Zirconia dispersion as well as preparation method and application thereof
By using zirconia raw materials with specific pore volume and size, and combining them with dispersants and resins, the zirconia dispersion achieves stable and durable thin films with enhanced weather resistance and optical performance.
Patent Information
- Application Number
- JP2025095828
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-06-14
- Filing Date
- 2025-06-09
- Publication Date
- 2025-12-25
AI Technical Summary
Zirconia-based film products exhibit poor weather resistance and optical performance due to high pore volume and pore size in zirconia dispersions, leading to reduced stability and service life.
A zirconia dispersion is prepared using zirconia raw materials with a pore volume of 0.3 cm³/g or less and pore size of 12 nm or less, combined with a dispersant and resin component, and surface-modified with organic compounds to enhance stability and optical properties.
The resulting thin films demonstrate excellent weather resistance and optical performance, maintaining a light attenuation rate of 2% or less after a 240-hour test at 85°C and 85% humidity, with improved service life and optical path adjustment capabilities.
Smart Images

Figure 2025188032000001
Abstract
Description
[Technical Field]
[0001] The present invention is in the technical field of zirconia materials, and specifically relates to zirconia dispersions, their preparation methods and uses. [Background technology]
[0002] Zirconia nanoparticles have characteristics such as a high refractive index, good optical transparency in the visible light range, good abrasion resistance, and excellent corrosion resistance, and in recent years have often been combined with resins to prepare stable nano-dispersions for use in various optical fields. However, in the prior art, film products prepared with zirconia dispersions have poor weather resistance and therefore poor optical performance. It is with this in mind that the present invention is provided. Summary of the Invention
[0003] The present invention aims to provide a zirconia dispersion, its preparation method and use, which solves or improves the above technical problems.
[0004] The present invention is realized as follows. In a first aspect, the present invention provides a zirconia dispersion, the zirconia dispersion comprising a zirconia component, a dispersant, and a resin component, The zirconia raw material used as the zirconia component has a pore volume of 0.3 cm 3 / g or less and the pore size is 12 nm or less.
[0005] In an alternative embodiment, the average particle size of the zirconia raw material is 1 nm to 50 nm. In an alternative embodiment, the average particle size of the zirconia raw material is 5 nm to 20 nm. In an alternative embodiment, the content of the zirconia raw material in the zirconia dispersion is 40 wt% to 75 wt%. In an alternative embodiment, the content of the zirconia raw material in the zirconia dispersion is 45 wt% to 70 wt%.
[0006] In an alternative embodiment, the content of the zirconia raw material in the zirconia dispersion is 50 wt% to 65 wt%. In an alternative embodiment, the amount of dispersant used is 1 wt% to 20 wt% of the zirconia raw material, and preferably 5 wt% to 10 wt%. In an alternative embodiment, the zirconia component is obtained by modifying a zirconia raw material with a surface modifier. In an alternative embodiment, the amount of the surface modifier used is 1 wt% to 30 wt% of the zirconia raw material, and preferably 5 wt% to 20 wt%.
[0007] In alternative embodiments, the surface modifier comprises at least one of an organic acid compound, a phosphonic acid compound, a coupling agent, and a chelating agent. In an alternative embodiment, the coupling agent is a silane coupling agent, or the organic acid compound is an organic acid modifier having a double bond. In an alternative embodiment, the resin component is an optical resin. In an alternative embodiment, the resin component is a UV-curable acrylic resin.
[0008] In a second aspect, the present invention provides a method for preparing a zirconia dispersion according to any one of the above embodiments, comprising the steps of mixing a mixed solution containing an organic solvent, a zirconia component, and a dispersant with a resin component, and removing the organic solvent. In an alternative embodiment, the content of the zirconia raw material in the mixed solution is 10 wt% to 80 wt%, preferably 20 wt% to 50 wt%, and more preferably 20 wt% to 30 wt%.
[0009] In an alternative embodiment, the organic solvent includes at least one of an alcohol, a ketone, an ether, an ester, an aliphatic hydrocarbon, an alicyclic hydrocarbon, and an aromatic solvent, and more preferably, the organic solvent includes at least one of propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, toluene, methyl ethyl ketone, and butyl acetate.
[0010] In a third aspect, the present invention provides an optical path adjustment coating layer, wherein raw materials for preparing the optical path adjustment coating layer include a zirconia dispersion according to any one of the above embodiments.
[0011] In an alternative embodiment, the raw materials for preparing the light path control coating layer further include an initiator. In an alternative embodiment, when the resin component is a UV-curable acrylic resin, the initiator is a photoinitiator. In an alternative embodiment, the amount of photoinitiator used is 1 wt % to 5 wt % of the zirconia dispersion.
[0012] In a fourth aspect, the present invention provides a method for preparing an optical path adjustment coating layer according to any one of the above embodiments, comprising applying a raw material for preparing the optical path adjustment coating layer to a surface of a substrate and curing the raw material. In an alternative embodiment, the light transmittance of the substrate is 89% or greater, preferably 90% or greater. In alternative embodiments, the substrate comprises polyethylene terephthalate, triacetate cellulose, polycarbonate, or polymethyl methacrylate.
[0013] In a fifth aspect, the present invention provides a use of an optical path adjustment coating layer according to any one of the above embodiments, wherein the optical path adjustment coating layer can be used to adjust an optical path; In alternative embodiments, the light path adjusting coating layer can be used in LCD modules, lenses, camera modules, cameras, architectural glass, or optical adhesives.
[0014] The present invention includes the following beneficial effects: The present invention is directed to a pore volume of 0.3 cm 3 By preparing a zirconia dispersion using a zirconia raw material with a density of 0.1 / g or less and a pore diameter of 12 nm or less, the resulting thin film, after being subjected to a 240-hour weathering test at 85°C and 85% humidity, maintained a light attenuation rate of 2% or less, demonstrating relatively good weathering stability, a relatively long service life, and suitability for adjusting the optical path. The larger the pore volume and pore diameter of the zirconia raw material, the smaller the mass ratio of zirconia at the same volume ratio after film formation. On the other hand, the larger the pore volume and pore diameter, the more likely pores will form during the crosslinking and curing process of the dispersion. As a result, the weathering resistance of the film after formation is poor, and the optical performance of the thin film is reduced. DETAILED DESCRIPTION OF THE INVENTION
[0015] In order to more clearly explain the objectives, technical solutions and advantages of the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely explained below. In the examples, the specific conditions not specified can be carried out under conventional conditions or conditions recommended by the manufacturer. For reagents or equipment whose manufacturers are not specified, conventional products available on the market can be used.
[0016] The zirconia dispersion according to the present invention, its preparation method, and use will now be described in detail. The present invention provides a zirconia dispersion, which includes a zirconia component, a dispersant, and a resin component. The zirconia raw material used as the zirconia component has a pore volume of 0.3 cm 3 / g or less and the pore size is 12 nm or less.
[0017] Zirconia dispersions prepared from zirconia raw materials vary in their weather resistance after film formation depending on their pore volume and pore size, and this influence is relatively significant. The present invention prepares a zirconia dispersion using a zirconia raw material having the above-mentioned pore volume and pore size. After forming a film from the zirconia dispersion, the resulting thin film maintains a light attenuation rate of 2% or less after a 240-hour weathering test at 85°C and 85% humidity, demonstrating relatively good weather resistance stability and a relatively long service life. The larger the pore volume and pore size of the zirconia raw material, the smaller the mass ratio of zirconia at the same volume ratio after film formation. On the other hand, the larger the pore volume and pore size, the more likely pores will form during the crosslinking and curing process of the dispersion. As a result, the weather resistance of the film after formation is poor, and the optical performance of the thin film is reduced.
[0018] In some alternative embodiments, the pore volume of the zirconia raw material is 0.0372 cm 3 / g, 0.0746cm 3 / g, 0.1163cm 3 / g, 0.1853cm 3 / g, 0.2012cm 3 / g, 0.2139cm 3 / g, 0.2427cm 3 / g, 0.2681cm 3 / g, 0.2801cm 3 / g or 0.2924cm 3 / g, etc., and 3 Other values in the range of 0.15 to 1 / g may also be used.
[0019] In some alternative embodiments, the pore size of the zirconia raw material may be 0.8645 nm, 1.1645 nm, 3.1145 nm, 5.4552 nm, 6.8235 nm, 8.2648 nm, 9.6626 nm, 10.0456 nm, 10.5896 nm, or 11.7823 nm, or other values within the range of 12 nm or less.
[0020] In some embodiments, the average particle size of the zirconia raw material is 1 nm to 50 nm, such as 1 nm, 5 nm, 10 nm, 15 nm, 20 nm, 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, or 50 nm, or other values within the range of 1 nm to 50 nm, in some preferred embodiments, the average particle size of the zirconia raw material is 5 nm to 20 nm.
[0021] In the present invention, the crystal type of the zirconia raw material is not limited, and when used, zirconia raw material of a crystal type such as monoclinic, tetragonal or mixed crystal can be used. In the present invention, the content of the zirconia raw material in the zirconia dispersion is 40 wt% to 75 wt%, for example, 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, or 75 wt%, or may be other values within the range of 40 wt% to 75 wt%. In some preferred embodiments, the content of the zirconia raw material in the zirconia dispersion is 45 wt% to 70 wt%. In some more preferred embodiments, the content of the zirconia raw material in the zirconia dispersion is 50 wt% to 65 wt%.
[0022] If the content of the zirconia raw material in the zirconia dispersion is less than 40 wt%, the refractive index of the prepared dispersion is relatively low, which is unfavorable for adjusting the optical path, whereas if the content of the zirconia raw material in the zirconia dispersion is more than 75 wt%, the zirconia content exceeds the upper limit, making it impossible to obtain a dispersion.
[0023] In the present invention, the zirconia component is obtained by modifying a zirconia raw material with a surface modifier. By performing surface modification on the zirconia raw material, the surface properties of the zirconia raw material can be improved and groups that have an affinity for the resin can be grafted onto the surface. The method of surface modification is not limited, and examples thereof include polishing, heating, mixing and stirring, etc.
[0024] The type of surface modifier is not limited as long as it has affinity for the resin. In some embodiments, the surface modifier includes at least one of an organic acid compound having various groups, a phosphonic acid compound, a coupling agent, and a chelating agent.
[0025] In some preferred embodiments, the surface modifier includes at least one of a coupling agent and an organic acid modifier. The coupling agent is preferably a silane coupling agent, such as a silane containing a group such as an acrylate group, a (meth)acrylic group, an epoxy group, an alkyl group, an alkoxyl group, a vinyl group, a phenyl group, a methacryloxy group, an amino group, a chlorosilane group, a chloropropyl group, or a sulfhydryl group. The organic acid compound is preferably an organic acid modifier having a double bond, such as at least one of acrylic acid, methacrylic acid, ethylacrylic acid, α-acrylic acid, β-methacrylic acid, α-phenylacrylic acid, β-acryloxypropionic acid, sorbic acid, α-chlorosorbic acid, angelic acid, cinnamic acid, β-styrylacrylic acid, itaconic acid, maleic acid, citraconic acid, mesaconic acid, glutaconic acid, aconitic acid, and fumaric acid.
[0026] In some embodiments, the amount of surface modifier used is 1 wt% to 30 wt% of the zirconia raw material, such as 1 wt%, 5 wt%, 10 wt%, 15 wt%, 20 wt%, 25 wt%, or 30 wt%, or other values within the range of 1 wt% to 30 wt%. In some preferred embodiments, the amount of surface modifier used is 5 wt% to 20 wt% of the zirconia raw material.
[0027] In the present invention, the dispersant plays a role in assisting dispersion and wetting. In the present invention, the dispersion method is not particularly limited, and methods such as ultrasonic waves, stirring, and grinding can be used. In addition, in the present invention, the type of dispersant is not limited, and various commercially available models and types of dispersants can be used. Various dispersants can be used individually or in combination.
[0028] In some alternative embodiments, the dispersant includes, by way of example and not limitation, at least one of BYK-P104, BYK-220S, BYK-110, BYK-111, BYK-170, BYK-171, BYK-180, BYK-181, BYK-174, BYK-2095, EFKA5010, EFKA5065, EFKA5066, EFKA5070, EFKA7500, EFKA7554, Solsperse 3000, Sol-sperse 16000, Sol-sperse 17000, Sol-sperse 18000, Sol-sperse 36000, Sol-sperse 36600, and Sol-sperse 4100.
[0029] In some alternative embodiments, the amount of dispersant used is 1 wt% to 20 wt% of the zirconia raw material, such as 1 wt%, 2 wt%, 5 wt%, 8 wt%, 10 wt%, 12 wt%, 15 wt%, 18 wt%, or 20 wt%, or other values within the range of 1 wt% to 20 wt%. In some preferred embodiments, the amount of dispersant used is 5 wt% to 10 wt% of the zirconia raw material.
[0030] In the present invention, the resin component is an optical resin. In some preferred embodiments, the resin component is an ultraviolet-curable acrylic resin, and examples thereof include, but are not limited to, benzyl acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl acrylate, phenyl methacrylate, biphenyl methacrylate, 2-acrylic acid nitrophenyl ester, 4-methacrylic acid nitrophenyl ester, 2-methacrylic acid nitrobenzyl ester, 4-methacrylic acid nitrobenzyl ester, 2-acrylic acid chlorophenyl ester, 4-acrylic acid chlorophenyl ester, 2-meth ... and at least one of methyl acrylate, methyl meth ...
[0031] In some embodiments, the amount of resin used can be obtained by subtracting the total content of the zirconia raw material, surface modifier, and dispersant in the zirconia dispersion from 100%.
[0032] The present invention further provides a method for preparing the above-mentioned zirconia dispersion, which comprises the steps of mixing a mixed solution containing an organic solvent, a zirconia component, and a dispersant with a resin component, and then removing the organic solvent.
[0033] In some embodiments, first, a zirconia raw material is modified with a surface modifier to obtain a zirconia component, the zirconia component, a dispersant, and an organic solvent are mixed to obtain a mixed solution, the mixed solution is mixed with a resin component, and the organic solvent is removed to obtain a zirconia dispersion.
[0034] In some embodiments, the content of the zirconia raw material in the mixed solution is 10 wt% to 80 wt%, such as 10 wt%, 20 wt%, 30 wt%, 40 wt%, 50 wt%, 60 wt%, 70 wt%, or 80 wt%, or may be other values within the range of 10 wt% to 80 wt%. In some preferred embodiments, the content of the zirconia raw material in the mixed solution is 20 wt% to 50 wt%. In some more preferred embodiments, the content of the zirconia raw material in the mixed solution is 20 wt% to 30 wt%.
[0035] In some embodiments, the amount of organic solvent used can be obtained by subtracting the total content of the zirconia raw material, the surface modifier, and the dispersant in the mixed solution from 100%.
[0036] In the present invention, the organic solvent is not specifically limited. In some embodiments, the organic solvent comprises at least one of alcohols, ketones, ethers, esters, aliphatic hydrocarbons, alicyclic hydrocarbons, and aromatics. In some preferred embodiments, the organic solvent comprises at least one of propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, toluene, methyl ethyl ketone, and butyl acetate.
[0037] In the present invention, the method for removing the organic solvent is not particularly limited, and for example and without limitation, the organic solvent can be removed by using a rotary evaporator or other vacuum rectification equipment.
[0038] The present invention further provides an optical path adjustment coating layer, wherein raw materials for preparing the optical path adjustment coating layer include the above-described zirconia dispersion. Furthermore, the raw materials for preparing the optical path adjusting coating layer further include an initiator. In an alternative embodiment, when the resin component is a UV-curable acrylic resin, the initiator is a photoinitiator.
[0039] The photoinitiator used in the present invention is not particularly limited. In some embodiments, the photoinitiator includes at least one cationic photoinitiator, such as a diazonium salt, a sulfonium salt, or an imidazole. In other embodiments, the photoinitiator includes at least one radical photoinitiator, such as a phosphorus-based, triazine-based, benzophenone-based, benzoin-based, oxime-based, acetone-based, aminoketone-based, ketone-based, anthraquinone-based, or aromatic phosphine oxide compound. In some preferred embodiments, the photoinitiator includes at least one of TPO, 1173, 184, and 907.
[0040] In some embodiments, the amount of photoinitiator used is between 1 wt% and 5 wt% of the zirconia dispersion, such as 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, or 5 wt%, or other values within the range of 1 wt% to 5 wt%.
[0041] The present invention further provides a method for preparing the above-mentioned light path adjustment coating layer, which comprises the steps of applying a raw material for preparing the light path adjustment coating layer to the surface of a substrate and curing it. The coating method is not particularly limited, and examples thereof include roll coating, spray coating, curtain coating, and spin coating. The substrate to be coated is not particularly limited, but is preferably a substrate with high transmittance. In some embodiments, the substrate has a light transmittance of 89% or more, preferably 90% or more. In some specific embodiments, the substrate includes polyethylene terephthalate, triacetate cellulose, polycarbonate, polymethyl methacrylate, or the like.
[0042] Curing can be achieved by means of, for example and without limitation, mercury vapor lamps and LEDs. The present invention also provides a use of the above-mentioned light path adjusting coating layer, which can be used to adjust the light path. In some embodiments, the light path adjusting coating layer can be used in an LCD module, a lens, a camera module, a camera, architectural glass, or an optical adhesive.
[0043] The features and performance of the present invention will be described in more detail below with reference to examples. Example 1
[0044] The present invention provides a light path adjustment coating layer, and a method for preparing the light path adjustment coating layer includes the following steps: Step 1: 50 g of zirconia raw material powder (pore volume: 0.0372 cm) was mixed with 5 g of 3-(methacryloyloxy)propyltrimethoxysilane as a silane coupling agent. 3 Modified zirconia was obtained by modifying the zirconia (pore size: 0.8645 nm, average particle size: 10 nm) to obtain modified zirconia. The modified zirconia was dispersed in an organic solvent, propylene glycol monomethyl ether, by ball milling using 2.5 g of BYK-110 as a dispersant to obtain a mixed solution. The content of the zirconia raw material powder in the mixed solution was 30 wt%. Step 2: 42.5 g of 3-phenoxybenzyl acrylate was taken as a resin component and added to the above mixed solution, and the propylene glycol monomethyl ether was removed using a rotary evaporator to obtain a zirconia dispersion. Step 3: 2 wt % of TPO, a photoinitiator, was added to the above zirconia dispersion, and the mixture was applied to PET and photocured to form a film, thereby obtaining an optical path adjusting coating layer.
[0045] Example 2 This example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.0746 cm 3 / g and the pore size was 1.1645 nm.
[0046] Example 3 This example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.1163 cm 3 / g, and the pore size was 3.1145 nm. The dispersant was BYK-180. The resin component was benzyl acrylate. The amount of TPO used as the photoinitiator was 3 wt% of the zirconia dispersion.
[0047] Example 4 This example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.1853 cm 3 / g, and the pore size was 5.4552 nm. The dispersant was BYK-111. The resin component was biphenylmethanol acrylate. The amount of TPO used as the photoinitiator was 3 wt% of the zirconia dispersion.
[0048] Example 5 This example differs from Example 1 in the following respects: The zirconia raw material powder has a pore volume of 0.2012 cm 3 / g, and the pore size was 6.8235 nm. The silane coupling agent was 3-glycidyloxypropyltrimethoxysilane. The content of zirconia raw material powder in the mixed solution was 40 wt%. The amount of resin component used was 25.8 g. The amount of photoinitiator TPO used was 3 wt% of the zirconia dispersion.
[0049] Example 6 This example differs from Example 5 in the following respects: The zirconia raw material powder had a pore volume of 0.2139 cm 3 The resin component was used in an amount of 19 g.
[0050] Example 7 This example differs from Example 6 in the following respects: The zirconia raw material powder had a pore volume of 0.2427 cm 3 / g and the pore size was 9.6626 nm.
[0051] Example 8 This example differs from Example 5 in the following respects: The zirconia raw material powder had a pore volume of 0.2681 cm 3 / g and the pore size was 10.0456 nm.
[0052] Example 9 This example differs from Example 5 in the following respects: The zirconia raw material powder had a pore volume of 0.2801 cm 3 The resin component was used in an amount of 19 g.
[0053] Example 10 This example differs from Example 5 in the following respects: The zirconia raw material powder had a pore volume of 0.2924 cm 3 / g and the pore size was 11.7823 nm.
[0054] Comparative Example 1 This comparative example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.3111 cm 3 / g and the pore size was 12.5326 nm.
[0055] Comparative Example 2 This comparative example differs from Example 2 in the following respects: The zirconia raw material powder had a pore volume of 0.3526 cm 3 / g and the pore size was 12.8252 nm.
[0056] Comparative Example 3 This comparative example differs from Example 3 in the following respects: The zirconia raw material powder had a pore volume of 0.3889 cm 3 / g and the pore size was 13.7567 nm.
[0057] Comparative Example 4 This comparative example differs from Example 4 in the following respects: The zirconia raw material powder had a pore volume of 0.4270 cm 3 / g and the pore size was 14.2333 nm.
[0058] Comparative Example 5 This comparative example differs from Example 5 in the following respects: The zirconia raw material powder had a pore volume of 0.4611 cm 3 / g and the pore size was 14.8749 nm.
[0059] Comparative Example 6 This comparative example differs from Example 6 in the following respects: The zirconia raw material powder had a pore volume of 0.4985 cm 3 / g and the pore size was 15.5744 nm.
[0060] Comparative Example 7 This comparative example differs from Example 7 in the following respects: The zirconia raw material powder had a pore volume of 0.5331 cm 3 / g and the pore size was 16.2365 nm.
[0061] Comparative Example 8 This comparative example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.2872 cm 3 / g and the pore size was 13.5231 nm.
[0062] Comparative Example 9 This comparative example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.3472 cm 3 / g and the pore size was 11.0645 nm.
[0063] Comparative Example 10 In the preparation of this comparative example, the zirconia content in the system was 76 wt %, and as a result, a zirconia dispersion could not be obtained at this content.
[0064] The specific preparation steps include the following steps: Step 1: 50 g of zirconia raw material powder (pore volume: 0.0372 cm) was mixed with 5 g of 3-(methacryloyloxy)propyltrimethoxysilane as a silane coupling agent. 3Modified zirconia was obtained by modifying the zirconia (pore size: 0.8645 nm, average particle size: 10 nm) to obtain modified zirconia. The modified zirconia was dispersed in an organic solvent, propylene glycol monomethyl ether, by ball milling using 2.5 g of BYK-110 as a dispersant to obtain a mixed solution. The content of the zirconia raw material powder in the mixed solution was 30 wt%.
[0065] Step 2: 8.29 g of 3-phenoxybenzyl acrylate was added to the above mixed solution as a resin component, and propylene glycol monomethyl ether was used in a rotary evaporator to obtain a zirconia dispersion (the zirconia content in the system was 76 wt%).
[0066] Test Example The optical path adjustment coating layers prepared in Examples 1 to 10 and Comparative Examples 1 to 9 were each subjected to a weathering test for 240 hours at a temperature of 85°C and a humidity of 85%, and then the optical attenuation rate of the thin film was measured. The results are shown in Table 1.
[0067] [Table 1]
[0068] As can be seen from Table 1, after a 240-hour weather resistance test under conditions of a temperature of 85°C and a humidity of 85%, the optical path adjustment coating layers prepared in Examples 1 to 10 maintained an optical attenuation rate of 2% or less and had better weather resistance stability than the optical path adjustment coating layers prepared in Comparative Examples 1 to 10.
[0069] As mentioned above, the present invention provides a porous membrane having a pore volume of 0.3 cm 3By preparing a zirconia dispersion using a zirconia raw material with a densification rate of 0.1% or less and a pore size of 12 nm or less, the zirconia dispersion can be formed into a thin film. After a 240-hour weathering test at a temperature of 85°C and a humidity of 85%, the thin film maintains an optical attenuation rate of 2% or less, exhibiting relatively good weathering stability and a relatively long service life. The thin film can be used to adjust the optical path and can be used in LCD modules, lenses, camera modules, cameras, architectural glass, or optical adhesives.
[0070] The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. Those skilled in the art will appreciate that the present invention may have various modifications and variations. Any modifications, equivalent replacements, improvements, etc. made without departing from the spirit and principle of the present invention are within the scope of protection of the present invention.
Claims
1. A zirconia dispersion comprising: The zirconia dispersion contains a zirconia component, a dispersant, and a resin component, The zirconia raw material used as the zirconia component has a pore volume of 0.3 cm 3 / g or less, and the pore size is 12 nm or less A zirconia dispersion characterized by:
2. The average particle size of the zirconia raw material is 1 nm to 50 nm, Preferably, the average particle size of the zirconia raw material is 5 nm to 20 nm. The zirconia dispersion according to claim 1 .
3. The content of the zirconia raw material in the zirconia dispersion is 40 wt % to 75 wt %; Preferably, the content of the zirconia raw material in the zirconia dispersion is 45 wt % to 70 wt %; More preferably, the content of the zirconia raw material in the zirconia dispersion is 50 wt % to 65 wt %. The zirconia dispersion according to claim 1 .
4. The zirconia component is obtained by modifying the zirconia raw material with a surface modifier, Preferably, the amount of the surface modifier used is 1 wt % to 30 wt % of the zirconia raw material, more preferably 5 wt % to 20 wt %; Preferably, the surface modifier includes at least one of an organic acid compound, a phosphonic acid compound, a coupling agent, and a chelating agent, More preferably, the coupling agent is a silane coupling agent, or the organic acid compound is an organic acid modifier having a double bond. The zirconia dispersion according to any one of claims 1 to 3.
5. The amount of the dispersant used is 1 wt % to 20 wt % of the zirconia raw material, and more preferably 5 wt % to 10 wt %. The zirconia dispersion according to any one of claims 1 to 3.
6. the resin component is an optical resin, Preferably, the resin component is an ultraviolet-curable acrylic resin. The zirconia dispersion according to any one of claims 1 to 3.
7. A method for preparing the zirconia dispersion according to any one of claims 1 to 3, comprising: a step of mixing a mixed solution containing an organic solvent, a zirconia component, and a dispersant with a resin component, and removing the organic solvent; Preferably, the content of the zirconia raw material in the mixed solution is 10 wt % to 80 wt %, more preferably, the content of the zirconia raw material in the mixed solution is 20 wt % to 50 wt %, and even more preferably, the content of the zirconia raw material in the mixed solution is 20 wt % to 30 wt %; Preferably, the organic solvent includes at least one of alcohols, ketones, ethers, esters, aliphatic hydrocarbons, alicyclic hydrocarbons, and aromatic solvents, and more preferably, the organic solvent includes at least one of propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, toluene, methyl ethyl ketone, and butyl acetate. A method for preparing a zirconia dispersion, comprising:
8. An optical path adjustment coating layer, The raw material for preparing the optical path adjusting coating layer contains the zirconia dispersion according to any one of claims 1 to 3, Preferably, the raw materials for preparing the optical path adjusting coating layer further include an initiator, Preferably, when the resin component is an ultraviolet-curable acrylic resin, the initiator is a photoinitiator; Preferably, the amount of the photoinitiator used is 1 wt % to 5 wt % of the zirconia dispersion. An optical path adjusting coating layer characterized by:
9. 9. A method for preparing an optical path adjusting coating layer according to claim 8, comprising: A step of applying a raw material for preparing the optical path adjustment coating layer to a surface of a substrate and curing the raw material; Preferably, the light transmittance of the substrate is 89% or more, preferably 90% or more; Preferably, the substrate comprises polyethylene terephthalate, triacetate cellulose, polycarbonate, or polymethyl methacrylate.
1. A method for preparing an optical path adjusting coating layer, comprising:
10. Use of the optical path adjustment coating layer according to claim 8, The optical path adjusting coating layer can be used to adjust the optical path, Preferably, the light path adjusting coating layer can be used in LCD modules, lenses, camera modules, cameras, architectural glass, or optical adhesives.
1. Use of a light path adjusting coating layer.
Citation Information
Patent Citations
Method for synthesizing metal oxide with high specific surface area and high porosity, resulting oxide, and catalyst containing said oxide
JP1993501102A
High specific surface area zirconium oxide material and its manufacturing method
JP2001253714A
Highly durable spherical inorganic porous body and production method therefor
JP2003300719A
Manganese-based ozone decomposition catalyst and method for producing the same
JP2006525112A
Transparent zirconia dispersion liquid, transparent composite material and method for producing transparent composite material
JP2007099931A