Surface nickel plating process for quartz glass

By pretreating the surface of quartz glass and optimizing the electroless nickel plating process, the problems of insufficient bonding force and unevenness of the nickel layer are solved, and the formation of a high-performance nickel layer is achieved, and it meets environmental protection standards.

CN119663256AInactive Publication Date: 2025-03-21ZHENJIANG JINXING SURFACE ENG TECH CO LTD
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Patent Information

Application Number
CN202411761103.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-03
Publication Date
2025-03-21
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

In the process of nickel-surface nickel-based surface, the prior art has problems such as insufficient bonding force between the nickel layer and the quartz glass substrate and inhomogeneity of the nickel layer, resulting in limited functional performance.

Method used

Pretreatment steps include surface cleaning, coarse treatment, sensitization treatment and activation treatment, followed by electroless nickel plating, and finally waste liquid treatment to achieve uniform adhesion and efficient precipitation of the nickel layer.

Benefits of technology

The bonding force between the nickel layer and quartz glass is significantly improved, the uniformity and high performance of the nickel layer are achieved, and it has good conductivity and corrosion resistance, and it complies with environmental protection standards.

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Abstract

The invention discloses a surface nickel plating process for quartz glass, and aims to improve the adhesive force, uniformity and functional performance of a nickel plating layer, simplify the process flow and meet the environmental protection requirement. The process comprises the following steps: firstly, cleaning and roughening the surface of quartz glass, removing surface impurities through a 2% sodium hydroxide solution and a 10% hydrofluoric acid solution, and forming a microscopic rough structure; then treating in a sensitizing solution composed of stannous chloride and hydrochloric acid to enable the surface to adsorb stannous ions; then treating in an activating solution composed of palladium chloride and hydrochloric acid to form a catalytic active layer; then carrying out nickel plating reaction in a chemical nickel plating solution with the temperature of 85 DEG C and the pH value of 4.5, wherein the thickness of a plating layer is 5-10 microns; and finally, the waste liquid is neutralized and flocculated to realize environment-friendly discharge. The process is simple and convenient to operate, and the generated nickel coating is uniform and compact, has excellent conductivity and corrosion resistance, and can be widely applied to the fields of electronics, optics and chemistry.
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Description

Technical Field

[0001] The invention relates to a nickel surface treatment process, and more particularly to a nickel surface treatment process for quartz glass. Background Art

[0002] Quartz glass is an inorganic non-metallic material with excellent properties. It is widely used in optics, electronics, chemicals and high-temperature environments. Due to its high hardness, high melting point, low thermal expansion coefficient, chemical corrosion resistance and excellent optical transmittance, quartz glass is widely used in the manufacture of optical components, semiconductor substrates, high-temperature containers, etc. However, the chemical inertness and smooth surface of quartz glass make it difficult to functionalize its surface, limiting its application in certain specific fields.

[0003] Nickel is a metal material with excellent performance, good corrosion resistance, electrical conductivity and catalytic activity, so it has important application value in the electronics industry, optical thin films and electrochemical fields. Nickel plating on the surface of quartz glass can significantly enhance its surface conductivity and give it multiple functions such as anti-oxidation, anti-corrosion and optical regulation, thereby expanding the application of quartz glass in special fields.

[0004] At present, the processes for nickel coating on the surface of quartz glass mainly include chemical nickel plating, electrolytic nickel plating and other methods. However, these traditional methods have the following technical difficulties in the process of nickel coating on the surface of quartz glass:

[0005] ① Due to the chemical inertness of the quartz glass surface, it is difficult to form a strong bond between the nickel layer and the quartz glass substrate, which can easily lead to the nickel layer falling off or failure.

[0006] ② The nickel plating layer is prone to unevenness on the surface of quartz glass, resulting in limited functional performance. Summary of the invention

[0007] In order to solve the above problems, this patent proposes an innovative nickel surface treatment process for quartz glass, which aims to improve the adhesion between the nickel layer and the quartz glass substrate, while simplifying the process, reducing costs and achieving green environmental protection. The specific solution is as follows:

[0008] A process for nickel coating the surface of quartz glass, the process comprising the following steps:

[0009] S1. Pre-treat the quartz glass surface:

[0010] S2, sensitization treatment: immerse the quartz glass in the sensitizing solution, control the temperature to 25°C; immerse for 5 minutes, so that the surface of the quartz glass evenly adsorbs stannous ions; rinse with deionized water after sensitization to prevent the active layer from falling off;

[0011] S3, activation treatment: immerse the sensitized quartz glass in activation solution, control the temperature to 25°C; immerse for 3 minutes, so that a catalytic active layer is formed on the surface of the quartz glass; rinse with deionized water until there is no residual liquid on the surface;

[0012] S4, chemical nickel plating: prepare chemical nickel plating solution; adjust pH value to 4.5; maintain temperature at 85°C; immerse activated quartz glass in chemical nickel plating solution, stir evenly, nickel plating time is 30 minutes; nickel plating layer thickness is 5-10μm; rinse with deionized water after nickel plating, and dry in a hot air drying oven at 60°C for 20 minutes;

[0013] S5. Waste liquid treatment: Use alkaline solution to neutralize the acidic waste liquid and adjust the pH to 7-8; add flocculant to precipitate metal ions; the precipitate is dried and then centrally treated, and the wastewater is discharged after passing the test.

[0014] Furthermore, the surface pretreatment of S1 quartz glass includes the following steps: cleaning the quartz glass with deionized water to remove dust and impurities on the surface; ultrasonic cleaning at 40° C. for 10 minutes in a 2% by volume sodium hydroxide solution; and rinsing with deionized water until neutral.

[0015] Furthermore, the sensitizing solution in S2 consists of 10 g / L stannous chloride and 40 mL / L hydrochloric acid.

[0016] Furthermore, the activation solution in S3 is composed of 1 g / L palladium chloride and 30 mL / L hydrochloric acid.

[0017] Furthermore, S4 is composed of 1 g / L of palladium chloride and 30 mL / L of hydrochloric acid.

[0018] Furthermore, the thickness of the nickel layer in S4 is 5-10 μm.

[0019] Furthermore, the cleaned quartz glass was immersed in a hydrofluoric acid solution with a volume fraction of 10% for 2 minutes to perform surface roughening treatment; and rinsed with deionized water to ensure that there was no residual acid on the surface.

[0020] Beneficial effects:

[0021] The present invention provides a process for surface nickel coating of quartz glass, which has the following beneficial effects:

[0022] (1) The microstructure is generated by surface roughening treatment, which improves the mechanical interlocking effect between the quartz glass surface and the nickel coating. The sensitization and activation steps make the surface evenly adsorb stannous ions and palladium catalyst layer, which enhances the reaction activity and bonding strength of chemical nickel plating. The nickel coating does not fall off in the peeling test, and the adhesion is greatly improved.

[0023] (2) The optimized chemical nickel plating solution formula and stirring control ensure uniform distribution of the plating solution and excellent uniformity of nickel layer thickness. Scanning electron microscopy shows that the coating surface is dense and defect-free, meeting the requirements of high-performance applications.

[0024] (3) The obtained nickel plating layer has good electrical conductivity, and the surface resistance value is less than 0.01Ω·cm, which meets the electrical conductivity requirements of the electronics industry; the plating layer has no obvious corrosion after being immersed in 3.5% NaCl solution for 48 hours, showing excellent corrosion resistance; it can be widely used in semiconductors, electrochemical catalysis, optical components and other fields.

[0025] (4) After the process flow of the present invention is optimized, only five main steps are required, namely, cleaning, roughening, sensitization, activation and chemical nickel plating, which is easy to operate; the use of a low-cost plating solution formula reduces the amount of chemical reagents and production costs; the efficient nickel plating process shortens the production time and improves production efficiency. The waste liquid is treated by alkali solution neutralization and flocculation precipitation, and the wastewater discharge meets environmental protection standards after the metal ions are removed; the number of chemicals used in the process is reduced, which reduces the impact on the environment and meets the requirements of modern green production. DETAILED DESCRIPTION

[0026] In order to deepen the understanding of the present invention, the present invention will be further described in detail below in conjunction with examples. The examples are only used to explain the present invention and do not constitute a limitation on the protection scope of the present invention.

[0027] Example:

[0028] A process for surface nickel treatment of quartz glass comprises the following steps:

[0029] Step S1: Quartz glass surface pretreatment

[0030] (1) Cleaning

[0031] Wash the quartz glass with deionized water to remove surface dust and impurities;

[0032] The quartz glass was placed in a 2% sodium hydroxide solution and ultrasonically cleaned at 40°C for 10 minutes.

[0033] Rinse repeatedly with deionized water until neutral, ensuring no residual alkali.

[0034] (2) Roughening treatment

[0035] The cleaned quartz glass was immersed in a hydrofluoric acid solution with a volume fraction of 10% for 2 minutes; and rinsed with deionized water to ensure that there was no residual acid on the surface.

[0036] Organic pollutants and dust are removed by alkaline cleaning, and combined with hydrofluoric acid roughening treatment, a certain surface roughness is generated, which significantly enhances the adhesion of the subsequent nickel plating layer to the quartz glass substrate.

[0037] Step S2: Sensitization treatment

[0038] (1) Preparation of sensitizing solution

[0039] Prepare the sensitizing solution, the composition is as follows:

[0040] Stannous chloride: 10g / L;

[0041] Hydrochloric acid: 40mL / L.

[0042] Sensitization Operation

[0043] Immerse the pretreated quartz glass in the sensitizing solution at 25°C for 5 minutes;

[0044] The sensitized quartz glass was rinsed with deionized water to prevent the active layer from falling off.

[0045] The sensitization treatment allows the quartz glass surface to adsorb stannous ions, providing a uniform seed layer for subsequent activation treatment and enhancing the uniformity and stability of the active layer formation.

[0046] Step S3: Activation treatment

[0047] Preparation of activation solution

[0048] Prepare the activation solution, the composition is as follows:

[0049] Palladium chloride: 1g / L;

[0050] Hydrochloric acid: 30mL / L.

[0051] Activation operation

[0052] Immerse the sensitized quartz glass in the activation solution at 25°C for 3 minutes;

[0053] The activated glass was rinsed with deionized water until no residual liquid remained on the surface.

[0054] The activation treatment generates a uniform palladium catalytic active layer on the surface of the quartz glass, which significantly improves the initial activity of the chemical nickel plating reaction.

[0055] Step S4: Chemical nickel plating

[0056] Plating solution preparation

[0057] The composition of chemical nickel plating solution is as follows:

[0058] Nickel sulfate: 30g / L;

[0059] Sodium hypophosphite: 20g / L;

[0060] Potassium sodium tartrate: 15g / L;

[0061] Acetic acid: 5mL / L;

[0062] The temperature was controlled at 85°C and the pH was adjusted to 4.5.

[0063] Nickel plating operation

[0064] Immersing the activated quartz glass into a chemical nickel plating solution;

[0065] Stir the plating solution to ensure that the solution is evenly distributed. The nickel plating time is 30 minutes;

[0066] The coating thickness is controlled at 5-10μm;

[0067] After nickel plating, rinse with deionized water;

[0068] Dry in a hot air drying oven at 60°C for 20 minutes.

[0069] The chemical nickel plating process produces a dense and uniform nickel coating through uniform plating solution composition and stable reaction conditions, giving quartz glass good conductivity and corrosion resistance.

[0070] Step S5: Wastewater treatment

[0071] Wastewater Neutralization

[0072] Add alkaline solution such as sodium hydroxide solution to the acidic waste liquid to adjust the pH to 7-8.

[0073] Metal ion precipitation

[0074] Adding a flocculant such as polyacrylamide to the neutralized wastewater to precipitate the metal ions;

[0075] The sediment is dried and then processed centrally, and the wastewater is discharged after passing the test.

[0076] Through neutralization and precipitation processes, harmful metal ions in the waste liquid are effectively removed, meeting the requirements of environmental protection and green production.

[0077] The following are the results of optimizing the nickel plating process:

[0078] ① Enhanced adhesion: Surface roughening combined with sensitization and activation treatment significantly improves the bonding strength between the nickel layer and the quartz glass;

[0079] ② Improved uniformity: Optimize the plating solution formula and reaction conditions to ensure that the nickel plating surface is uniform and free of defects;

[0080] ③ Improved functionality: The obtained coating has good conductivity (surface resistance <0.01Ω·cm) and corrosion resistance;

[0081] ④ Green and environmentally friendly: Through strict waste liquid treatment process, environmental pollution is reduced and environmental regulations are complied with.

[0082] As a further improvement, the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for surface nickel coating of quartz glass, characterized in that: The process comprises the following steps: S1. Pre-treat the quartz glass surface: S2, sensitization treatment: immerse the quartz glass in the sensitizing solution, control the temperature to 25°C; immerse for 5 minutes, so that the surface of the quartz glass evenly adsorbs stannous ions; rinse with deionized water after sensitization to prevent the active layer from falling off; S3, activation treatment: immerse the sensitized quartz glass in activation solution, control the temperature to 25°C; immerse for 3 minutes, so that a catalytic active layer is formed on the surface of the quartz glass; rinse with deionized water until there is no residual liquid on the surface; S4, chemical nickel plating: prepare chemical nickel plating solution; adjust pH value to 4.5; maintain temperature at 85°C; immerse activated quartz glass in chemical nickel plating solution, stir evenly, nickel plating time is 30 minutes; nickel plating layer thickness is 5-10μm; rinse with deionized water after nickel plating, and dry in a hot air drying oven at 60°C for 20 minutes; S5. Waste liquid treatment: Use alkaline solution to neutralize the acidic waste liquid and adjust the pH to 7-8; add flocculant to precipitate metal ions; the precipitate is dried and then centrally treated, and the wastewater is discharged after passing the test.

2. A process for surface nickel coating of quartz glass according to claim 1, characterized in that: S1 Quartz glass surface pretreatment includes the following steps: clean the quartz glass with deionized water to remove surface dust and impurities; perform ultrasonic cleaning at 40°C for 10 minutes in a 2% by volume sodium hydroxide solution; rinse with deionized water until neutral.

3. A process for surface nickel coating of quartz glass according to claim 1, characterized in that: The sensitizing solution in S2 is composed of 10 g / L stannous chloride and 40 mL / L hydrochloric acid.

4. A process for surface nickel coating of quartz glass according to claim 1, characterized in that: The activation solution in S3 is composed of 1 g / L palladium chloride and 30 mL / L hydrochloric acid.

5. A process for surface nickel coating of quartz glass according to claim 1, characterized in that: S4 is composed of 1 g / L palladium chloride and 30 mL / L hydrochloric acid.

6. A process for surface nickel coating of quartz glass according to claim 1, characterized in that: The thickness of the nickel layer in S4 is 5-10 μm.

7. A process for surface nickel coating of quartz glass according to claim 2, characterized in that: The cleaned quartz glass was immersed in a hydrofluoric acid solution with a volume fraction of 10% for 2 minutes to perform surface roughening treatment; and rinsed with deionized water to ensure that there was no residual acid on the surface.

Citation Information

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