CN115287638A - Low-temperature chemical nickel liquid medicine, preparation method and plating method - Google Patents

Low-temperature chemical nickel liquid medicine, preparation method and plating method Download PDF

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Publication number
CN115287638A
CN115287638A CN202210923964.8A CN202210923964A CN115287638A CN 115287638 A CN115287638 A CN 115287638A CN 202210923964 A CN202210923964 A CN 202210923964A CN 115287638 A CN115287638 A CN 115287638A
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concentration
controlled
chemical nickel
low
temperature
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高升
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Dongguan Zhongrui Surface Treatment Co ltd
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Dongguan Zhongrui Surface Treatment Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C18/00—Chemical 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
    • C23C18/16—Chemical 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
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C18/00—Chemical 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
    • C23C18/16—Chemical 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1675—Process conditions
    • C23C18/168—Control of temperature, e.g. temperature of bath, substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C18/00—Chemical 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
    • C23C18/16—Chemical 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1675—Process conditions
    • C23C18/1683—Control of electrolyte composition, e.g. measurement, adjustment

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

Abstract

A low-temperature chemical nickel liquid medicine, a preparation method and a plating method comprise an aqueous solution, wherein main salt, a complexing agent, an activating agent and a reducing agent are added into the aqueous solution, the concentration of the main salt is controlled to be 30-49g/L, the concentration of the complexing agent is controlled to be 40-50g/L, the concentration of the activating agent is controlled to be 30-60g/L, the concentration of the reducing agent is controlled to be 8-15g/L, the pH value of the aqueous solution is controlled to be 7.6-8.6, and the use temperature is controlled to be 40-50 ℃. The invention can realize nickel plating treatment in a low-temperature environment, can reduce the potential safety hazard of high-temperature production compared with the high-temperature chemical nickel in the traditional plastic industry, can effectively reduce ammonia volatilization under the low-temperature condition, and reduces the addition of liquid medicine and the production cost.

Description

Low-temperature chemical nickel liquid medicine, preparation method and plating method
Technical Field
The invention relates to a chemical liquid medicine, in particular to a low-temperature chemical nickel liquid medicine capable of reducing energy consumption and production accidents, a preparation method and a plating method.
Background
Electroless nickel plating is a process for depositing a layer of nickel on the surface of a metallic article by redox action without the aid of an external current. Used for improving corrosion resistance and wear resistance, and increasing luster and beauty. It is suitable for bright nickel plating of tubular or complex-shaped small parts without polishing.
Chinese patent with publication number CN108220932A discloses an electroless nickel plating solution, which comprises the following components in volume ratio: chemical nickel A solution: chemical nickel B solution: water =1, pH adjusted to 4.5-5.5 with ammonia or acetic acid; the chemical nickel A liquid comprises the following components in mass concentration: 200-400g/L of nickel sulfate hexahydrate, 20-40g/L of potassium citrate, 3-10g/L of potassium acetate, 5-15g/L of 2-hydroxypropionic acid, 10-50mg/L of sodium dodecyl sulfate, 10-20mg/L of cysteine hydrochloride, 3-8mg/L of 7-ethyl bicyclic oxazoline and 3-8mg/L of bromochlorophene; the chemical nickel B liquid comprises the following components in mass concentration: 50-80g/L of potassium citrate, 30-70g/L of potassium acetate, 80-120g/L of sodium hypophosphite, 10-30g/L of 2-hydroxypropionic acid and 5-15g/L of saccharin sodium. In the above chemical nickel solution, because holistic pH value is lower, need higher temperature just can carry out effective reaction, need reach the temperature more than 60 degrees centigrade usually, moreover, its pH value is acid environment, is unfavorable for the reaction of six water nickel sulfate, in actual production, because the temperature that needs is higher, the accident risk takes place easily, also can the increase consumption.
Disclosure of Invention
The invention aims to provide a low-temperature chemical nickel liquid medicine, a preparation method and a plating method.
In order to solve the technical problem, the invention adopts the following technical scheme:
a low-temperature chemical nickel liquid medicine comprises an aqueous solution, wherein main salt, a complexing agent, an activating agent and a reducing agent are added into the aqueous solution, the concentration of the main salt is controlled to be 30-49g/L, the concentration of the complexing agent is controlled to be 40-50g/L, the concentration of the activating agent is controlled to be 30-60g/L, the concentration of the reducing agent is controlled to be 8-15g/L, the pH value of the aqueous solution is controlled to be 7.6-8.6, and the use temperature is controlled to be 40-50 ℃.
As a further improvement, the main salt is nickel sulfate.
As a further improvement, the complexing agent is trisodium citrate dihydrate, and the concentration of the complexing agent is greater than that of the main salt.
As a further improvement, the activator is sodium chloride.
As a further improvement, the reducing agent is sodium hypophosphite.
As a further improvement, when the pH value of the aqueous solution is adjusted, the pH value is controlled by adding a pH adjusting agent so that the pH value is maintained at 7.6 to 8.6.
As a further improvement, the pH regulator is sodium hydroxide aqueous solution or ammonia water.
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution between 7.6 and 8.6, wherein the concentration of the nickel sulfate is controlled to be 30 to 50g/L, the concentration of the trisodium citrate dihydrate is controlled to be 40 to 50g/L, the concentration of the sodium chloride is controlled to be 30 to 60g/L, and the concentration of the sodium hypophosphite is controlled to be 8 to 15g/L.
A plating method of a low-temperature chemical nickel liquid medicine comprises the following steps:
cleaning the base material;
putting the cleaned substrate into a low-temperature chemical nickel liquid medicine, keeping the temperature between 40 and 50 ℃, and soaking for a set time;
taking out the substrate, rinsing with clear water, and drying to complete plating.
The cleaning comprises hot alkali liquid oil removal, hot water washing, acid washing and activation.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the alkaline aqueous solution is adopted, and meanwhile, the low-temperature environment of 40-50 ℃ is combined, so that the actual working environment of the chemical nickel liquid medicine is realized, the traditional working environment generally higher than 80 ℃ is not needed, the potential safety hazard caused by the high-temperature environment can be avoided, and the safety and the reliability of production are improved.
2. Because the process is carried out at low temperature, the volatilization of ammonia water can be effectively reduced at low temperature, and the addition and production cost of liquid medicine is reduced.
3. The content of each component is strictly controlled to ensure the stability of the nickel layer crystal.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to further understand the features and technical means of the invention and achieve specific objects and functions.
The invention discloses a low-temperature chemical nickel liquid medicine which comprises an aqueous solution, wherein main salt, a complexing agent, an activating agent and a reducing agent are added into the aqueous solution, the concentration of the main salt is controlled to be 30-49g/L, the concentration of the complexing agent is controlled to be 40-50g/L, the concentration of the activating agent is controlled to be 30-60g/L, the concentration of the reducing agent is controlled to be 8-15g/L, the pH value of the aqueous solution is controlled to be 7.6-8.6, and the use temperature is controlled to be 40-50 ℃.
Wherein the main salt is nickel sulfate; the complexing agent is trisodium citrate dihydrate, and the concentration of the complexing agent is greater than that of the main salt; the activating agent is sodium chloride; the reducing agent is sodium hypophosphite; when the pH value of the aqueous solution is adjusted, a pH regulator is added for control, so that the pH value is kept between 7.6 and 8.6, and the pH regulator is a sodium hydroxide aqueous solution or ammonia water.
The complexing agent can effectively prevent the precipitation in the plating solution, and the service life of the plating solution is prolonged to a certain extent; in addition, the complexing agent can effectively control the concentration of metal ions in the solution and maintain the balance of a solution system; finally, the complexing agent can improve the crystallization condition of the coating, so that the crystallization layer is uniform and fine. Further, it has been found through a number of experiments that the complexing agent, which is trisodium citrate dihydrate and set at a concentration greater than that of the main salt, can be used as a conductive salt and a complexing agent in electroless nickel plating to prevent nickel from forming a hydroxide precipitate.
Example one
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 7.6, controlling the concentration of nickel sulfate at 30g/L, controlling the concentration of trisodium citrate dihydrate at 40g/L, controlling the concentration of sodium chloride at 30g/L and controlling the concentration of sodium hypophosphite at 8g/L. The pH was adjusted by adding aqueous sodium hydroxide solution. The temperature environment used was 40 ℃.
Example two
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.0, controlling the concentration of nickel sulfate at 40g/L, controlling the concentration of trisodium citrate dihydrate at 45g/L, controlling the concentration of sodium chloride at 45g/L and controlling the concentration of sodium hypophosphite at 10g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 45 ℃.
EXAMPLE III
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to ensure that the pH value of the aqueous solution is kept at 8.6, the concentration of nickel sulfate is controlled at 49g/L, the concentration of trisodium citrate dihydrate is controlled at 50g/L, the concentration of sodium chloride is controlled at 60g/L, and the concentration of sodium hypophosphite is controlled at 15g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 50 ℃.
Example four
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.2, controlling the concentration of nickel sulfate at 38g/L, controlling the concentration of trisodium citrate dihydrate at 44g/L, controlling the concentration of sodium chloride at 45g/L and controlling the concentration of sodium hypophosphite at 11g/L. The pH was adjusted by adding aqueous sodium hydroxide solution. The temperature environment used was 50 ℃.
EXAMPLE five
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to ensure that the pH value of the aqueous solution is kept at 8.3, the concentration of the nickel sulfate is controlled at 44g/L, the concentration of the trisodium citrate dihydrate is controlled at 46g/L, the concentration of the sodium chloride is controlled at 55g/L, and the concentration of the sodium hypophosphite is controlled at 12g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 48 ℃.
EXAMPLE six
A preparation method of a low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.0, controlling the concentration of nickel sulfate at 47g/L, controlling the concentration of trisodium citrate dihydrate at 48g/L, controlling the concentration of sodium chloride at 35g/L and controlling the concentration of sodium hypophosphite at 14g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 45 ℃.
When plating, cleaning the base piece; putting the cleaned substrate into a low-temperature chemical nickel liquid medicine, keeping the temperature between 40 and 50 ℃, and soaking for a set time; taking out the substrate, rinsing with clear water, and drying to complete plating.
In the invention, nickel sulfate is adopted to realize the reaction of chemical nickel by matching with alkaline PH environment. Higher main salt content in a chemical nickel liquid medicine system can obtain higher efficiency, but other corresponding coordination liquid medicines also require higher content, and the internal stress of the crystal of the plating layer obtained at higher speed is higher, so that the quality of the plating layer is influenced, and the concentration of nickel sulfate is controlled to be 30-50G/L, so that the stability of the crystal of the nickel layer is ensured.
The pH value of the aqueous solution is 7.6-8.6. Easily soluble in water has excellent solubility properties, and the solubility increases with increasing water temperature. Has good ph regulation and buffering performance. Sodium citrate is a weak acid strong base salt, and is particularly suitable for being applied to occasions where the pH is not suitable for changing in a large range. In addition, the sodium citrate also has excellent retarding performance and stability. Trisodium citrate dihydrate is used as a conductive salt and complexing agent in electroless nickel plating to prevent the nickel from forming a hydroxide precipitate.
Sodium chloride is used as an inorganic ionic compound, and the chemical formula of NaCl plays a role in activating the anode in plating solution, so that nickel ions are prevented from being passivated, and the activity of the liquid medicine is improved.
The sodium hypophosphite is used as a source of nickel and hypophosphite, one advantage is that the existence of sulfate ions is avoided, the accumulation amount of alkali metal ions can reach the minimum value when nickel salt is supplemented, the cost can be reduced, and the method has the advantages of easy control of plating solution, good corrosion resistance of a plating layer and the like. Main and side reactions are formed during the whole reaction process:
main reaction: ni 2 ++2H 2 PO 2 -+2H 2 O→Ni+2HPO 32 -+4H++H 2
Side reaction: 4H 2 PO 2 -→2HPO 32 -+2P+2H 2 O+H 2 。
Comparative example 1
Corresponding to the first embodiment, the preparation method of the low-temperature chemical nickel liquid comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 5.6, controlling the concentration of nickel sulfate at 30g/L, controlling the concentration of trisodium citrate dihydrate at 40g/L, controlling the concentration of sodium chloride at 30g/L and controlling the concentration of sodium hypophosphite at 8g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 40 ℃. The difference from the first example is that the pH of the aqueous solution is different.
Comparative example No. two
Corresponding to the second embodiment, the preparation method of the low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel chloride, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to ensure that the pH value of the aqueous solution is kept at 8.0, the concentration of nickel sulfate is controlled at 40g/L, the concentration of trisodium citrate dihydrate is controlled at 45g/L, the concentration of sodium chloride is controlled at 45g/L, and the concentration of sodium hypophosphite is controlled at 10g/L. The pH was adjusted by adding aqueous sodium hydroxide solution. The temperature environment used was 45 ℃. The difference from the second example is that nickel chloride is used as the main salt.
Comparative example No. three
Corresponding to the third embodiment, the preparation method of the low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium borohydride and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.6, controlling the concentration of nickel sulfate at 49g/L, controlling the concentration of trisodium citrate dihydrate at 50g/L, controlling the concentration of sodium chloride at 60g/L and controlling the concentration of sodium hypophosphite at 15g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 50 ℃. The difference from the example is that sodium borohydride is used as the reducing agent.
Comparative example No. four
Corresponding to the fourth embodiment, the preparation method of the low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.2, controlling the concentration of nickel sulfate at 20g/L, controlling the concentration of trisodium citrate dihydrate at 25g/L, controlling the concentration of sodium chloride at 45g/L and controlling the concentration of sodium hypophosphite at 11g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 40 ℃. In contrast to example four, the difference is the amount of nickel sulfate and trisodium citrate dihydrate.
Comparative example five
Corresponding to the fifth embodiment, the preparation method of the low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.3, controlling the concentration of nickel sulfate at 55g/L, controlling the concentration of trisodium citrate dihydrate at 70g/L, controlling the concentration of sodium chloride at 80g/L and controlling the concentration of sodium hypophosphite at 12g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 48 ℃. The difference from the fifth embodiment is that the ratio of the nickel sulfate, the trisodium citrate dihydrate and the sodium chloride is different.
Comparative example six
Corresponding to the sixth embodiment, the preparation method of the low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel chloride, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution at 8.0, controlling the concentration of nickel chloride at 60g/L, controlling the concentration of trisodium citrate dihydrate at 40g/L, controlling the concentration of sodium chloride at 35g/L and controlling the concentration of sodium hypophosphite at 14g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 45 ℃. The difference from the embodiment is that the main salt adopts nickel chloride, the dosage ratio of the nickel chloride and the trisodium citrate dihydrate is different, and the concentration of the trisodium citrate dihydrate as the complexing agent is less than that of the nickel chloride as the main salt.
Comparative example seven
Corresponding to the sixth embodiment, the preparation method of the low-temperature chemical nickel liquid medicine comprises the following steps:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, oxalic acid and a pH regulator into water, and fully dissolving so that the pH value of the aqueous solution is kept at 8.0, the concentration of the nickel sulfate is controlled at 47g/L, the concentration of the trisodium citrate dihydrate is controlled at 48g/L, the concentration of the sodium chloride is controlled at 35g/L, and the concentration of the oxalic acid is controlled at 14g/L. The pH was adjusted by adding aqueous sodium hydroxide. The temperature environment used was 45 ℃. The reducing agent is oxalic acid.
The prepared liquid medicine is respectively subjected to plating treatment.
From comparative example 1, it was confirmed that the aqueous solution was adjusted to a value of 5.6 of the compatibility, and an effective reaction could not be performed at a low temperature range of 40 to 50 ℃ and an effective plating process could not be performed.
The nickel liquid medicine of the second embodiment is subjected to plating treatment, and the nickel liquid medicine is subjected to plating treatment with the nickel liquid medicine prepared in the comparison document 2, and tests show that the stress of the nickel plated layer obtained after the nickel liquid medicine of the comparison document 2 is plated is obviously greater than the stress of the nickel liquid medicine formed by nickel sulfate in the second embodiment.
In the third embodiment, sodium hypophosphite is adopted as the reducing agent, so that the existence of sulfate ions is avoided; in the third comparative example, sodium borohydride is adopted, and tests show that obvious sulfate ions exist, so that the subsequent plating process is influenced, and the stress in the nickel layer is influenced.
In comparative examples four and five, when the ratio of the amounts of the respective components is more or less than the ratio defined in the present invention, it was found through tests that the effect of the reaction is very retarded in the low temperature range.
In the sixth comparative example, nickel chloride was used as the main salt, and the amount of complexing agent was less than the concentration of the main salt, which resulted in formation of a large amount of hydroxide precipitate, which was not favorable for the preparation process.
In comparative example seven, oxalic acid was used as the reducing agent, and the reducing effect was significantly worse than that of sodium hypophosphite in the present invention in the entire formulation.
In the invention, the plating process can be effectively realized by combining a low-temperature application system at 40-50 ℃ and a pH value of 7.6-8.6.
Although the present invention has been described in detail with reference to the embodiments, it will be apparent to those skilled in the art that modifications, equivalents, improvements, and the like can be made in the technical solutions of the foregoing embodiments or in some of the technical features of the foregoing embodiments, but those modifications, equivalents, improvements, and the like are all within the spirit and principle of the present invention.

Claims (10)

1. A low-temperature chemical nickel liquid medicine is characterized by comprising an aqueous solution, wherein main salt, a complexing agent, an activating agent and a reducing agent are added into the aqueous solution, the concentration of the main salt is controlled to be 30-49g/L, the concentration of the complexing agent is controlled to be 40-50g/L, the concentration of the activating agent is controlled to be 30-60g/L, the concentration of the reducing agent is controlled to be 8-15g/L, the pH value of the aqueous solution is controlled to be 7.6-8.6, and the use temperature is controlled to be 40-50 ℃.
2. The cryogenic chemical nickel bath of claim 1, wherein the primary salt is nickel sulfate.
3. The cryogenic chemical nickel reagent as claimed in claim 1, wherein the complexing agent is trisodium citrate dihydrate, and the concentration of the complexing agent is greater than that of the main salt.
4. The cryogenic chemical nickel bath of claim 1, wherein the activator is sodium chloride.
5. The cryogenic chemical nickel reagent of claim 1, wherein the reducing agent is sodium hypophosphite.
6. The low-temperature chemical nickel solution as claimed in claim 1, wherein the pH value of the aqueous solution is controlled to be 7.6 to 8.6 by adding a pH regulator.
7. The low-temperature chemical nickel solution as claimed in claim 6, wherein the pH regulator is sodium hydroxide aqueous solution or ammonia water.
8. The preparation method of the low-temperature chemical nickel liquid medicine is characterized by comprising the following steps of:
adding nickel sulfate, trisodium citrate dihydrate, sodium chloride, sodium hypophosphite and a pH regulator into water, and fully dissolving to keep the pH value of the aqueous solution between 7.6 and 8.6, wherein the concentration of the nickel sulfate is controlled to be 30 to 50g/L, the concentration of the trisodium citrate dihydrate is controlled to be 40 to 50g/L, the concentration of the sodium chloride is controlled to be 30 to 60g/L, and the concentration of the sodium hypophosphite is controlled to be 8 to 15g/L.
9. The method for plating the low-temperature chemical nickel liquid according to claim 8, comprising the steps of:
cleaning the base piece;
putting the cleaned substrate into a low-temperature chemical nickel liquid medicine, keeping the temperature between 40 and 50 ℃, and soaking for a set time;
taking out the substrate, rinsing with clear water, and drying to complete plating.
10. The method of claim 9, wherein the cleaning comprises hot alkaline degreasing, hot water washing, acid washing, and activation.
CN202210923964.8A 2022-08-02 2022-08-02 Low-temperature chemical nickel liquid medicine, preparation method and plating method Pending CN115287638A (en)

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CN105200761A (en) * 2015-10-13 2015-12-30 四川大学 Palladium-free activation chemical nickel-plating method for electromagnetic shielding polyphenylene sulfide fiber
CN113502467A (en) * 2021-07-09 2021-10-15 贵州理工学院 Nickel-phosphorus plated part and low-temperature neutral simplified chemical nickel-phosphorus plating method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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