Polishing solution for K9 optical glass as well as preparation method and application of polishing solution

By using water, hard abrasives, soft abrasives, pH adjusters, dispersants and complexing agents in the K9 optical glass polishing liquid, combined with a suitable grinding process, the problems of low removal rate and uneven surface of the K9 optical glass polishing liquid in the prior art are solved, and the effect of efficient removal and good planarization is achieved.

CN119529677APending Publication Date: 2025-02-28SHANGHAI ADVANCED SILICON TECH CO LTD +1
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Patent Information

Application Number
CN202411715944.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-27
Publication Date
2025-02-28

AI Technical Summary

Technical Problem

The existing polishing liquid used for K9 optical glass is difficult to compatible with processing efficiency and surface flattening, resulting in low removal rate and uneven surface, affecting product quality and application surface.

Method used

A polishing liquid including water, hard abrasives, soft abrasives, pH adjusters, dispersants and complexing agents is adopted. By selecting suitable dispersants and grinding processes, the coordinated combination and good dispersion of the soft abrasives and hard abrasives are ensured, and the removal rate and planarization effect of the polishing liquid are improved.

Benefits of technology

It achieves efficient removal rate and good planarization of K9 optical glass. The polished surface is free of scratches and corrosion pits under three-level strong light, taking into account both processing efficiency and surface planarization, and is suitable for mechanical polishing of K9 optical glass.

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Abstract

The invention provides a polishing solution for K9 optical glass and a preparation method and application thereof. The polishing solution comprises water, a hard abrasive, a soft abrasive, a pH regulator, a dispersing agent and a complexing agent, and the dispersing agent comprises a dispersing agent A, a dispersing agent B and a dispersing agent C; by selecting the three dispersants for matching and adopting a preparation process of respectively grinding the soft grinding material and the hard grinding material with the dispersant A and the dispersant B step by step, the obtained polishing solution is uniform in dispersion and proper in particle size, and further has an efficient removal rate on the K9 optical glass; the method has the advantages that the removal efficiency is high, the surface flatness of the polished K9 optical glass is good, scratches and corrosion pits are avoided under third-level strong light, the machining efficiency and the surface planarization can be considered, and the method is very suitable for being applied to mechanical polishing of the K9 optical glass.
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Description

Technical Field

[0001] The invention belongs to the technical field of polishing, and in particular relates to a polishing liquid for K9 optical glass and a preparation method and application thereof. Background Art

[0002] K9 glass is a common optical material. Due to its good fire resistance, high physical strength, thermal stability and low price, it is widely used in various fields such as chemical industry, aerospace, military, and medical treatment. Its processing has become a hot spot in the current market.

[0003] Chemical mechanical polishing (CMP) is a means of interconnected flattening. Different from the traditional purely mechanical or chemical polishing methods, CMP can achieve trace removal of workpiece materials through the interaction between abrasive particles, chemical reactions and processing environment, and achieve nano-scale or sub-nanometer surface. After years of development, it has become almost the only technology that can achieve global flattening, meeting the use requirements of most optical glasses. In CMP polishing, polishing liquid is one of the cores. The polishing liquid is mainly composed of polishing abrasive particles and chemical additives. The synergistic effect between the abrasive particles and the added substances is used to treat the processed surface.

[0004] However, the polishing liquid currently used for K9 optical glass still has the problem of incompatibility between processing efficiency and surface flattening. On the one hand, the low removal rate will increase the company's processing time and increase costs; on the other hand, the lower flattening affects the application surface and product quality of K9 glass.

[0005] Therefore, in view of the above technical problems, it is urgent to develop a polishing liquid that has a high removal rate for K9 optical glass and can obtain a relatively flat surface. Summary of the invention

[0006] In view of the deficiencies in the prior art, the object of the present invention is to provide a polishing liquid for K9 optical glass, a preparation method and an application thereof. The polishing liquid has a high removal rate for K9 glass material. It not only has a high removal efficiency but also has a good surface flatness of the K9 optical glass obtained after polishing, and is very suitable for the polishing of K9 optical glass.

[0007] To achieve this object, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a polishing liquid for K9 optical glass, the polishing liquid comprising water, a hard abrasive, a soft abrasive, a pH adjuster, a dispersant and a complexing agent, the dispersant comprising dispersant A, dispersant B and dispersant C;

[0009] The dispersant A comprises any one of sodium hexametaphosphate, polyvinyl pyrrolidone or sodium dodecylbenzene sulfonate or a combination of at least two thereof;

[0010] The dispersant B includes any one or a combination of at least two of magnesium aluminum silicate, hexadecyl trimethylamine or sodium lauroyl amino acid;

[0011] The dispersant C includes any one of polyoxyethylene ether, triethanolamine or propylene glycol, or a combination of at least two of them.

[0012] The polishing liquid for K9 optical glass provided by the present invention is prepared by selecting a soft abrasive and a hard abrasive for synergistic combination, selecting the above three dispersants for matching, and matching the soft abrasive and the hard abrasive with dispersant A and dispersant B for step-by-step grinding, so that the obtained polishing liquid has a high removal rate for the K9 optical glass material, and the surface flatness of the K9 optical glass obtained after polishing is good, without scratches and corrosion pits under level three strong light, and can take into account both processing efficiency and surface flatness, and is very suitable for application in the mechanical polishing of K9 optical glass.

[0013] In some preferred embodiments, based on the total mass of 100%, the amounts of the components contained in the polishing liquid are as follows: 0.5-3% of hard abrasive, 1-8% of soft abrasive, 0.1-1% of pH adjuster, 0.5-1% of dispersant A, 0.1-0.5% of dispersant B, 0.1-0.5% of dispersant C, 0.1-0.5% of complexing agent and the balance of deionized water.

[0014] The content of the hard abrasive may be 0.5%, 1%, 1.5%, 2%, 2.5% or 3%, etc.

[0015] The content of the soft abrasive can be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 7% or 8%, etc.

[0016] The content of the pH adjuster can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8% or 0.9%, etc.

[0017] The content of the dispersant A may be 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95% or 1%, etc.

[0018] The dosage of the dispersant B can be 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%, etc.

[0019] The dosage of the dispersant C can be 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%, etc.

[0020] The dosage of the complexing agent can be 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%, etc.

[0021] In some preferred embodiments, the hard abrasive includes any one of diamond, zirconium dioxide and silicon carbide, or a combination of at least two thereof.

[0022] In some preferred embodiments, the soft abrasive includes any one of cerium dioxide, aluminum oxide, silicon dioxide and lanthanum cerium oxyfluoride, or a combination of at least two thereof.

[0023] In some preferred embodiments, the pH adjuster includes any one of ammonium citrate, citric acid, oxalic acid, hydrochloric acid, potassium hydroxide, sodium hydroxide, sodium carbonate or triethanolamine, or a combination of at least two thereof.

[0024] In some preferred embodiments, the complexing agent includes any one or a combination of at least two of ethylenediaminetetraacetic acid, calcium polyacrylate, ferrous citrate, sodium gluconate, citric acid, calcium chloride, sodium polyacrylate or tartaric acid.

[0025] In some preferred embodiments, the polishing liquid further comprises a moisturizer.

[0026] In some preferred embodiments, the mass percentage of the moisturizing agent in the polishing liquid is 0.1-0.5%, for example, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%, etc.

[0027] In some preferred embodiments, the humectant includes any one or a combination of at least two of polyethylene glycol, glycerin, stearic acid, sodium carboxymethyl cellulose, xylitol, β-glucan, sodium γ-polyglutamate or sorbitol.

[0028] In some preferred embodiments, the polishing liquid also includes a bactericidal agent.

[0029] In some preferred embodiments, the mass percentage of the bactericidal agent in the polishing liquid is 0.05-0.2%, for example, 0.05%, 0.07%, 0.09%, 0.11%, 0.13%, 0.15%, 0.17%, 0.19% or 0.2%, etc.

[0030] In some preferred embodiments, the sterilizing agent includes any one of perchloro-meta-xylenol, ethanol, copper sulfate, ammonium persulfate, o-phenylphenol or hydrogen peroxide, or a combination of at least two thereof.

[0031] In a second aspect, the present invention provides a method for preparing a polishing liquid for K9 optical glass as described in the first aspect, the preparation method comprising the following steps:

[0032] (1) wet-milling a soft abrasive and a dispersant A in water to obtain a component A; wet-milling a hard abrasive and a dispersant B in water to obtain a component B;

[0033] (2) mixing component A and component B obtained in step (1), adding a complexing agent and performing wet ball milling to obtain component C;

[0034] (3) adding dispersant C to component C obtained in step (2) and stirring and mixing, and then adding a pH adjuster to adjust the pH value of the system to obtain the polishing liquid for K9 optical glass.

[0035] The invention provides a method for preparing a polishing liquid for K9 optical glass. The method comprises the following steps: firstly wet-milling a soft abrasive and a hard abrasive with a dispersant A and a dispersant B respectively, and then wet-milling them with a complexing agent. Finally, the abrasive and the hard abrasive are stirred and mixed with a dispersant C, and a pH regulator is added to adjust the pH value of the system. The soft abrasive and the hard abrasive are respectively dispersed by ball milling with the dispersant for multiple times. After reaching a certain dispersibility, the abrasive and the hard abrasive are mixed for secondary dispersion, so that a mixed abrasive polishing liquid with better dispersion, uniform dispersion, and appropriate particle size can be obtained, so that the polishing effect of the obtained polishing liquid on the K9 optical glass is better.

[0036] In some preferred embodiments, the forward and reverse rotation speeds of wet ball milling the soft abrasive and dispersant A in water and wet ball milling the hard abrasive and dispersant B in water in step (1) are independently 200-600 rpm, for example, 200 rpm, 250 rpm, 300 rpm, 350 rpm, 400 rpm, 450 rpm, 500 rpm, 550 rpm or 600 rpm, etc.

[0037] In some preferred embodiments, the time for wet ball milling the soft abrasive and dispersant A in water and wet ball milling the hard abrasive and dispersant B in water in step (1) is independently 20 to 40 min, for example, 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min or 40 min, etc.

[0038] In some preferred embodiments, the total time of the wet ball milling in step (2) is 120 to 180 min, for example, 120 min, 130 min, 140 min, 150 min, 160 min, 170 min or 180 min.

[0039] In some preferred embodiments, the forward and reverse rotation speeds of the wet ball milling in step (2) are both 400-800 rpm, for example, 400 rpm, 450 rpm, 500 rpm, 550 rpm, 600 rpm, 650 rpm, 700 rpm, 750 rpm or 800 rpm.

[0040] In some preferred embodiments, the stirring and mixing time in step (3) is 20 to 40 min, for example, 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min or 40 min, etc.

[0041] In some preferred embodiments, the stirring and mixing speed in step (3) is 400-600 rpm, for example, 400 rpm, 420 rpm, 440 rpm, 460 rpm, 480 rpm, 500 rpm, 520 rpm, 540 rpm, 560 rpm, 580 rpm or 600 rpm, etc.

[0042] In some preferred embodiments, after the stirring and mixing in step (3), a step of adding a moisturizer and a bactericide for mixing is also included.

[0043] In some preferred embodiments, the pH value of the system is adjusted to 10-11 by adding a pH adjuster in step (3), such as 10, 10.2, 10.4, 10.6, 10.8 or 11.

[0044] In a third aspect, the present invention provides a use of the polishing liquid as described in the first aspect in polishing K9 optical glass.

[0045] Compared with the prior art, the present invention has the following beneficial effects:

[0046] The polishing liquid for K9 optical glass provided by the present invention comprises water, a hard abrasive, a soft abrasive, a pH regulator, a dispersant and a complexing agent, and the dispersant comprises a dispersant A, a dispersant B and a dispersant C. By selecting the above three dispersants for matching and matching with a preparation process of grinding with the dispersants in steps, the obtained polishing liquid has a high removal rate for K9 glass material, and the flatness of the polished surface is good, there are no scratches and corrosion pits under three levels of strong light, and both processing efficiency and surface flatness can be taken into account, and the polishing liquid is very suitable for application in the polishing of K9 optical glass. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 This is an optical morphology image of K9 optical glass polished with the polishing liquid provided in Example 1;

[0048] Figure 2 This is an optical morphology image of K9 optical glass polished with the polishing liquid provided in Example 2;

[0049] Figure 3 This is an optical morphology image of K9 optical glass polished with the polishing liquid provided in Example 4;

[0050] Figure 4 This is an optical morphology image of K9 optical glass polished with the polishing liquid provided in Example 5;

[0051] Figure 5 The optical morphology of K9 optical glass after polishing with the polishing liquid provided in Comparative Example 1;

[0052] Figure 6 The 3D surface profile of K9 optical glass after being polished by the polishing liquid provided in Example 1;

[0053] Figure 7 The 3D surface profile of K9 optical glass after being polished by the polishing liquid provided in Example 2;

[0054] Figure 8 The 3D surface profile of K9 optical glass after being polished by the polishing liquid provided in Example 4;

[0055] Fig. 9 The 3D surface profile of K9 optical glass after being polished by the polishing liquid provided in Example 5;

[0056] Fig.10 This is a 3D surface profile of the K9 optical glass after polishing using the polishing liquid provided in Comparative Example 1. DETAILED DESCRIPTION

[0057] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0058] Unless otherwise specified, the raw materials involved in the following specific embodiments are all conventional materials in the art and can be purchased from commercial products.

[0059] Example 1

[0060] A polishing liquid for K9 optical glass, with the total amount being 100%, the amounts of the components included are shown in Table 1:

[0061] Table 1

[0062]

[0063] The method for preparing the polishing liquid for K9 optical glass provided in this embodiment comprises the following steps:

[0064] (1) Put a soft abrasive and a dispersant A into a ball mill, add 50 wt% of water to perform all-round wet ball milling, and the wet ball milling is specifically as follows: first, rotate forward at a speed of 400 rpm for 30 minutes, rest for 1 minute, and then rotate reversely at a speed of 400 rpm for 30 minutes to obtain component A;

[0065] Put the hard abrasive and dispersant B into a ball mill, add the remaining 50wt% of water and perform all-round wet ball milling. The wet ball milling is as follows: first, rotate forward at a speed of 400 rpm for 30 minutes, rest for 1 minute, and then reverse at a speed of 400 rpm for 30 minutes to obtain component B;

[0066] (2) Component A and component B obtained in step (1) are mixed, and a complexing agent is added to perform wet ball milling. The wet ball milling is specifically as follows: first, the mixture is rotated forward at a speed of 600 rpm for 30 min, rested for 1 min, then reversed at a speed of 600 rpm for 30 min, rested for 1 min, then rotated forward at a speed of 600 rpm for 30 min, rested for 1 min, and then reversed at a speed of 600 rpm for 30 min, to obtain component C;

[0067] (3) Component C obtained in step (2) and dispersant C are stirred at a rotation speed of 500 rpm for 30 minutes, a moisturizer and a bactericide are added and stirring is continued for 20 minutes, and a pH adjuster is added to adjust the pH value of the solution to 10.5, thereby obtaining the polishing liquid for K9 optical glass.

[0068] Example 2

[0069] A polishing liquid for K9 optical glass, with the total amount being 100%, the amounts of the components included are shown in Table 2:

[0070] Table 2

[0071]

[0072]

[0073] The preparation method of the polishing liquid for K9 optical glass provided in this embodiment is the same as that in Example 1.

[0074] Example 3

[0075] A polishing liquid for K9 optical glass, with the total amount being 100%, the amounts of the components included are shown in Table 3:

[0076] Table 3

[0077]

[0078] The method for preparing the polishing liquid for K9 optical glass provided in this embodiment comprises the following steps:

[0079] (1) Put a soft abrasive and a dispersant A into a ball mill, add 50 wt% of water to perform all-round wet ball milling, and the wet ball milling is as follows: first, rotate forward at 500 rpm for 30 min, rest for 1 min, and then rotate reversely at 500 rpm for 30 min to obtain component A;

[0080] Put the hard abrasive and dispersant B into a ball mill, add the remaining 50wt% of water and perform all-round wet ball milling. The wet ball milling is as follows: first, rotate forward at a speed of 500 rpm for 30 minutes, rest for 1 minute, and then reverse at a speed of 500 rpm for 30 minutes to obtain component B;

[0081] (2) Component A and component B obtained in step (1) are mixed, and a complexing agent is added to perform wet ball milling. The wet ball milling is specifically as follows: first, the mixture is rotated forward at 500 rpm for 35 min, followed by a 1-min interval, then rotated reversely at 500 rpm for 35 min, followed by a 1-min interval, then rotated forward at 500 rpm for 35 min, followed by a 1-min interval, and then rotated reversely at 500 rpm for 35 min, to obtain component C;

[0082] (3) Component C obtained in step (2) and dispersant C are stirred at a rotation speed of 500 rpm for 30 minutes, a moisturizer and a bactericide are added and stirring is continued for 20 minutes, and a pH adjuster is added to adjust the pH value of the solution to 11, thereby obtaining the polishing liquid for K9 optical glass.

[0083] Example 4

[0084] A polishing liquid for K9 optical glass, with the total amount being 100%, the amounts of the components included are shown in Table 4:

[0085] Table 4

[0086]

[0087] The method for preparing the polishing liquid for K9 optical glass provided in this embodiment comprises the following steps:

[0088] (1) Put soft abrasive, dispersant A and dispersant B into a ball mill, add water and perform all-round wet ball milling. The wet ball milling is as follows: first, rotate forward at 400 rpm for 30 min, rest for 1 min, and then rotate reversely at 400 rpm for 30 min to obtain component A;

[0089] (2) adding a complexing agent to the component A obtained in step (1) and performing wet ball milling, wherein the wet ball milling comprises: first rotating forward at a speed of 600 rpm for 30 min, resting for 1 min, then rotating reversely at a speed of 600 rpm for 30 min, resting for 1 min, then rotating forward at a speed of 600 rpm for 30 min, resting for 1 min, and then rotating reversely at a speed of 600 rpm for 30 min, to obtain component B;

[0090] (3) Component B obtained in step (2) and dispersant C are stirred at a rotation speed of 500 rpm for 30 minutes, a moisturizer and a bactericide are added and stirring is continued for 20 minutes, and a pH adjuster is added to adjust the pH value of the solution to 10.5, thereby obtaining the polishing liquid for K9 optical glass.

[0091] Example 5

[0092] A polishing liquid for K9 optical glass, with the total amount being 100%, the amounts of the components included are shown in Table 5:

[0093] Table 5

[0094]

[0095] The method for preparing the polishing liquid for K9 optical glass provided in this embodiment comprises the following steps:

[0096] (1) Put a hard abrasive, dispersant A and dispersant B into a ball mill, add water and perform all-round wet ball milling. The wet ball milling is as follows: first, rotate forward at a speed of 400 rpm for 30 minutes, rest for 1 minute, and then rotate reversely at a speed of 400 rpm for 30 minutes to obtain component A;

[0097] (2) adding a complexing agent to the component A obtained in step (1) and performing wet ball milling, wherein the wet ball milling comprises: first rotating forward at a speed of 600 rpm for 30 min, resting for 1 min, then rotating reversely at a speed of 600 rpm for 30 min, resting for 1 min, then rotating forward at a speed of 600 rpm for 30 min, resting for 1 min, and then rotating reversely at a speed of 600 rpm for 30 min, to obtain component B;

[0098] (3) Component B obtained in step (2) and dispersant C are stirred at a rotation speed of 500 rpm for 30 minutes, a moisturizer and a bactericide are added and stirring is continued for 20 minutes, and a pH adjuster is added to adjust the pH value of the solution to 10.5, thereby obtaining the polishing liquid for K9 optical glass.

[0099] Example 6

[0100] A polishing liquid for K9 optical glass, which differs from Example 1 in that the forward and reverse rotation speeds of the wet ball mill in step (1) of the preparation method are both 800 rpm, and other substances, amounts and steps are the same as those in Example 1.

[0101] Example 7

[0102] A polishing liquid for K9 optical glass, which differs from Example 1 in that the forward and reverse rotation speeds of the wet ball mill in step (1) of the preparation method are both 150 rpm, and other substances, amounts and steps are the same as those in Example 1.

[0103] Comparative Example 1

[0104] A polishing liquid for K9 optical glass, with the total amount being 100%, the amounts of the components included are shown in Table 6:

[0105] Table 6

[0106]

[0107] The method for preparing the polishing liquid for K9 optical glass provided in this embodiment comprises the following steps:

[0108] (1) Put soft abrasive, hard abrasive and dispersant A into a ball mill, add water and perform all-round wet ball milling. The wet ball milling is as follows: first, rotate forward at 400 rpm for 30 min, rest for 1 min, and then rotate reversely at 400 rpm for 30 min to obtain component A;

[0109] (2) adding a complexing agent to the component A obtained in step (1) and performing wet ball milling, wherein the wet ball milling comprises: first rotating forward at a speed of 600 rpm for 30 min, resting for 1 min, then rotating reversely at a speed of 600 rpm for 30 min, resting for 1 min, then rotating forward at a speed of 600 rpm for 30 min, resting for 1 min, and then rotating reversely at a speed of 600 rpm for 30 min, to obtain component B;

[0110] (3) Component B obtained in step (2) and dispersant C are stirred at a rotation speed of 500 rpm for 30 minutes, a moisturizer and a bactericide are added and stirring is continued for 20 minutes, and a pH adjuster is added to adjust the pH value of the solution to 10.5, thereby obtaining the polishing liquid for K9 optical glass.

[0111] Comparative Example 2

[0112] A polishing liquid for K9 optical glass, which differs from Example 1 in that no complexing agent is added, and other substances, dosages and preparation methods are the same as those in Example 1.

[0113] Performance Testing:

[0114] The polishing liquids provided in Examples 1 to 7 and Comparative Examples 1 to 2 were used to polish the K9 optical glass samples, wherein the K9 glass samples were circular sheets with a diameter of 10 mm, a thickness of 0.3 mm, and a measurement range of 50×50 μm. 2 The polishing pressure was 40 kPa, the rotation speed was 100 rpm, the swing arm rotation speed was 10 rpm, the flow rate of the polishing liquid was 10 mL / min, and the polishing time was 15 min to obtain the polished K9 optical glass.

[0115] (1) Optical morphology observation: The optical morphology of the polished K9 optical glass was tested using Olympus BX43, and the optical morphology of the K9 optical glass polished using the polishing solution provided in Example 1 was obtained as shown in FIG. Figure 1 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Example 2 is obtained as shown in FIG. Figure 2 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Example 4 is obtained as shown in FIG. Figure 3 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Example 5 is obtained as shown in FIG. Figure 4 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Comparative Example 1 is obtained as shown in Figure 5 As shown;

[0116] from Figure 1 to Figure 5 It can be seen that: Figure 1 to Figure 3 The surface of the polished K9 optical glass is very smooth without obvious scratches or corrosion pits. Figure 4 The polished K9 optical glass surface has obvious pits and scratches. Figure 5 There are also slight scratches on the surface of the polished K9 optical glass.

[0117] (2) 3D surface morphology observation: using the 3D optical surface profiler NewView TM The 3D surface morphology of the polished K9 optical glass was tested by 9000, and the 3D surface profile of the K9 optical glass polished by the polishing liquid provided in Example 1 was obtained as shown in FIG. Figure 6 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Example 2 is obtained as shown in FIG. Figure 7As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Example 4 is obtained as shown in FIG. Figure 8 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Example 5 is obtained as shown in FIG. Fig. 9 As shown, the 3D surface profile of the K9 optical glass after polishing with the polishing liquid provided in Comparative Example 1 is obtained as shown in Fig.10 As shown;

[0118] from Figure 6 to Figure 10 It can be seen that: Figure 6-7 The surface roughness of the K9 optical glass after polishing is low and the flatness is high. However, since no hard abrasive is added to the polishing liquid provided in Example 4, Figure 8 The surface roughness of the K9 optical glass after polishing in the embodiment 5 is improved, and since no soft abrasive is added to the polishing liquid provided in the embodiment 5, the same Fig. 9 The surface roughness of the polished K9 optical glass is improved; however, due to the uneven dispersion of particles in the polishing liquid provided in Comparative Example 1, the surface flatness of the polished K9 optical glass is also adversely affected.

[0119] (3) Roughness (Ra) and reflection wave surface precision (PV): Using the three-dimensional optical surface profiler NewView TM Obtained after testing 9000 pairs of polished K9 optical glass.

[0120] (4) Removal rate (MRR): refer to Calculated;

[0121] Wherein, MRR represents the removal rate, and the unit is nm / min;

[0122] △m is the mass change of K9 optical glass before and after polishing, in g;

[0123] ρ is the density of K9 optical glass, in g / cm 3 ;

[0124] s is the surface area of ​​K9 optical glass, in cm 2 ;

[0125] t is the polishing time, in minutes.

[0126] The MRR, Ra and PV of the K9 optical glass samples obtained by polishing the K9 optical glass samples with the polishing liquids provided in Examples 1 to 7 and Comparative Examples 1 to 2 using the above test method were tested, and the results are statistically shown in Table 7.

[0127] Table 7

[0128]

[0129]

[0130] According to the data in Table 7, we can see that:

[0131] (1) The polishing liquids provided in Examples 1 to 3 all have excellent polishing effects on K9 optical glass. The Ra of the K9 optical glass obtained after polishing is only 0.403 to 0.453 nm, the PV is only 4.72 to 6.92, and the removal rate is relatively high, reaching 1690.89 to 1826.16 nm / min.

[0132] (2) By comparing the data of Example 1 and Examples 4 to 7, it can be seen that if no hard abrasive is added (Example 4), the MRR of the polishing liquid will decrease, and the processing efficiency of the polishing liquid will be low; if no soft abrasive is added (Example 5), the Ra of the K9 optical glass after polishing with the obtained polishing liquid will be higher; if the rotation speed is too fast when dispersing the soft abrasive and the hard abrasive (Example 6), the MRR of the polishing liquid will decrease, and the processing efficiency of the polishing liquid will be low; if the rotation speed is too slow when dispersing the soft abrasive and the hard abrasive (Example 7), the Ra and PV of the K9 optical glass after polishing with the obtained polishing liquid will be higher, and the surface flatness will decrease.

[0133] (3) Comparison of the data of Example 1 and Comparative Examples 1-2 also shows that batch milling of soft abrasives and hard abrasives with different dispersants helps to improve the overall MRR and Ra of the polishing liquid; the addition of a complexing agent helps to improve the overall MRR and Ra of the polishing liquid.

[0134] The applicant declares that the present invention illustrates a polishing liquid for K9 optical glass and its preparation method and application through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A polishing liquid for K9 optical glass, characterized in that: The polishing liquid comprises water, a hard abrasive, a soft abrasive, a pH regulator, a dispersant and a complexing agent, wherein the dispersant comprises dispersant A, dispersant B and dispersant C; The dispersant A comprises any one of sodium hexametaphosphate, polyvinyl pyrrolidone or sodium dodecylbenzene sulfonate or a combination of at least two thereof; The dispersant B includes any one or a combination of at least two of magnesium aluminum silicate, hexadecyl trimethylamine or sodium lauroyl amino acid; The dispersant C includes any one of polyoxyethylene ether, triethanolamine or propylene glycol, or a combination of at least two of them.

2. The polishing liquid according to claim 1, characterized in that Based on the total mass of 100%, the polishing liquid comprises the following components: 0.5-3% of hard abrasive, 1-8% of soft abrasive, 0.1-1% of pH regulator, 0.5-1% of dispersant A, 0.1-0.5% of dispersant B, 0.1-0.5% of dispersant C, 0.1-0.5% of complexing agent and the balance of deionized water.

3. The polishing liquid according to claim 1 or 2, characterized in that: The hard abrasive material includes any one or a combination of at least two of diamond, zirconium dioxide and silicon carbide; Preferably, the soft abrasive comprises any one of cerium dioxide, aluminum oxide, silicon dioxide and lanthanum cerium oxyfluoride or a combination of at least two thereof; Preferably, the pH adjuster includes any one or a combination of at least two of ammonium citrate, citric acid, oxalic acid, hydrochloric acid, potassium hydroxide, sodium hydroxide, sodium carbonate or triethanolamine; Preferably, the complexing agent includes any one of ethylenediaminetetraacetic acid, calcium polyacrylate, ferrous citrate, sodium gluconate, citric acid, calcium chloride, sodium polyacrylate or tartaric acid, or a combination of at least two thereof.

4. The polishing liquid according to any one of claims 1 to 3, characterized in that: The polishing liquid also includes a moisturizer; Preferably, the mass percentage of the moisturizing agent in the polishing liquid is 0.1 to 0.5%; Preferably, the moisturizing agent comprises any one or a combination of at least two of polyethylene glycol, glycerin, stearic acid, sodium carboxymethyl cellulose, xylitol, β-glucan, sodium γ-polyglutamate or sorbitol.

5. The polishing liquid according to any one of claims 1 to 4, characterized in that: The polishing liquid also includes a sterilizing agent; Preferably, the mass percentage of the bactericide in the polishing liquid is 0.05-0.2%; Preferably, the sterilizing agent comprises any one of perchloro-meta-xylenol, ethanol, copper sulfate, ammonium persulfate, o-phenylphenol or hydrogen peroxide, or a combination of at least two thereof.

6. A method for preparing a polishing liquid for K9 optical glass as claimed in any one of claims 1 to 5, characterized in that: The preparation method comprises the following steps: (1) wet-milling a soft abrasive and a dispersant A in water to obtain a component A; wet-milling a hard abrasive and a dispersant B in water to obtain a component B; (2) mixing component A and component B obtained in step (1), adding a complexing agent and performing wet ball milling to obtain component C; (3) adding dispersant C to component C obtained in step (2) and stirring and mixing, and then adding a pH adjuster to adjust the pH value of the system to obtain the polishing liquid for K9 optical glass.

7. The preparation method according to claim 6, characterized in that: In step (1), the forward and reverse rotation speeds of wet ball milling the soft abrasive and dispersant A in water and wet ball milling the hard abrasive and dispersant B in water are independently 200 to 600 rpm; Preferably, the time for wet ball milling the soft abrasive and dispersant A in water and wet ball milling the hard abrasive and dispersant B in water in step (1) is independently 20 to 40 minutes.

8. The preparation method according to claim 6 or 7, characterized in that: The wet ball milling time in step (2) is 120 to 180 minutes; Preferably, the forward and reverse rotation speeds of the wet ball milling in step (2) are 400 to 800 rpm; Preferably, the stirring and mixing time in step (3) is 20 to 40 minutes; Preferably, the stirring and mixing in step (3) is performed at a speed of 400 to 600 rpm.

9. The preparation method according to any one of claims 6 to 8, characterized in that: After the stirring and mixing in step (3), the step of adding a moisturizer and / or a bactericide to mix the mixture may also be performed; Preferably, in step (3), the pH value of the system is adjusted to 10-11 by adding a pH adjuster.

10. Use of the polishing liquid according to any one of claims 1 to 5 in polishing K9 optical glass.