Polishing liquids, methods of making, applications, and polishing processes

By combining polishing powder, dispersant, chelating agent and pH adjuster in a specific ratio, the dispersibility and stability problems of cerium oxide polishing slurry are solved, achieving efficient and stable polishing effect and extended service life, while reducing the cost of the polishing process.

CN119775904BActive Publication Date: 2026-02-17SHENZHEN ZHONGWANG LIHUA MICROELECTRONIC MATERIAL CO LTD
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Patent Information

Application Number
CN202411917195.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-24
Publication Date
2026-02-17
Estimated Expiration
2044-12-24

AI Technical Summary

Technical Problem

Existing cerium oxide polishing slurries suffer from problems such as uneven polishing powder particle size, poor dispersibility, and sedimentation and agglomeration, resulting in unstable polishing effects and short service life, thus increasing the cost of the polishing process.

Method used

A stable dispersion system is formed by using a combination of polishing powder, dispersant, chelating agent, pH adjuster and bactericide in a specific ratio. The dispersibility and suspension of the polishing powder are improved by electrostatic repulsion and chelation, and the pH value is adjusted to ensure the stability and efficiency of the polishing process.

Benefits of technology

It improves the dispersibility and stability of the polishing slurry, extends its service life, improves polishing efficiency and quality, and reduces the cost of the polishing process.

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Abstract

The application discloses a polishing liquid, a preparation method, application and a polishing process, and relates to the technical field of polishing. The raw materials of the polishing liquid include cerium dioxide polishing powder, a dispersing agent, a chelating agent, a pH regulator, a bactericide and deionized water; the dispersing agent is selected from any one of an anionic dispersing agent and a non-ionic dispersing agent. The polishing liquid has good dispersibility, stability, service life and polishing performance, the preparation method is simple, safe and pollution-free, and the polishing liquid has a wide application prospect; and the polishing process of the application can be well combined with the polishing liquid, so that the polishing efficiency and polishing quality are further improved.
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Description

Technical Field

[0001] This invention relates to the field of polishing technology, and in particular to a polishing slurry, its preparation method, its application, and its polishing process. Background Technology

[0002] With the rapid development of the optics field, unprecedented progress has been made in many areas such as space technology, while the requirements for the performance and surface quality of optical component materials are also becoming increasingly stringent. Polishing is a crucial step in the processing of optical components, and polishing slurry, as an essential tool in the polishing process, is particularly important. Traditional polishing slurries suffer from problems such as poor suspension, poor dispersibility, and unstable surface quality, resulting in low polishing efficiency and poor polishing quality. Cerium oxide is a commonly used rare-earth polishing material; however, existing cerium oxide polishing slurries are prone to problems such as uneven polishing powder particle size, poor dispersibility, and sedimentation and agglomeration, leading to unstable polishing results. Furthermore, existing cerium oxide polishing slurries have a short lifespan, leading to waste and significantly increasing the cost of the polishing process. Summary of the Invention

[0003] The main objective of this invention is to develop a polishing fluid with excellent suspension and dispersibility, which can maintain the polishing process stably and efficiently and improve polishing quality and efficiency.

[0004] To achieve the above objectives, the present invention provides a polishing liquid comprising the following raw materials in the indicated mass percentages: polishing powder: 30%–60%; dispersant: 0.02%–1%; chelating agent: 0.1%–2%; pH adjuster: 0.5%–5%; bactericide: 0.05%–0.5%; and the balance being deionized water; wherein the polishing powder comprises cerium dioxide; and the dispersant is selected from any one of anionic dispersants and nonionic dispersants.

[0005] In one embodiment, the dispersant is an anionic dispersant, which includes sodium hexametaphosphate and sodium polyacrylate; wherein the mass ratio of sodium hexametaphosphate to sodium polyacrylate is 1:(0.8-1.1).

[0006] In one embodiment, the dispersant is a nonionic dispersant, which includes polyvinylpyrrolidone and hexadecyl alcohol polyoxyethylene ether; wherein the mass ratio of polyvinylpyrrolidone to hexadecyl alcohol polyoxyethylene ether is (0.8-1.2):2.

[0007] In one embodiment, the particle size range of the polishing powder satisfies the following: D50 is 0.5 to 2 μm, D10 is greater than 0.2 μm, and D100 is less than 5 μm.

[0008] In one embodiment, the polishing powder contains more than 99 wt% cerium dioxide.

[0009] In one embodiment, the pH adjuster comprises an organic base and an inorganic base; wherein the mass ratio of the organic base to the inorganic base in the pH adjuster is 1:(0.08 to 0.15).

[0010] In one embodiment, the organic base is selected from any one of diethanolamine, triethanolamine, ethylenediamine, and hydroxyethyldiamine.

[0011] In one embodiment, the inorganic base is selected from any one of sodium hydroxide, potassium hydroxide, and strontium hydroxide.

[0012] In one embodiment, the pH adjuster adjusts the pH of the polishing solution to 8-10.

[0013] In one embodiment, the chelating agent includes at least one of disodium ethylenediaminetetraacetate, aminotriacetic acid, diethylenetriaminepentaacetic acid, and citric acid.

[0014] The present invention also proposes a method for preparing the polishing slurry, comprising the following steps:

[0015] S10. Add the dispersant to deionized water, stir and disperse to obtain a dispersion.

[0016] S20. Add polishing powder to the dispersion obtained in step S10, stir and disperse to obtain a suspension.

[0017] S30. Add the chelating agent, bactericide, and pH adjuster to the suspension obtained in step S20, stir and disperse to obtain the polishing liquid.

[0018] The present invention also proposes the application of the polishing fluid in optical glass, liquid crystal panels and mobile phone cover glass.

[0019] The present invention also proposes a polishing process using the aforementioned polishing liquid, specifically comprising the following steps:

[0020] T10. Use the polishing slurry to perform rough polishing on the flat optical glass. The polishing pad material is a polyurethane white abrasive polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing slurry flow rate is set to 60 ml / min, the polishing pressure is set to 50 kPa, and the polishing time is set to 30 min to obtain rough polished glass.

[0021] T20. Use the polishing liquid to fine polish the rough-polished glass obtained in step T10. The polishing pad material is a polyurethane black damping cloth polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing liquid flow rate is set to 40 ml / min, the polishing pressure is set to 30 kPa, and the polishing time is set to 2 min to obtain the polished product.

[0022] The technical solution of this invention designs a polishing slurry, its preparation method, application, and polishing process using the polishing slurry. The polishing slurry of this invention constructs a stable dispersion system by adding specific types and proportions of compositions as dispersants. The polishing slurry of this invention also uses specific types and proportions of compositions as pH adjusters to rapidly respond to the acid-base chemical changes during the polishing process, ensuring the continuous chemical reaction on the glass surface and thus guaranteeing polishing efficiency and quality. The polishing slurry of this invention also incorporates specific polishing powders, chelating agents, and antibacterial agents, exhibiting good dispersibility, stability, service life, and polishing performance. The preparation method is simple, safe, and pollution-free, with broad application prospects. Furthermore, the polishing process of this invention can effectively combine with the above-mentioned polishing slurry, further improving polishing efficiency and quality. Detailed Implementation

[0023] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0024] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), the directional indications are only used to explain the relative positional relationship and movement of the components in a specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0025] Furthermore, if the embodiments of this invention involve descriptions such as "first" or "second," these descriptions are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the use of "and / or" or "and / or" throughout the text includes three parallel solutions. For example, "A and / or B" includes solution A, solution B, or a solution where both A and B are satisfied simultaneously. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.

[0026] The technical problem solved by this invention is that existing cerium oxide polishing slurries are prone to problems such as uneven particle size, poor dispersibility, and precipitation and agglomeration of polishing powder, which leads to unstable polishing effect. Moreover, existing cerium oxide polishing slurries have a short service life and are prone to waste, which will significantly increase the cost of the polishing process.

[0027] To address the aforementioned technical problems, a polishing slurry with excellent suspension and dispersibility is designed to maintain the stability and efficiency of the polishing process and improve polishing quality and efficiency. This invention proposes a polishing slurry comprising the following raw materials in the indicated mass percentages: polishing powder: 30%–60%; dispersant: 0.02%–1%; chelating agent: 0.1%–2%; pH adjuster: 0.5%–5%; bactericide: 0.05%–0.5%; and the balance being deionized water; wherein the polishing powder comprises cerium dioxide; and the dispersant is selected from either anionic or nonionic dispersants.

[0028] In one embodiment, the dispersant is an anionic dispersant, which includes sodium hexametaphosphate and sodium polyacrylate; wherein the mass ratio of sodium hexametaphosphate to sodium polyacrylate is 1:(0.8-1.1).

[0029] It should be noted that anionic dispersants are essentially anionic surfactants. In this embodiment, the anionic dispersants include sodium hexametaphosphate and sodium polyacrylate, and are limited to sodium hexametaphosphate and sodium polyacrylate. Sodium hexametaphosphate forms a bilayer structure and imparts a negative charge to the polishing powder particles, thereby achieving efficient dispersion of the polishing powder in the polishing liquid through electrostatic repulsion. In addition, sodium hexametaphosphate can also complex easily precipitated metal ions in the polishing liquid to prevent precipitation. Sodium polyacrylate utilizes the carboxyl groups on its polymer chain to chelate with the metal ions on the surface of the polishing powder particles, changing the surface charge state of the polishing powder particles. It achieves dispersion through charge neutralization and electrostatic repulsion. At the same time, the polymer chain of sodium polyacrylate acts as a bridge to stabilize the dispersion system.

[0030] It should also be noted that the mass ratio of sodium hexametaphosphate to sodium polyacrylate in this embodiment can be 1:0.8, 1:0.9, 1:1, or 1:1.1, including but not limited to the ratios listed above, and any ratio within the above range is acceptable; preferably, the mass ratio of sodium hexametaphosphate to sodium polyacrylate is 1:1. It should be noted that the above ratio is the result of the inventor's precise control over the type and amount of anionic dispersant, which is crucial to the dispersing effect of the dispersant.

[0031] In one embodiment, the dispersant is a nonionic dispersant, which includes polyvinylpyrrolidone and hexadecyl alcohol polyoxyethylene ether; wherein the mass ratio of polyvinylpyrrolidone to hexadecyl alcohol polyoxyethylene ether is (0.8-1.2):2.

[0032] It should be noted that nonionic dispersants are essentially nonionic surfactants. In this embodiment, the nonionic dispersants include polyvinylpyrrolidone (PVP) and cetyl alcohol polyoxyethylene ether (CEPE), and are limited to PPVP and CEPE. PPVP contains hydrophilic groups in its structure, which interact with active groups such as hydroxyl groups on the surface of the polishing powder particles. This allows PPVP to form an adsorption film on the surface of the polishing powder particles, thus separating the particles and generating repulsive forces, preventing particle aggregation. Furthermore, it can regulate the rheological properties of the solution and enhance the stability of the polishing liquid. CEPE has good wetting and dispersing effects on the surface of the polishing powder particles, forming a stable interfacial film. The polyoxyethylene segments in its molecular structure provide steric hindrance, further preventing particle aggregation, thereby constructing a stable dispersion system.

[0033] It should also be noted that the mass ratio of polyvinylpyrrolidone (PVP) to hexadecyl alcohol polyoxyethylene ether (HEPE) in this embodiment can be 0.8:2, 0.9:2, 1:2, or 1.2:2, including but not limited to the ratios listed above, and any ratio falling within the above range is acceptable. Preferably, the mass ratio of PPVP to HEPE is 1:2. It should be noted that the above ratio is the result of the inventor's precise control over the type and amount of nonionic dispersant, which is crucial to the dispersing effect of the dispersant. The synergistic effect of the two is better, which can further improve polishing efficiency and shows a significant synergistic enhancement effect.

[0034] In one embodiment, the particle size range of the polishing powder satisfies: D50 is 0.5-2 μm, D10 > 0.2 μm, and D100 < 5 μm.

[0035] Optionally, in one embodiment, the particle size range of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0036] Optionally, in one embodiment, the particle size range of the polishing powder satisfies: D50 is 0.5 μm, D10 > 0.2 μm, and D100 < 2 μm.

[0037] In one embodiment, the polishing powder contains more than 99 wt% cerium dioxide.

[0038] It should be noted that cerium dioxide, as a polishing material with moderate hardness, causes minimal scratches on the material surface during polishing. Cerium has multiple valence states and the conversion between different valence states is easy, which makes cerium dioxide easily destroy the silicate lattice during polishing. Through chemical adsorption, the substances in contact with the polishing agent on the glass surface are oxidized or form complexes and removed. Therefore, it is widely used in mechanical and chemical polishing processes.

[0039] In one embodiment, the pH adjuster comprises an organic base and an inorganic base; wherein the mass ratio of the organic base to the inorganic base in the pH adjuster is 1:(0.08-0.15);

[0040] In one embodiment, the organic base is selected from any one of diethanolamine, triethanolamine, ethylenediamine, and hydroxyethyldiamine.

[0041] In one embodiment, the inorganic base is selected from any one of sodium hydroxide, potassium hydroxide, and strontium hydroxide.

[0042] It should be noted that cerium dioxide consumes hydroxide ions during the polishing process to break down the silicate lattice. Therefore, a pH adjuster needs to be added to the polishing solution to provide sufficient hydroxide ions for the above reaction. At the same time, the concentration of hydroxide ions in the polishing solution also affects the reaction rate between cerium dioxide and silicates on the glass surface. Therefore, the pH adjuster in this invention is a combination of organic and inorganic bases, which can make the concentration change of hydroxide ions in the polishing solution more gradual, thereby ensuring the stable occurrence of the relevant reactions during the polishing process and preventing them from being too fast or too slow.

[0043] It should also be noted that changes in the pH value of the polishing solution affect the surface charge of cerium oxide polishing powder particles, thus influencing the electrostatic repulsion between particles. An appropriate pH value can enhance the repulsive force between particles, resulting in better dispersion of the polishing powder in the polishing solution, reducing agglomeration, and improving the suspension stability of the polishing solution. Simultaneously, it allows the polishing powder to be more evenly distributed and covered on the polished surface, thereby improving polishing efficiency and surface quality. pH adjusters can change the pH value of the polishing solution, which affects the zeta potential of the polishing solution. A higher absolute value of the zeta potential indicates greater repulsive force between polishing powder particles and higher stability of the polishing solution.

[0044] In one embodiment, the pH adjuster comprises diethanolamine and potassium hydroxide, wherein the mass ratio of diethanolamine to potassium hydroxide is 1:(0.08-0.12). In a preferred embodiment, the pH adjuster comprises diethanolamine and potassium hydroxide, wherein the mass ratio of diethanolamine to potassium hydroxide is 1:0.1.

[0045] In one embodiment, the pH adjuster comprises triethanolamine and sodium hydroxide, wherein the mass ratio of triethanolamine to sodium hydroxide is 1:(0.1 to 0.15). In a preferred embodiment, the pH adjuster comprises triethanolamine and sodium hydroxide, wherein the mass ratio of triethanolamine to sodium hydroxide is 1:0.1.

[0046] It should be noted that both of the above pH adjusters are combinations of organic bases and strong inorganic bases. By using organic bases and strong inorganic bases in combination, the pH value of the polishing solution can be effectively adjusted to a suitable range, improving polishing efficiency while ensuring the stability and dispersibility of the polishing solution.

[0047] In one embodiment, the pH adjuster adjusts the pH value of the polishing solution to 8-10. It should be noted that a suitable pH value allows the polishing powder to be more evenly distributed and covered on the polished surface, thereby improving polishing efficiency and surface quality; it can also affect the Zeta potential of the polishing solution, thus enhancing its stability.

[0048] In one embodiment, the chelating agent includes at least one of disodium ethylenediaminetetraacetate, aminotriacetic acid, diethylenetriaminepentaacetic acid, and citric acid.

[0049] It should be noted that the chelating agent in the polishing slurry can form stable chelates with various metal ions in the slurry, which helps to improve the stability of the polishing slurry. The chelating agent can also increase the removal rate of metal ions in the polishing slurry, which affects the rate control and surface morphology improvement in the chemical mechanical polishing process. In addition, the chelating agent ensures the stable progress of the polishing process by inhibiting the occurrence of side reactions during the polishing process. During the polishing process, the chelating agent helps to reduce the contamination of the system by metal chips on the machine, thereby maintaining the performance of the polishing slurry.

[0050] In one embodiment, the bactericide is 1,2-benzisothiazolin-3-one.

[0051] It should be noted that 1,2-benzisothiazolin-3-one exhibits broad-spectrum activity against bacteria and fungi, and possesses advantages such as good water solubility, low toxicity, and easy degradation. 1,2-benzisothiazolin-3-one is characterized by being halogen-free, not requiring metal ions for stability, heat-resistant, and having low toxicity. Its good solubility allows it to be formulated into pure aqueous solutions, effectively resisting contamination by a variety of microorganisms.

[0052] The present invention also proposes a method for preparing the polishing slurry, comprising the following steps:

[0053] S10. Add the dispersant to deionized water, stir and disperse to obtain a dispersion.

[0054] S20. Add polishing powder to the dispersion obtained in step S10, stir and disperse to obtain a suspension.

[0055] S30. Add the chelating agent, bactericide, and pH adjuster to the suspension obtained in step S20, stir and disperse to obtain the polishing liquid.

[0056] In one embodiment, in step S10, the stirring rate is 50 rpm and the stirring time is 1 to 3 minutes.

[0057] In one embodiment, in step S20, the stirring rate is 50 rpm and the stirring time is 2 to 5 minutes.

[0058] In one embodiment, in step S20, the stirring rate is 50 rpm and the stirring time is 5 to 10 min.

[0059] The present invention also proposes the application of the polishing fluid in optical glass, liquid crystal panels and mobile phone cover glass.

[0060] The present invention also proposes a polishing process using the aforementioned polishing slurry, specifically including the following steps:

[0061] T10. Use the polishing slurry to perform rough polishing on the flat optical glass. The polishing pad material is a polyurethane white abrasive polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing slurry flow rate is set to 60 ml / min, the polishing pressure is set to 50 kPa, and the polishing time is set to 30 min to obtain rough polished glass.

[0062] T20. Use the polishing liquid to fine polish the rough-polished glass obtained in step T10. The polishing pad material is a polyurethane black damping cloth polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing liquid flow rate is set to 40 ml / min, the polishing pressure is set to 30 kPa, and the polishing time is set to 2 min to obtain the polished product.

[0063] The present invention will be further illustrated below through specific embodiments:

[0064] All raw materials used in the embodiments of this invention are commercially available, and this invention does not impose any special restrictions on the source of raw materials.

[0065] Example 1

[0066] The polishing slurry in Example 1 comprises the following raw materials in weight percentages:

[0067] The composition includes 50% polishing powder, 0.4% dispersant, 0.5% chelating agent, 0.2% bactericide, 2.2% pH adjuster, and 46.7% deionized water.

[0068] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0069] The dispersant is a combination of anionic dispersants, including sodium hexametaphosphate and sodium polyacrylate in a mass ratio of 1:1; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 1,2-benzisothiazolin-3-one.

[0070] The preparation method of the polishing slurry in Example 1 includes the following steps:

[0071] S10. Add the dispersant to deionized water and stir at 50 rpm until completely dissolved to obtain a dispersion.

[0072] S20. Add polishing powder to the dispersion obtained in step S10, and stir and disperse at a rate of 50 rpm for 2 minutes to obtain a suspension.

[0073] S30. The chelating agent, bactericide, and pH adjuster are added sequentially to the suspension obtained in step S20, and the mixture is stirred and dispersed at a rate of 50 rpm for 5 minutes to obtain the polishing solution.

[0074] Using an optical glass substrate as a polishing sample, the polishing solution and corresponding polishing process described in Example 1 were applied to the sample, specifically including the following steps:

[0075] T10. The optical glass substrate is rough polished. The polishing pad material is polyurethane white abrasive polishing pad. The polishing head speed is set to 80 r / min, the polishing disk speed is set to 60 r / min, the polishing fluid flow rate is set to 60 ml / min, the polishing pressure is set to 50 kPa, and the polishing time is set to 30 min to obtain the rough polished sample.

[0076] T20. The rough polished sample obtained in step T10 is finely polished. The polishing pad material is a polyurethane black damping cloth polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing liquid flow rate is set to 40 ml / min, the polishing pressure is set to 30 kPa, and the polishing time is set to 2 min to obtain the polished sample.

[0077] Example 2

[0078] The polishing slurry in Example 2 comprises the following raw materials in weight percentages:

[0079] The composition includes 40% polishing powder, 0.2% dispersant, 0.5% chelating agent, 0.2% bactericide, 3.3% pH adjuster, and 55.8% deionized water.

[0080] The polishing powder is cerium dioxide polishing powder, and the cerium dioxide content in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 0.5 μm, D10 is greater than 0.2 μm, and D100 is less than 2 μm.

[0081] The dispersant is a combination of anionic dispersants, including sodium hexametaphosphate and sodium polyacrylate in a mass ratio of 1:1; the pH adjuster is a combination of diethanolamine and potassium hydroxide, including diethanolamine and potassium hydroxide in a mass ratio of 1:0.1; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 1,2-benzisothiazolin-3-one.

[0082] The polishing slurry in Example 2 was prepared using the same method as in Example 1.

[0083] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Example 2. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0084] Example 3

[0085] The polishing slurry in Example 3 comprises the following raw materials in weight percentages:

[0086] Polishing powder 55%, dispersant 0.8%, chelating agent 1%, bactericide 0.4%, pH adjuster 3.3%, deionized water 39.5%.

[0087] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0088] The dispersant is a combination of nonionic dispersants, including polyvinylpyrrolidone and hexadecyl alcohol polyoxyethylene ether in a mass ratio of 1:2; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1.

[0089] The polishing slurry in Example 3 was prepared using the same method as in Example 1.

[0090] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Example 3. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0091] Example 4

[0092] The polishing slurry in Example 4 comprises the following raw materials in weight percentages:

[0093] The composition includes 60% polishing powder, 1% dispersant, 0.1% chelating agent, 0.05% bactericide, 5% pH adjuster, and 33.85% deionized water.

[0094] The polishing powder is cerium dioxide polishing powder, and the cerium dioxide content in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 0.5 μm, D10 is greater than 0.2 μm, and D100 is less than 2 μm.

[0095] The dispersant is a combination of nonionic dispersants, including polyvinylpyrrolidone and cetyl alcohol polyoxyethylene ether in a mass ratio of 0.8:2; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1.

[0096] The polishing slurry in Example 4 was prepared using the same method as in Example 1.

[0097] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Example 4. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0098] Example 5

[0099] The polishing slurry in Example 5 comprises the following raw materials in weight percentages:

[0100] The composition includes 30% polishing powder, 0.02% dispersant, 2% chelating agent, 0.5% bactericide, 0.5% pH adjuster, and 66.98% deionized water.

[0101] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0102] The dispersant is a combination of anionic dispersants, including sodium hexametaphosphate and sodium polyacrylate in a mass ratio of 1:0.8; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 1,2-benzisothiazolin-3-one.

[0103] The polishing slurry in Example 5 was prepared using the same method as in Example 1.

[0104] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Example 5. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0105] Comparative Example 1

[0106] The polishing slurry in Comparative Example 1 comprises the following raw materials by mass percentage:

[0107] The composition includes 50% polishing powder, 1% dispersant, 0.6% chelating agent, 0.3% bactericide, 1% pH adjuster, and 47.1% deionized water.

[0108] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0109] The dispersant is a combination of other anionic dispersants, specifically sodium butylnaphthalenesulfonate (dispersant powder) and sodium methylene bisnaphthalenesulfonate (NNO) in a mass ratio of 1:1; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 1,2-benzisothiazolin-3-one.

[0110] The polishing slurry in Comparative Example 1 was prepared using the same method as in Example 1.

[0111] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Comparative Example 1. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0112] Comparative Example 2

[0113] The polishing slurry in Comparative Example 2 comprises the following raw materials by mass percentage:

[0114] The composition includes 40% polishing powder, 1% dispersant, 0.5% chelating agent, 0.4% bactericide, 1% pH adjuster, and 57.1% deionized water.

[0115] The polishing powder is cerium dioxide polishing powder, and the cerium dioxide content in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies the following conditions: D50 is 0.5 μm, D10 is greater than 0.1 μm, and D100 is less than 3 μm.

[0116] The dispersant is a combination of nonionic dispersants, including polyvinylpyrrolidone and polyethylene glycol 400 in a mass ratio of 1:2; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 1,2-benzisothiazolin-3-one.

[0117] The polishing slurry in Comparative Example 2 was prepared using the same method as in Example 1.

[0118] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Comparative Example 2. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0119] Comparative Example 3

[0120] The polishing slurry in Comparative Example 3 comprises the following raw materials by mass percentage:

[0121] The composition includes 55% polishing powder, 1% dispersant, 0.6% chelating agent, 0.3% bactericide, 0.1% pH adjuster, and 43% deionized water.

[0122] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0123] The dispersant is a combination of anionic and nonionic dispersants, including sodium hexametaphosphate and hexadecyl polyoxyethylene ether in a mass ratio of 1:2; the pH adjuster is a combination of triethanolamine and sodium hydroxide, including triethanolamine and sodium hydroxide in a mass ratio of 1:0.1; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 1,2-benzisothiazolin-3-one.

[0124] The polishing slurry in Comparative Example 3 was prepared using the same method as in Example 1.

[0125] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Comparative Example 3. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0126] Comparative Example 4

[0127] The polishing slurry in Comparative Example 4 comprises the following raw materials by mass percentage:

[0128] The composition includes 50% polishing powder, 1% dispersant, 0.6% chelating agent, 0.3% bactericide, 0.1% pH adjuster, and 48.0% deionized water.

[0129] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0130] The dispersant is a combination of other anionic dispersants, including sodium hexametaphosphate and sodium polyacrylate in a mass ratio of 1:0.8; the pH adjuster is sodium hydroxide; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 2-methyl-1,2-benzisothiazol-3-one (MBIT).

[0131] The polishing slurry in Comparative Example 4 was prepared using the same method as in Example 1.

[0132] An optical glass substrate was used as a polishing sample and polished using the polishing solution and corresponding polishing process in Comparative Example 4. The polishing process was the same as in Example 1, and the polished sample was obtained.

[0133] Comparative Example 5

[0134] The polishing solution and preparation method in Comparative Example 5 are the same as those in the Example. The polishing process in Comparative Example 5 includes the following steps:

[0135] The composition consists of 50% polishing powder, 1% dispersant, 0.6% chelating agent, 0.3% bactericide, 0.1% pH adjuster, and 48% deionized water.

[0136] The polishing powder is cerium dioxide polishing powder, and the content of cerium dioxide in the polishing powder is greater than 99 wt%. The particle size distribution of the polishing powder satisfies: D50 is 1 μm, D10 > 0.3 μm, and D100 < 3 μm.

[0137] The dispersant is a combination of other anionic dispersants, including sodium hexametaphosphate and sodium polyacrylate in a mass ratio of 1:0.8; the pH adjuster is sodium hydroxide; the chelating agent is disodium ethylenediaminetetraacetate; and the bactericide is 2-methyl-1,2-benzisothiazol-3-one (MBIT).

[0138] An optical glass substrate was used as the polishing sample and polished using the polishing slurry and corresponding polishing process in Comparative Example 5. The polishing process specifically included the following steps:

[0139] T10. The optical glass substrate is rough polished. The polishing pad material is polyurethane white abrasive polishing pad. The polishing head speed is set to 50 r / min, the polishing disk speed is set to 40 r / min, the polishing fluid flow rate is set to 30 ml / min, the polishing pressure is set to 60 kPa, and the polishing time is set to 30 min to obtain the rough polished sample.

[0140] T20. The rough polished sample obtained in step T10 is finely polished. The polishing pad material is a polyurethane black damping cloth polishing pad. The polishing head speed is set to 50 r / min, the polishing disc speed is set to 40 r / min, the polishing liquid flow rate is set to 20 ml / min, the polishing pressure is set to 70 kPa, and the polishing time is set to 2 min to obtain the polished sample.

[0141] Performance testing:

[0142] (1) The average apparent yield, average removal amount and surface roughness Ra of the polished samples in Examples 1-5 and Comparative Examples 1-5 were measured respectively. The measurement results are shown in Table 1.

[0143] (2) The polishing liquids in Examples 1-5 and Comparative Examples 1-5 were circulated and polished for 24 hours and then polished again. The average apparent yield, average removal amount and surface roughness Ra of the samples were measured respectively. The measurement results are shown in Table 2.

[0144] (3) Comparison of the layer height before and after standing of the polishing liquids in Examples 1-5 and Comparative Examples 1-5 for different periods: Weigh an appropriate amount of the polishing liquids in Examples 1-5 and Comparative Examples 1-5 and place them in a slender 25mL glass graduated cylinder. Measure the layer height before and after standing. The test results are shown in Table 3.

[0145] The average removal amount was measured by dividing the mass difference of the optical glass substrate before and after polishing by the area of ​​the optical glass substrate and then by the polishing time; the surface roughness of the optical glass after polishing was measured using an atomic force microscope.

[0146] Table 1

[0147] Item Average apparent rate of removal Average removal amount Surface roughness Ra (nm) Example 1 96.9% 1.12 μm / min 0.637 Example 2 95.5% 0.97 μm / min 0.549 Example 3 93.9% 1.31 μm / min 0.621 Example 4 94.0% 1.45 μm / min 0.701 Example 5 97.1% 0.90 μm / min 0.423 Comparative Example 1 94.5% 0.89 μm / min 0.823 Comparative Example 2 96.7% 0.73 μm / min 0.719 Comparative Example 3 93.2% 1.12 μm / min 0.932 Comparative Example 4 93.0% 1.08 μm / min 0.895 Comparative Example 5 83.5% 0.523 μm / min 1.321

[0148] Table 2

[0149] Item Average apparent rate of removal Average removal amount Surface roughness Ra (nm) Example 1 96.2% 1.10 μm / min 0.731 Example 2 95.1% 1.01 μm / min 0.623 Example 3 93.5% 1.22 μm / min 0.701 Example 4 93.6% 1.33 μm / min 0.765 Example 5 96.2% 0.88 μm / min 0.533 Comparative Example 1 94.1% 0.63 μm / min 1.089 Comparative Example 2 95.1% 0.55 μm / min 0.802 Comparative Example 3 93.0% 0.84 μm / min 1.022 Comparative Example 4 91.2% 0.98 μm / min 0.855 Comparative Example 5 80.4% 0.46 μm / min 1.457

[0150] Table 3

[0151] Item 0h 0.5h 1h 2h 3h 6h Example 1 10 / 10 cm 10 / 9.5 cm 10 / 9.0 cm 10 / 8.1 cm 10 / 7.5 cm 10 / 7.2 cm Example 2 10 / 10 cm 10 / 9.6 cm 10 / 9.2 cm 10 / 8.5 cm 10 / 8.0 cm 10 / 7.8 cm Example 3 10 / 10 cm 10 / 9.3 cm 10 / 8.8 cm 10 / 8.0 cm 10 / 7.4 cm 10 / 7.1 cm Example 4 10 / 10 cm 10 / 9.5 cm 10 / 9.3 cm 10 / 8.8 cm 10 / 8.3 cm 10 / 7.9 cm Example 5 10 / 10 cm 10 / 9.2 cm 10 / 8.9 cm 10 / 8.5 cm 10 / 7.9 cm 10 / 7.4 cm Comparative Example 1 10 / 10 cm 10 / 9.1 cm 10 / 8.2 cm 10 / 7.3 cm 10 / 6.8 cm 10 / 6.3 cm Comparative Example 2 10 / 10 cm 10 / 9.2 cm 10 / 8.2 cm 10 / 7.5 cm 10 / 6.7 cm 10 / 6.3 cm Comparative Example 3 10 / 10 cm 10 / 8.9 cm 10 / 7.9 cm 10 / 7.0 cm 10 / 6.5 cm 10 / 6.2 cm Comparative Example 4 10 / 10 cm 10 / 9.0 cm 10 / 8.1 cm 10 / 7.4 cm 10 / 6.7 cm 10 / 6.4 cm Comparative Example 5 10 / 10 cm 10 / 9.0 cm 10 / 8.1 cm 10 / 7.4 cm 10 / 6.7 cm 10 / 6.4 cm

[0152] Analysis of Tables 1-3 shows that the polishing slurries in Examples 1-5 exhibit superior performance in terms of suspension, polishing rate, and surface roughness stability. They demonstrate significant performance advantages and are more suitable for long-term use and maintaining stable polishing results. In contrast, the polishing slurries in Comparative Examples 1-5, after prolonged standing, show sedimentation and stratification, requiring longer stirring times to restore uniform dispersion, and their lifespan for cyclic polishing also suffers more severe degradation.

[0153] The above description is merely an exemplary embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention under the technical concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.

Claims

1. A polishing process, characterized in that, Specifically, the following steps are included: T10. Use polishing slurry to rough polish the flat optical glass. The polishing pad material is polyurethane white abrasive polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing slurry flow rate is set to 60 ml / min, the polishing pressure is set to 50 kPa, and the polishing time is set to 30 min to obtain rough polished glass. T20. Use polishing slurry to fine polish the rough polished glass obtained in step T10. The polishing pad material is a polyurethane black damping cloth polishing pad. The polishing head speed is set to 80 r / min, the polishing disc speed is set to 60 r / min, the polishing slurry flow rate is set to 40 ml / min, the polishing pressure is set to 30 kPa, and the polishing time is set to 2 min to obtain the polished product. The polishing slurry comprises the following raw materials by weight percentage: polishing powder: 30%~60%; Dispersant: 0.02%~1%; Chelating agent: 0.1%~2%; pH adjuster: 0.5%~5%; bactericide: 0.05%~0.5%; and the balance being deionized water; The dispersant is selected from any one of anionic and nonionic dispersants; the anionic dispersant includes sodium hexametaphosphate and sodium polyacrylate, wherein the mass ratio of sodium hexametaphosphate to sodium polyacrylate is 1:(0.8~1.1); and / or, the nonionic dispersant includes polyvinylpyrrolidone and hexadecyl alcohol polyoxyethylene ether, wherein the mass ratio of polyvinylpyrrolidone to hexadecyl alcohol polyoxyethylene ether is (0.8~1.2):2; The polishing powder has the following particle size range: D50 is 0.5–2 μm, D10 is >0.2 μm, and D100 is <5 μm; and the cerium dioxide content in the polishing powder is greater than 99 wt%. The pH adjuster comprises an organic base and an inorganic base, wherein the mass ratio of the organic base to the inorganic base is 1:(0.08~0.15), the organic base is selected from any one of diethanolamine, triethanolamine, ethylenediamine, and hydroxyethyldiamine, and the inorganic base is selected from any one of sodium hydroxide, potassium hydroxide, and strontium hydroxide.

2. The polishing process as described in claim 1, characterized in that, The pH adjuster comprises diethanolamine and potassium hydroxide, wherein the mass ratio of diethanolamine to potassium hydroxide is 1:(0.08~0.12). Alternatively, the pH adjuster may comprise triethanolamine and sodium hydroxide, wherein the mass ratio of triethanolamine to sodium hydroxide is 1:(0.1~0.15).

3. The polishing process as described in claim 1, characterized in that, The pH adjuster adjusts the pH value of the polishing solution to 8-10.

4. The polishing process as described in claim 1, characterized in that, The chelating agent includes at least one of disodium ethylenediaminetetraacetate, aminotriacetic acid, diethylenetriaminepentaacetic acid, and citric acid.

5. The polishing process as described in claim 1, characterized in that, The preparation method of the polishing slurry includes the following steps: S10. Add the dispersant to deionized water, stir and disperse to obtain a dispersion. S20. Add polishing powder to the dispersion obtained in step S10, stir and disperse to obtain a suspension. S30. Add the chelating agent, bactericide, and pH adjuster to the suspension obtained in step S20, stir and disperse to obtain the polishing liquid.

6. The application of a polishing process as described in any one of claims 1 to 5 in optical glass, liquid crystal panels, and mobile phone cover glass.

Citation Information

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