditions are as follows: 22.5g/L of nickel sulfate, 24g/L of sodium hypophosphite, 30ml/L of lactic acid, 2.2ml/L of propionic acid, 0.5g/L of sodium fluoride and 0.2mg/L of lead acetate, and preparing a solution by using water: deionized water, temperature: 86-88 ℃, pH: 4.2 to 4.3, and the time is 4 to 4.5 hours. Note: the chemical nickel plating solution must be prepared by deionized water, when the pH value is adjusted by sodium hydroxide, the chemical nickel plating solution is diluted to about 5-6 and is slowly added under the condition of continuous stirring; the pH value of the solution is not allowed to be adjusted in the chemical nickel plating process; adjusting the pH value of the newly prepared solution to the upper limit at the beginning, and adjusting the pH value to a process range before chemical nickel plating; the test piece with the oil stain removed completely is placed into a plastic barrel which is heated to the working temperature in a thermostatic water bath, the test piece is shaken continuously after being placed in the groove, the coating is ensured to be uniform, and small catalytic metal fragments such as scrap iron or nickel scraps are not allowed to be brought in, because the fragments are to become active centers in the bath solution, the natural decomposition of the bath solution is easily triggered.
8) Cleaning: washing in flowing cold water for 0.3-3 min. Note: cleaning the test piece after chemical nickel plating, keeping the surface of the test piece wet, and immediately transferring to the next working procedure.
9) And (3) post-treatment: the solution components and the process conditions are as follows: 23.8g/L of sodium dichromate, 6.4g/L of ammonium heptamolybdate, 6.8g/L of sodium chloride, 2.8ml/L of glycol amine, temperature: 49-51 ℃, time: 15-20 minutes.
10) Cleaning: washing in hot water at 50 deg.C or higher for 0.3-3 min.
11) And (3) drying: drying with clean compressed air.
4 results of the test
According to the test flow, the prepared test piece is cleaned and dried, and then is sent into a neutral salt spray test box. FIG. 1 is a graph of the appearance of a test piece after 500 hours of salt spray test and a report of the qualification of the 500 hours of salt spray test. According to the tests, the corrosion resistance of the acid chemical nickel plating can be greatly improved by the process method, the neutral salt spray test reaches 500 hours, and the surface of the metal matrix is not corroded.

Claims (10)

1. An acid chemical nickel plating method comprises the steps of preparing a test piece, hanging, electrolyzing and deoiling, washing with water for the first time, soaking and polishing, washing with water for the second time and chemical nickel plating, and is characterized in that: the acid chemical nickel plating method also comprises a third time of water cleaning and post-treatment after chemical nickel plating; the post-treatment is to place the test piece after the chemical nickel plating and the third water cleaning in a post-treatment solution for 10 to 25 minutes, wherein the post-treatment solution comprises 23 to 25g/L of sodium dichromate and 5.5 to 7g/L of ammonium heptamolybdate; the temperature of the post-treatment solution is 48 ℃ to 55 ℃, and the pH of the post-treatment solution is 5.0 to 6.0.
2. An acidic electroless nickel plating process according to claim 1, characterized in that: the post-treatment solution also includes sodium chloride at a concentration of 6.5-8 g/L.
3. An acidic electroless nickel plating process according to claim 2, characterized in that: the post-treatment solution also comprises glycol amine with the concentration of 2-3 ml/L.
4. An acidic electroless nickel plating process according to claim 3, characterized in that: the post-treatment solution is sodium dichromate with the concentration of 23.8g/L, ammonium heptamolybdate with the concentration of 6.4g/L, sodium chloride with the concentration of 6.8g/L and glycol amine with the concentration of 2.8ml/L, the temperature of the post-treatment solution is 49-51 ℃, and the post-treatment time is 15-20 minutes.
5. An acidic electroless nickel plating process according to claim 1, 2, 3 or 4, characterized in that: the chemical nickel plating is to place the test piece cleaned by the second water in the chemical nickel plating solution for 4 to 4.5 hours; the chemical nickel plating solution comprises 21.5-23.5g/L nickel sulfate, 23-25g/L sodium hypophosphite, 29-31ml lactic acid and 2.0-2.4ml/L propionic acid; the temperature of the chemical nickel plating solution is 85-92 ℃, and the pH of the chemical nickel plating solution is 4-4.5.
6. An acidic electroless nickel plating process according to claim 5, characterized in that: the chemical nickel plating solution also comprises 0.15-0.3mg/L of lead acetate.
7. An acidic electroless nickel plating process according to claim 6, characterized in that: the chemical nickel plating solution also comprises 0.4-0.6g/L of sodium fluoride.
8. An acidic electroless nickel plating process according to claim 7, characterized in that: the chemical nickel plating solution comprises nickel sulfate with the concentration of 22.5g/L, sodium hypophosphite with the concentration of 24g/L, lactic acid with the concentration of 30ml/L, propionic acid with the concentration of 2.2ml/L, sodium fluoride with the concentration of 0.5g/L and lead acetate with the concentration of 0.2mg/L, the temperature of the chemical nickel plating solution is 86-88 ℃, and the pH value of the chemical nickel plating solution is 4.2-4.3.
9. A post-treatment solution for use in an acidic electroless nickel plating process, characterized by: the post-treatment solution comprises sodium dichromate in a concentration of 23-25g/L and ammonium heptamolybdate in a concentration of 5.5-7 g/L.
10. The post-treatment solution of claim 9, characterized in that: the post-treatment solution also comprises sodium chloride with the concentration of 6.5-8g/L and glycol amine with the concentration of 2-3 ml/L.
CN201911158608.6A 2019-11-22 2019-11-22 Acidic chemical nickel plating method and solution Withdrawn CN110965053A (en)

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Cited By (1)

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CN113718248A (en) * 2021-09-01 2021-11-30 筑磊半导体技术(上海)有限公司 Cleaning method of semiconductor process pipeline

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