A high-hardness wear-resistant material and its preparation method
By oxidizing and fluorinating nanodiamonds and combining them with a chelate of aluminum isopropoxide and zirconium n-propoxide, a micro-nano hierarchical structure was constructed. The problem of insufficient hardness and wear resistance of the optical coating was solved by using UV pre-curing and gradient thermal curing processes, thereby improving the mechanical strength and transmittance of the optical coating.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-12
- Publication Date
- 2026-04-03
AI Technical Summary
Existing optical coating materials are insufficient in terms of hardness and wear resistance, especially when matched with flexible substrates, they are prone to brittleness or wear, affecting the transmittance and imaging quality of optical systems.
By oxidizing and fluorinating nanodiamonds and combining them with a chelate of aluminum isopropoxide and zirconium n-propoxide, a micro-nano hierarchical structure is constructed, and a high-hardness, wear-resistant optical coating is formed by using a UV pre-curing and gradient thermal curing process.
It significantly improves the mechanical strength and wear resistance of the optical coating, reduces brittleness, maintains optical transmittance, and solves the problems of poor adhesion and easy peeling of the optical coating on the substrate.
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Figure CN121471742B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of optical coating technology, specifically to a high-hardness wear-resistant treatment material and its preparation method. Background Technology
[0002] In the field of modern precision optics, optical coating materials are required not only to possess specific spectral characteristics but also to withstand harsh environmental conditions. Traditional high-hardness optical coating materials are mainly concentrated in oxide or fluoride systems. These materials are typically prepared by electron beam evaporation or magnetron sputtering, using high-energy particles to bombard the substrate to form a dense layer, providing necessary mechanical protection. They are widely used in fields such as eyeglasses, mobile phone touchscreens, camera lenses, and automotive LiDAR windows.
[0003] However, existing optical coatings face severe performance bottlenecks. Pure inorganic coatings (such as pure SiO2) have extremely high hardness, but their coefficient of thermal expansion is severely mismatched with the substrate (such as polymers like PC and PMMA), making them prone to internal stress, resulting in brittleness and easy cracking upon impact. Traditional organic-inorganic hybrid coatings, while improving flexibility, suffer from reduced hardness and low wear resistance due to the high proportion of organic components and the tendency of inorganic particles to agglomerate. In harsh environments, the coating surface is easily scratched, leading to increased light scattering and severely affecting the transmittance and imaging quality of the optical system.
[0004] To address this, a high-hardness wear-resistant material and its preparation method are proposed. Summary of the Invention
[0005] The purpose of this invention is to design a high-hardness wear-resistant treatment material and its preparation method. This invention involves oxidizing and fluorinating nanodiamonds to obtain a diamond treatment solution; chelating aluminum isopropoxide and zirconium n-propoxide to prepare a chelating material; synthesizing a silane-based material containing double bonds; mixing the diamond treatment solution, chelating material, and matrix material for a solvothermal reaction to obtain an optical treatment material; finally, adding additives for formulation, coating the surface of an optical substrate, and subjecting it to UV pre-curing and gradient thermal curing to obtain a high-hardness wear-resistant treatment material, ultimately significantly improving the mechanical strength and wear resistance of the optical coating.
[0006] To achieve the above objectives, the present invention provides the following technical solution:
[0007] This invention provides a method for preparing a high-hardness, wear-resistant material, comprising the following steps by weight:
[0008] A diamond treatment solution is obtained by oxidizing and fluorinating nanodiamonds.
[0009] Aluminum isopropoxide and zirconium n-propoxide were dissolved in ethyl acetoacetate to obtain a chelating material;
[0010] A matrix material is obtained by mixing γ-glycidyl etheroxypropyltrimethoxysilane, tetraethyl orthosilicate, and isocyanate-based acrylate. An optical treatment material is obtained by mixing the matrix material, diamond treatment solution, and chelating material and reacting them with a solvothermal agent. A photoinitiator and a leveling agent are added to the optical treatment material to obtain an optical coating material. The optical coating material is dip-coated onto the surface of the optical substrate and cured to form a high-hardness, wear-resistant treatment material.
[0011] Preferably, the diamond treatment solution is prepared as follows: 1 part of nano-diamond powder (particle size 4-6 nm, commercially available product, synthesized by detonation method) is placed in 80 parts of a concentrated sulfuric acid / concentrated nitric acid (3:1) mixture and ultrasonically dispersed at 60°C for 1-3 h. Then, it is centrifuged, washed with water until neutral, and vacuum dried to obtain diamond oxide. The diamond oxide is dispersed in anhydrous ethanol (solid concentration 1 mg / mL), and 0.1-0.5 parts of perfluorodecyltriethoxysilane are added. The system is kept acidic, and the reaction is carried out under reflux condensation at 75°C for 10-14 h. Subsequently, some solvent is removed by rotary evaporation, and the solid concentration is concentrated to 10-20 mg / mL to obtain the diamond treatment solution. The concentrated sulfuric acid has a mass fraction of 98%, and the concentrated nitric acid has a mass fraction of 65%.
[0012] Preferably, the preparation method of the chelating material is as follows: In a dry flask, 3-5 parts of aluminum isopropoxide are dissolved in 20 parts of anhydrous isopropanol, and ethyl acetoacetate (EAA) is slowly added dropwise, with an Al:EAA molar ratio of 1:2. The mixture is stirred for 40-50 minutes until the solution is clear and transparent to obtain chelating solution A. In another container, 10-14 parts of zirconium n-propoxide are mixed with EAA, with a Zr:EAA molar ratio of 1:1. The mixture is stirred for 20-40 minutes to obtain chelating solution B. The two chelating solutions are mixed and stirred in a sealed container at room temperature for 1 hour to form the chelating material.
[0013] Preferably, the matrix material is prepared by mixing 60-70 parts of γ-glycidyl etheroxypropyltrimethoxysilane and 30-40 parts of tetraethyl orthosilicate, adding 0.1M HCl dropwise under ice bath conditions, controlling H2O:Si=3.5:1, and aging at 25°C for 22-26 hours after the addition is complete. Then, 8 parts of isocyanate acrylate (AOI) are added, and the reaction is carried out at 60°C for 4 hours to obtain the matrix material.
[0014] Preferably, the optical processing material is prepared by: thoroughly mixing the matrix material, diamond processing solution and chelating material, stirring for 1 hour, and then transferring the mixture to a high-pressure reactor lined with polytetrafluoroethylene for a solvothermal reaction at a temperature of 120°C for 12-16 hours to obtain the optical processing material.
[0015] Preferred preparation method of high-hardness wear-resistant treatment material is as follows: 1-5 parts of photoinitiator 184 and 0.3 parts of leveling agent polyether-modified polydimethylsiloxane (BYK-333) are added to the optical treatment material, and diluted with a mixed solvent to a solid content of 30% and a viscosity of 8 mPa·s to obtain an optical coating material; subsequently, the optical coating material is dip-coated onto the surface of an optical substrate at a pulling speed of 15 cm / min, and UV pre-cured at 365 nm with a power of 450-550 mJ / cm. 2 Then, cure at 80℃ for 20 minutes, and then raise the temperature to 130℃ and cure for 2-3 hours to form a high-hardness wear-resistant material on the surface of the optical substrate.
[0016] Preferably, the mixed solvent is obtained by mixing isopropanol (IPA) and n-butanol, with IPA:n-butanol ratio of 3:1.
[0017] Another aspect of the present invention provides a high-hardness wear-resistant treatment material, comprising a diamond treatment solution, a chelating material and a matrix material, wherein the high-hardness wear-resistant treatment material is an optical coating material.
[0018] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0019] This invention utilizes a solvothermal reaction to induce in-situ growth of aluminum-doped zirconia, employing active sites on the surface of pretreated nanodiamonds as nucleation centers to construct a micro / nano hierarchical structure. This structure is not a simple physical mixture but rather forms a reinforcing system; the aluminum-doped zirconia can be physically anchored in the matrix material. When the optical coating is subjected to impact or bending, it can effectively induce crack deflection and dissipate stress energy, significantly reducing the brittleness of the optical coating and preventing cracking on flexible substrates.
[0020] This invention modifies nanodiamonds with perfluorodecylsilane grafting, utilizing the synergistic effect of fluorine's low surface energy and nanodiamond's ultra-high hardness. During the curing process, fluorine-containing segments spontaneously migrate to the surface of the optical coating, giving it a low coefficient of friction. When external objects rub against the surface of the optical coating, the coating exhibits a smooth exterior and a hard interior, resisting cutting forces through a high-hardness framework and significantly reducing frictional loss through surface self-lubrication, thereby significantly improving the material's wear resistance.
[0021] This invention introduces a mixed chelate formed by aluminum isopropoxide and zirconium n-propoxide to construct a high-density Si-O-Al-O-Zr inorganic network in a sol-gel system. The introduction of aluminum ions not only repairs dangling bond defects in the silicon-oxygen network caused by incomplete polymerization, but also increases the crosslinking density by utilizing their high coordination properties. This ternary hybrid network structure is dense and has a high modulus, which improves the hardness of the cured optical coating and effectively solves the problem of insufficient hardness in existing organosilicon optical coatings due to the loose network.
[0022] This invention employs a process combining UV pre-curing and gradient thermal curing. UV curing rapidly locks in the fluorine-containing layer on the surface and forms a rigid outer shell, while subsequent gradient thermal curing (80°C to 130°C) allows the underlying organic-inorganic network to slowly cross-link, retaining appropriate flexibility to match the thermal expansion coefficient of the substrate. This hard-on-the-outer-hard-on-the-inner curing mode effectively releases the internal stress during the coating formation process, solving the technical defects of poor adhesion and easy detachment of optical coatings on optical substrates.
[0023] Although this invention incorporates high-refractive-index inorganic fillers such as nanodiamond, zirconium oxide, and alumina, precise control of the solvothermal reaction conditions enables the monodispersity of inorganic particles at the molecular level and the growth of zirconium oxide, avoiding macroscopic particle aggregation. Furthermore, aluminum and zirconium elements enhance the refractive index of the matrix, achieving a good match with the refractive index of the nanodiamond. This eliminates light scattering (haze) caused by refractive index mismatch, allowing the final high-hardness, wear-resistant optical coating to maintain extremely high transmittance in the visible light band, fully meeting optical-grade application standards. Attached Figure Description
[0024] Figure 1 The diagram shows the wear resistance and impact resistance of Embodiment 1 and Comparative Examples 1-5 of the present invention. Detailed Implementation
[0025] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0026] This invention provides a high-hardness wear-resistant material and its preparation method, the technical solution of which is as follows:
[0027] Example 1
[0028] One part of nano-diamond powder was placed in a mixture of 80 parts concentrated sulfuric acid / concentrated nitric acid (3:1) and ultrasonically dispersed at 60℃ for 2 hours. Then, it was centrifuged, washed with water until neutral, and vacuum dried to obtain diamond oxide. The diamond oxide was dispersed in anhydrous ethanol, and 0.3 parts of perfluorodecyltriethoxysilane were added to control the system to be acidic. The reaction was carried out at 75℃ under reflux condensation for 12 hours. Then, part of the solvent was removed by rotary evaporation, and the solid concentration was concentrated to 15 mg / mL to obtain the diamond treatment solution.
[0029] In a dry flask, 4 parts of aluminum isopropoxide were dissolved in 20 parts of anhydrous isopropanol, and ethyl acetoacetate (EAA) was slowly added dropwise, with an Al:EAA molar ratio of 1:2. The mixture was stirred for 45 minutes until the solution was clear and transparent, yielding chelate solution A. In another container, 12 parts of zirconium n-propoxide were mixed with EAA, with a Zr:EAA molar ratio of 1:1. The mixture was stirred for 30 minutes to obtain chelate solution B. The two chelate solutions were then mixed and stirred in a sealed container at room temperature for 1 hour to form a chelated material.
[0030] 65 parts of γ-glycidyl oxypropyltrimethoxysilane and 35 parts of tetraethyl orthosilicate were mixed, and 0.1M HCl was added dropwise under ice bath conditions, controlling H2O:Si=3.5:1. After the addition was completed, the mixture was aged at 25℃ for 24h, and then 8 parts of isocyanate acrylate were added and reacted at 60℃ for 4h to obtain the matrix material.
[0031] The matrix material, diamond treatment solution, and chelating material were thoroughly mixed and stirred for 1 hour. The mixture was then transferred to a polytetrafluoroethylene-lined high-pressure reactor for a solvothermal reaction at 120°C for 14 hours to obtain the optical treatment material. Three parts of photoinitiator 184 and 0.3 parts of leveling agent polyether-modified polydimethylsiloxane were added to the optical treatment material, and the mixture was diluted with a mixed solvent to a solid content of 30% and a viscosity of 8 mPa·s to obtain the optical coating material. Subsequently, the optical coating material was dip-coated onto the surface of an optical substrate at a pull-out speed of 15 cm / min, followed by UV pre-curing at 365 nm with a power of 500 mJ / cm². 2 Then, it is cured at 80°C for 20 minutes, and then the temperature is raised to 130°C for 2.5 hours to form a high-hardness wear-resistant material on the surface of the optical substrate.
[0032] Examples 2-5 refer to the parameter conditions in Example 1, with specific differences shown in Table 1.
[0033] Table 1 Parameters and conditions for Examples 1-5
[0034] Example Ultrasonic dispersion time / h Dosage / parts of perfluorodecyltriethoxysilane Reflux condensation time / h Solid concentration / mg / mL Dosage / parts of γ-glycidyl oxypropyltrimethoxysilane Dosage of tetraethyl orthosilicate (parts) ripening time / h Example 1 2 0.3 12 15 65 35 24 Example 2 1 0.1 10 10 60 30 22 Example 3 3 0.2 11 10 62 32 23 Example 4 1 0.4 13 20 68 38 25 Example 5 3 0.5 14 20 70 40 26
[0035] Comparative Example 1 follows the same parameters and conditions as in Example 1, except that the nanodiamonds are not oxidized.
[0036] Comparative Example 2 follows the same parameters and conditions as in Example 1, except that the nanodiamonds are not fluorinated.
[0037] Comparative Example 3 follows the same parameters and conditions as in Example 1, except that the nanodiamonds are not oxidized or fluorinated.
[0038] Comparative Example 4 follows the same parameters and conditions as in Example 1, except that no diamond treatment solution is added.
[0039] Comparative Example 5 follows the same parameters and conditions as in Example 1, except that isocyanate-based acrylates are not added to the matrix material.
[0040] Experimental Example 1: Hardness, Abrasion Resistance and Impact Resistance Tests
[0041] The hardness of Examples 1-5 and Comparative Examples 1-5 was tested according to GB / T 6739-2006 standard; wear tests were conducted on Examples 1-5 and Comparative Examples 1-5, and the wear amount was calculated by measuring the mass change before and after wear; the impact resistance of Examples 1-5 and Comparative Examples 1-5 was tested according to GB / T 1732 standard; the results are shown in Table 2. The wear resistance and impact resistance of Examples 1 and Comparative Examples 1-5 are as follows: Figure 1 As shown.
[0042] Table 2. Hardness, abrasion resistance and impact resistance tests of Examples 1-5 and Comparative Examples 1-5
[0043] Example Hardness / H Wear amount / mg / h Impact resistance / kg·cm Example 1 7 0.45 69.8 Example 2 7 0.51 68.5 Example 3 6 0.48 68.9 Example 4 7 0.46 69.2 Example 5 7 0.49 68.6 Comparative Example 1 5 1.25 52.4 Comparative Example 2 6 0.98 58.6 Comparative Example 3 4 1.85 41.2 Comparative Example 4 3 2.65 45.3 Comparative Example 5 5 1.1 28.5
[0044] From Table 2 and Figure 1It can be observed that the hardness of Comparative Example 1 decreased to 5H, the wear rate increased to 1.25 mg / h, and the impact resistance decreased significantly. This is because the nanodiamonds were not oxidized, and the surface lacked sufficient hydroxyl and carboxyl active sites, resulting in an extremely low grafting rate of subsequent perfluorosilanes and an inability to effectively induce in-situ growth and chemical anchoring of aluminum / zirconium ions in the chelating material. During the coating curing process, the nanodiamonds easily agglomerated and could not be uniformly dispersed in the matrix material. The agglomerated large particles not only failed to play a role in dispersion reinforcement but also became stress concentration points (defects) in the optical coating, causing the coating to easily peel off and microcracks to propagate from the agglomeration points due to weak interfacial bonding when subjected to impact or friction. The hardness of Comparative Example 2 barely maintained 6H, but the wear rate (0.98 mg / h) was about twice that of the example. This is because although oxidation treatment imparts chemical reactivity to diamond, enabling it to form certain bonds with the matrix, the lack of perfluorinated segments results in high surface energy of the nanoparticles and poor dispersion stability in organic solvents. More importantly, the main function of fluorination treatment is to reduce the coefficient of friction of the optical coating surface and impart self-lubricating properties. Without this modification, the frictional resistance of the optical coating surface increases, and the shear force experienced in the wear test increases significantly, leading to faster wear and consumption of the material. Comparative Example 3 has a hardness of only 4H and a wear rate as high as 1.85 mg / h. This is because the original nanodiamond is a heterogeneous impurity in the organic-inorganic hybrid system. Due to the lack of both chemical bonding anchoring and steric hindrance effect from surface modification, the diamond powder severely agglomerates in the matrix. This physical doping not only fails to enhance the structure but also destroys the continuity and density of the siloxane network. In the test, the agglomerates easily detach, leaving pores, causing the coating structure to collapse rapidly. Comparative Example 4 represents the performance of the pure matrix material (sol-gel coating containing aluminum / zirconium doping), which has a hardness of only 3H and the largest wear. This fully illustrates the key role of the diamond treatment fluid as the ultra-hard core in this invention. Although the introduction of aluminum and zirconium improves the cross-linking degree of the sol-gel network, without nanodiamonds as a framework support, the simple organic-inorganic hybrid material cannot resist high-intensity mechanical friction, and its impact resistance is also generally poor due to the lack of toughening mechanisms of nanoparticles (such as crack deflection and pinning effect). The impact resistance of Comparative Example 5 showed a precipitous drop (28.5 kg·cm), and the hardness also decreased. This is because isocyanate-based acrylate (AOI) is a key bridge connecting the inorganic silicon / zirconium / aluminum network and the organic acrylic network. Without this component, the system cannot form an interpenetrating network structure (IPN), resulting in the failure of the UV pre-curing stage, and the inorganic network is mainly formed by thermal curing. Although this inorganic-based structure has a certain rigidity, it is extremely brittle and lacks the flexibility to absorb impact energy. When subjected to external impact, the optical coating cannot undergo microscopic deformation to dissipate energy, but instead fractures directly in a brittle manner.
[0045] Examples 6-9 refer to the parameter conditions in Example 1, with specific differences shown in Table 3.
[0046] Table 3 Parameter conditions for Examples 1 and 6-9
[0047] Example Aluminum isopropoxide dosage / part Stirring time of chelate solution A / min Dosage / parts of zirconium n-propoxide Stirring time of chelate solution B / min Solvent thermal reaction time / h Dosage of photoinitiator 184 per part <![CDATA[Pre-cured power / mJ / cm 2 > Curing time / h Example 1 4 45 12 30 14 3 500 2.5 Example 6 3 40 10 20 12 1 450 2 Example 7 5 50 11 25 13 2 480 2 Example 8 3 50 13 35 15 4 520 3 Example 9 5 40 14 40 16 5 550 3
[0048] Comparative Example 6 follows the same parameters and conditions as in Example 1, except that chelation solution A is not prepared.
[0049] Comparative Example 7 follows the same parameters and conditions as in Example 1, except that chelate solution B is not prepared.
[0050] Comparative Example 8 follows the same parameters and conditions as in Example 1, except that no solvothermal reaction is performed, and the mixture is simply stirred for 24 hours.
[0051] Comparative Example 9 follows the same parameters and conditions as in Example 1, except that no photoinitiator is added.
[0052] Comparative Example 10 follows the same parameters and conditions as in Example 1, except that UV pre-curing is not performed, and gradient curing is performed directly.
[0053] Comparative Example 11 follows the same parameters and conditions as in Example 1, except that gradient curing is not performed and curing is performed directly at 130°C.
[0054] Experiment Example 2: Hardness, Adhesion, and Light Transmittance Tests
[0055] The hardness of Examples 1, 6-9, and Comparative Examples 6-11 was tested according to the test method of Experimental Example 1; the adhesion of Examples 1, 6-9, and Comparative Examples 6-11 was tested according to GB / T9286-2021 standard; the haze (%) of Examples 1, 6-9, and Comparative Examples 6-11 was tested at 25℃. The lower the haze, the better the light transmittance and the less obvious the white fog phenomenon. The results are shown in Table 4.
[0056] Table 4. Hardness, adhesion, and light transmittance tests of Examples 1, 6-9, and Comparative Examples 6-11
[0057] Example Hardness / H Adhesion / Grade Haze at 25℃ (%) Example 1 7 0 0.3 Example 6 6 0 0.5 Example 7 7 0 0.4 Example 8 7 0 0.3 Example 9 7 0 0.4 Comparative Example 6 6 0 1.1 Comparative Example 7 4 0 3.8 Comparative Example 8 5 2 1.9 Comparative Example 9 2 0 0.6 Comparative Example 10 5 0 0.9 Comparative Example 11 6 3 1.5
[0058] Table 4 shows that the hardness of Comparative Example 6 decreased to 6H, while the haze increased to 1.1%. This indicates that aluminum isopropoxide (chelate A) played a crucial role in densification and refractive index fine-tuning in the system. The lack of an aluminum source, while providing basic hardness with zirconium oxide, resulted in insufficient film density due to the lack of aluminum ions to repair defects in the silicon-oxygen framework. More importantly, the absence of alumina prevented the refractive index of the matrix material from being precisely matched to that of nanodiamonds, leading to a larger refractive index difference between the matrix and the filler, which in turn caused enhanced Rayleigh scattering, manifested as a significant increase in haze. Comparative Example 7 exhibited a precipitous drop in performance, with a hardness of only 4H and a haze as high as 3.8%. This is because zirconium propoxide (chelate B) is the core inorganic component in this scheme for improving hardness and refractive index. Without a zirconium source, the film essentially degenerates into a common organosilicon coating with low intrinsic hardness. Simultaneously, the refractive index of pure organosilicon resin is lower than that of nanodiamonds; this refractive index mismatch leads to light scattering, causing the coating to lose transparency and fail to meet optical-grade requirements. Comparative Example 8 showed decreased adhesion (level 2), a drop in hardness to 5H, and increased haze. This demonstrates that the solvothermal reaction is not a simple physical mixing process, but a crucial step in inducing the growth and chemical bonding of aluminum-doped zirconia. With only simple stirring, the aluminum / zirconia precursor failed to grow in situ using nanodiamonds as nuclei, instead nucleating independently or physically agglomerating. This physical doping resulted in weak interfacial bonding between the inorganic and organic phases, making phase separation (poor adhesion) more likely under stress. Simultaneously, uncoated and undispersed nanoparticles were more prone to agglomeration, leading to increased haze. Comparative Example 9 exhibited extremely low hardness (2H), approaching an uncured state. This was because the lack of a photoinitiator caused the UV pre-curing step to fail, preventing the acrylate double bonds in the system from undergoing free radical polymerization to form the first network. The subsequent thermal curing to form a siloxane network was insufficient to support the mechanical strength of the entire film, and the remaining unreacted organic monomers acted as plasticizers, softening the coating. Comparative Example 10 had a hardness of 5H, with a slight increase in haze. Without UV pre-curing, the coating remains in a flowing liquid state before entering the thermal curing stage. During heating, although the low surface energy fluorine-containing components migrate, the lack of rapid locking through UV cross-linking results in an unstable surface structure. Furthermore, the unlocked inorganic particles are prone to secondary micro-agglomeration under thermal motion, leading to an uneven microstructure, which reduces the final hardness and increases light scattering. Comparative Example 11 exhibits severe adhesion failure (level 4, large-area peeling) and high haze, typical of thermal stress damage. Directly placing the coating at 130°C causes the solvent to boil and evaporate, resulting in numerous micropores within the film (increasing haze). Simultaneously, the rapid contraction of the organic-inorganic network prevents the release of enormous internal stress, far exceeding the interfacial bonding force between the coating and the substrate, making the coating extremely prone to brittle peeling during testing. Gradient curing is a necessary process to ensure stress-free film formation of thick-film optical coatings.
[0059] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a high-hardness, wear-resistant material, characterized in that, Includes the following steps: A diamond treatment solution is obtained by oxidizing and fluorinating nanodiamonds. Aluminum isopropoxide and zirconium n-propoxide were dissolved in ethyl acetoacetate to obtain a chelating material; A matrix material is obtained by mixing γ-glycidyl etheroxypropyltrimethoxysilane, tetraethyl orthosilicate, and isocyanate-based acrylate. The matrix material, the diamond treatment solution, and the chelating material are mixed and subjected to a solvothermal reaction to obtain an optical treatment material. A photoinitiator and a leveling agent are added to the optical treatment material to obtain an optical coating material. The optical coating material is dip-coated onto the surface of an optical substrate and cured to form the high-hardness, wear-resistant treatment material.
2. The method for preparing a high-hardness wear-resistant material according to claim 1, characterized in that, The specific process of oxidation and fluorination is as follows: nano-diamond powder is placed in a mixture of concentrated sulfuric acid and concentrated nitric acid, ultrasonically dispersed, centrifuged and washed, and vacuum dried to obtain diamond oxide; the diamond oxide is dispersed in anhydrous ethanol, perfluorodecyltriethoxysilane is added, refluxed and condensed, and rotary evaporated to obtain the diamond treatment solution.
3. The method for preparing a high-hardness wear-resistant material according to claim 1, characterized in that, The preparation method of the chelating material is as follows: dissolve aluminum isopropoxide in anhydrous isopropanol, add ethyl acetoacetate dropwise to obtain chelating solution A; mix zirconium n-propoxide with ethyl acetoacetate and stir to obtain chelating solution B; mix chelating solution A and chelating solution B, seal and stir to form the chelating material.
4. The method for preparing a high-hardness wear-resistant material according to claim 1, characterized in that, The matrix material is prepared by mixing the γ-glycidyl etheroxypropyltrimethoxysilane and the tetraethyl orthosilicate, adding HCl dropwise under ice bath conditions, aging, and then adding isocyanate acrylate to react and obtain the matrix material.
5. The method for preparing a high-hardness wear-resistant material according to claim 1, characterized in that, The specific process of the solvothermal reaction is as follows: the matrix material, the diamond treatment solution and the chelating material are thoroughly mixed and transferred to a reaction vessel for solvothermal reaction. The reaction time is 12-16 hours to obtain the optical treatment material.
6. The method for preparing a high-hardness wear-resistant material according to claim 1, characterized in that, The specific process of the curing treatment is as follows: photoinitiator 184 and leveling agent polyether modified polydimethylsiloxane are added to the optical treatment material and diluted with a mixed solvent to obtain the optical coating material; the optical coating material is dipped onto the surface of the optical substrate, and then UV pre-cured and gradient cured to form the high-hardness wear-resistant treatment material on the surface of the optical substrate.
7. A high-hardness, wear-resistant treated material, characterized in that: The high-hardness wear-resistant material is prepared by the preparation method described in any one of claims 1-6; the high-hardness wear-resistant material includes a diamond treatment solution, a chelating material, and a matrix material.
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