High-adhesion ultraviolet curing glue and preparation method thereof

Abstract

The invention provides high-adhesion ultraviolet curing glue and a preparation method thereof, and the high-adhesion ultraviolet curing glue comprises the following components by mass: 4-90% of an oligomer, 0-40% of a photocuring monomer, 0.05-10% of a photoinitiator, 0.05-10% of a leveling agent, and 30-90% of a titanium oxide nanoparticle dispersion liquid or a zirconium oxide nanoparticle dispersion liquid. And the oligomer adopts a polyurethane acrylate polymer with a hydroxyl value of more than or equal to 50. According to the present invention, 4-90% by mass of the oligomer is added to the glue, and the oligomer adopts the urethane acrylate polymer with the hydroxyl value of more than or equal to 50, such that the polarity of the polyurethane material is weakened through the large amount of the hydroxyl contained in the oligomer so as to improve the adhesion of the ultraviolet light curing glue to the waveguide substrate adopting the polyurethane material.

Description

Technical Field

[0001] This invention relates to the field of AR diffraction waveguide fabrication technology, specifically to a high-adhesion UV-curable adhesive and its preparation method. Background Technology

[0002] The existing methods for fabricating diffractive waveguides are generally as follows: 1. Prepare an imprint master with a preset grating structure.

[0003] 2. The grating structure of the embossing master is transferred to the soft film substrate through a nanoimprinting process to obtain a soft film plate with an inverse structure of grating structure.

[0004] Specifically, an imprinting adhesive is uniformly spin-coated onto an imprinting master, a soft film substrate is bonded to the imprinting master, and pressure is applied to fill the grating structure of the imprinting master with the imprinting adhesive, resulting in an inverse structure of the grating structure on the imprinting adhesive. The imprinting adhesive with the inverse structure of the grating structure is then cured and demolded using ultraviolet light, and transferred to the soft film substrate to obtain a soft film plate with an inverse structure of the grating structure.

[0005] 3. The inverse structure of the grating structure on the flexible film plate is transferred onto the waveguide substrate using a nanoimprinting process to obtain a diffractive waveguide.

[0006] Specifically, an tackifier and a product adhesive (UV-curable adhesive) are sequentially spin-coated onto a waveguide substrate (glass wafer substrate / polyurethane substrate). A flexible film with a grating structure inverse is then bonded to the product adhesive on the waveguide substrate (glass wafer substrate / polyurethane substrate). Pressure is applied to fill the grating structure inverse onto the flexible film, resulting in a grating structure on the product adhesive. UV curing and demolding are then performed to separate the flexible film with the grating structure inverse from the product adhesive with the grating structure, thus obtaining a waveguide substrate with a grating structure, thereby obtaining a diffractive waveguide.

[0007] As mentioned earlier, existing methods require a tackifier to be spin-coated onto the waveguide substrate before applying the adhesive to increase the interfacial adhesion between the adhesive and the substrate. However, since the refractive index of the tackifier differs from that of the waveguide substrate and the adhesive, this can negatively impact the optical performance of the diffractive waveguide. Summary of the Invention

[0008] To overcome the shortcomings of the prior art, the present invention provides a high-adhesion UV-curable adhesive and its preparation method.

[0009] This invention is achieved through the following technical solution: This invention provides a high-adhesion UV-curable adhesive, comprising the following components by weight percentage: Oligomers 4-30%; UV-curable monomers: 0-40%; Photoinitiator 0.05-10%; Leveling agent 0.05-10%; Titanium oxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion 30-90%; The oligomer is a polyurethane acrylate polymer; the hydroxyl value of the polyurethane acrylate polymer is ≥50.

[0010] Preferred by mass percentage, the oligomer content is 4-25%, more preferably 4-20%.

[0011] Preferred by mass percentage, the amount of photocurable monomer is 5-35%, and more preferably, the amount of photocurable monomer is 10-30%.

[0012] Preferred percentage by weight: 1-10% photoinitiator.

[0013] Preferred leveling agent content is 0.05-5% by weight, and more preferably, it is 0.05-1%.

[0014] Preferred by mass percentage, the titanium dioxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion is 35-85%, more preferably 40-85%.

[0015] Polyurethane acrylate polymers with a hydroxyl value ≥ 50 can be, for example, produced by Kunshan Castel Polymer Materials Co., Ltd., product model U-CURE 93721, functionality 2, hydroxyl value 160; or produced by Guangzhou Runao Chemical Materials Co., Ltd., product model FSP5520, functionality 4, hydroxyl value 70; or produced by Jingshuo Chemical Technology Co., Ltd., product model G-4793, hydroxyl value 50, functionality 2; or produced by Lankeluo New Materials Co., Ltd., product model L1380, hydroxyl value 155, functionality 2.

[0016] Furthermore, the functionality of the polyurethane acrylate polymer is ≤3.

[0017] Polyurethane acrylate polymers with a hydroxyl value ≥ 50 and functionality ≤ 3 can be, for example, produced by Jingshuo Chemical Technology Co., Ltd., product model G-4793, with a hydroxyl value of 50 and functionality of 2. Alternatively, they can be produced by Lankeluo New Materials Co., Ltd., product model L1380, with a hydroxyl value of 155 and functionality of 2.

[0018] Furthermore, the functionality of the photocurable monomer is 1.

[0019] Furthermore, the photocurable monomer is an acrylate monomer or a mercapto monomer. Acrylate monomers with a functionality of 1 include lauryl acrylate, stearyl acrylate, isobornyl acrylate, 2-carboxyethyl acrylate, tridecyl acrylate, 3,3,5-trimethylcyclohexyl acrylate, benzyl acrylate, p-cumenylphenoxyethyl acrylate, benzyl methacrylate, 2-phenoxyethyl acrylate, o-phenylphenoxyethyl acrylate, N-vinylpyrrolidone, etc. Mercapto monomers with a functionality of 1 include N-(3-mercaptophenyl)acetamide, 4-methyl-2-mercaptobenzothiazole, 5-methyl-2-mercaptobenzothiazole, 6-amino-2-mercaptobenzothiazole, 2,6-dimethylmercaptophenol, 2,4-dimethylmercaptophenol, methyl p-thiobenzoate, 2-mercaptonaphthalene, mercaptoacetylnaphthylamine, etc.

[0020] Furthermore, the photoinitiator is a pyrolysis-type photoinitiator or a hydrogen abstraction-type photoinitiator.

[0021] Cleavage-type photoinitiators include 2-hydroxy-2-methyl-1-phenylpropanone, 1-hydroxycyclohexylphenyl ketone, 2-methyl-1-[4-(methylthio)phenyl]-2-morpholino-1-propanone, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-butanone, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide, α,α-dimethoxy-α-phenylacetophenone, etc.; hydrogen-abstracting photoinitiators include benzophenone, michidone, isopropylthioxanthraphenone, 2,4-diethylthioxanthraphenone, 4-methylbenzophenone, 4-phenylbenzophenone, methyl o-benzoylbenzoate, etc.

[0022] Titanium oxide nanoparticle dispersions can be produced by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#. Zirconia nanoparticle dispersions can be produced by Nippon Shokubai Co., Ltd., product model ZP153.

[0023] Leveling agents can be selected from BYK Chemical's BYK310, BYK333, BYK307, BYK378, BYK354, etc., or from Evonik Industries' Flow 370, Flow 375, Flow 425, Flow 460 N, Flow ATF 2, Glide 100, Glide 110, etc.

[0024] Furthermore, by mass percentage, it also includes the following components: Silane coupling agent 0.05-10%; preferably, The silane coupling agent used is a silane coupling agent containing acrylate groups or mercapto groups. Examples of mercapto-containing silane coupling agents include 3-mercaptopropyltrimethoxysilane and γ-mercaptopropyltriethoxysilane. Examples of silane coupling agents containing acrylate groups include γ-methacryloyloxypropyltrimethoxysilane, γ-methacryloyloxypropyltriethoxysilane, γ-acryloyloxypropyltrimethoxysilane, methacryloyloxypropylmethyldimethoxysilane, and methacryloyloxypropyltri(methoxyethoxy)silane.

[0025] The present invention also provides a method for preparing the above-mentioned high-adhesion UV-curable adhesive, comprising the following steps: Weigh the oligomer, photocurable monomer, photoinitiator, and leveling agent according to the stated mass percentage; The oligomer, photocurable monomer, photoinitiator and leveling agent are stirred and mixed evenly, and then titanium oxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion is added and stirred and mixed evenly to obtain a UV-curable adhesive with high adhesion performance.

[0026] Furthermore, it also includes: Weigh 0.05-10% of the silane coupling agent according to the stated mass percentage; The oligomer, photocurable monomer, photoinitiator, silane coupling agent and leveling agent are stirred and mixed evenly, and then titanium oxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion is added and stirred and mixed evenly to obtain a UV-curable adhesive with high adhesion performance.

[0027] Compared with the prior art, the technical solution of the present invention has the following beneficial effects: This invention provides a high-adhesion UV-curable adhesive, comprising the following components by mass percentage: 4-90% oligomer, 0-40% photocurable monomer, 0.05-10% photoinitiator, 0.05-10% leveling agent, and 30-90% titanium dioxide nanoparticle dispersion or zirconium dioxide nanoparticle dispersion. The oligomer is a polyurethane acrylate polymer with a hydroxyl value ≥50. The titanium dioxide or zirconium dioxide nanoparticle dispersion in the adhesive, combined with the photocurable monomer, can significantly improve the refractive index of the UV-curable adhesive. Adding 4-90% by mass of oligomer, specifically a polyurethane acrylate polymer with a hydroxyl value ≥50, to the adhesive, on the one hand, weakens the polarity of the polyurethane material through the large number of hydroxyl groups contained in the oligomer, thereby improving the adhesion of the UV-curable adhesive to waveguide substrates made of polyurethane; on the other hand, the oligomer can react with the photocurable monomer, thus participating in the UV polymerization reaction of the UV-curable adhesive.

[0028] The high-adhesion UV-curable adhesive provided by this invention, based on the use of polyurethane acrylate polymers with hydroxyl values ​​≥50 as oligomers, further limits the functionality of the polyurethane acrylate polymers to ≤3, thereby reducing the curing shrinkage rate of the UV-curable adhesive and further improving the adhesion of the UV-curable adhesive to waveguide substrates made of polyurethane.

[0029] The high-adhesion UV-curable adhesive provided by this invention further limits the functionality of the UV-curable monomer to 1, further reduces the curing shrinkage rate of the UV-curable adhesive, and can further improve the adhesion of the UV-curable adhesive to waveguide substrates made of polyurethane.

[0030] The high-adhesion UV-curable adhesive provided by this invention further incorporates a silane coupling agent with a mass percentage content of 0.05-10%, wherein the silane coupling agent is a silane coupling agent containing acrylate groups or mercapto groups. On the one hand, this can improve the adhesion of the UV-curable adhesive to waveguide substrates made of glass. On the other hand, the silane coupling agent can react with photocurable monomers to participate in the UV polymerization reaction of the UV-curable adhesive. Detailed Implementation

[0031] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only 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.

[0032] In this document, the terms "first," "second," and other similar words are not intended to imply any order, quantity, or importance, but are merely used to distinguish different elements. The terms "one," "a," and other similar words are not intended to indicate the existence of only one of the stated things, but rather that the description refers only to one of the stated things, which may have one or more. The terms "comprising," "including," and other similar words are intended to indicate a logical relationship, not a spatial relationship. For example, "A includes B" means that logically B belongs to A, not that spatially B is located inside A. Furthermore, the meanings of the terms "comprising," "including," and other similar words should be considered open-ended, not closed. For example, "A includes B" means that B belongs to A, but B does not necessarily constitute all of A; A may also include other elements such as C, D, and E.

[0033] In this document, the terms "embodiment," "this embodiment," "preferred embodiment," and "one embodiment" do not imply that the description applies only to one specific embodiment, but rather that such description may also be applicable to one or more other embodiments. Those skilled in the art will understand that any description made herein with respect to one embodiment can be substituted, combined, or otherwise incorporated with the descriptions in one or more other embodiments. Such substitutions, combinations, or other incorporations resulting in new embodiments are readily conceived by those skilled in the art and fall within the scope of protection of this invention.

[0034] In this description, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified. Example 1

[0035] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 12.4g; Polyurethane acrylate polymer (manufactured by Jingshuo Chemical Technology Co., Ltd., product model G-4793): 9g; 4-Methylbenzophenone (4-MBP): 5.4g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.1g; Zirconia nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model ZP153): 104.29g.

[0036] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Jingshuo Chemical Technology Co., Ltd., product model G-4793), 4-methylbenzophenone (4-MBP), leveling agent (manufactured by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and zirconium oxide nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model ZP153).

[0037] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Jingshuo Chemical Technology Co., Ltd., product model G-4793), 4-methylbenzophenone (4-MBP), leveling agent (manufactured by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) are stirred evenly. Then, the above-mentioned quantities of zirconium oxide nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model ZP153) are added. The mixture is then accelerated and stirred in a centrifugal mixer at 2000 rpm for 3 minutes to obtain a high-adhesion UV-curable adhesive. Example 2

[0038] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 17.3g; Polyurethane acrylate polymer (manufactured by Lankeluo New Materials Co., Ltd., product model L1380): 4g; 4-Methylbenzophenone (4-MBP): 5.4g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Zirconia nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model ZP153): 104.29g.

[0039] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 4-methylbenzophenone (4-MBP), leveling agent (produced by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and zirconium oxide nanoparticle dispersion (produced by Nippon Shokubai Co., Ltd., product model ZP153).

[0040] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 4-methylbenzophenone (4-MBP), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) are stirred evenly. Then, the above-mentioned quantities of zirconium oxide nanoparticle dispersion (produced by Nippon Shokubai Co., Ltd., product model ZP153) are added. The mixture is then accelerated and stirred in a centrifugal mixer at 2000 rpm for 3 minutes to obtain a high-adhesion UV-curable adhesive. Example 3

[0041] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: 2-Phenoxyethyl acrylate (PHEA): 27.2g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 20g; 4-Methylbenzophenone (4-MBP): 8.4g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.3g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 193.83g.

[0042] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh the following components according to the above-mentioned weights: 2-phenoxyethyl acrylate (PHEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 4-methylbenzophenone (4-MBP), leveling agent (produced by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#).

[0043] The above-mentioned quantities of 2-phenoxyethyl acrylate (PHEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 4-methylbenzophenone (4-MBP), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) are stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#) are added. The mixture is then accelerated and stirred in a centrifuge at 2000 rpm for 3 minutes to obtain a high-adhesion UV-curable adhesive. Example 4

[0044] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 13.3g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 17g; 2,4-Diethylthioxanthone (DETX): 5.4g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 281.94g.

[0045] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4-diethylthioxanthone (DETX), leveling agent (produced by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#).

[0046] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4-diethylthioxanthone (DETX), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) were stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#) were added, and the mixture was accelerated and stirred in a centrifuge at 2000 rpm for 3 minutes to obtain a high-adhesion UV-curable adhesive. Example 5

[0047] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 11.8g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 6.6g; 2,4-Diethylthioxanthone (DETX): 3.3g; Leveling agent (manufactured by DIGIC, product model: Flow 370): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 343.61g.

[0048] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380), 2,4-diethylthioxanthone (DETX), leveling agent (produced by Digo Company, product model: Flow 370), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#).

[0049] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4-diethylthioxanthone (DETX), leveling agent (produced by DIGIC, product model: Flow 370), and γ-methacryloyloxypropyltrimethoxysilane (KH570) were stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#) were added, and the mixture was accelerated and stirred in a centrifuge at 2000 rpm for 3 minutes to obtain a high-adhesion UV-curable adhesive. Example 6

[0050] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 11.8g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 6.6g; 2,4,6-Trimethylbenzoyl-diphenylphosphine oxide (TPO): 3.3g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 281.94g.

[0051] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (produced by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#).

[0052] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) were stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#) were added, and the mixture was accelerated and stirred at 2000 rpm for 3 minutes in a centrifuge to obtain a high-adhesion UV-curable adhesive. Example 7

[0053] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: N-(3-mercaptophenyl)acetamide: 11.8g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 6.6g; 2,4,6-Trimethylbenzoyl-diphenylphosphine oxide (TPO): 3.3g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 281.94g.

[0054] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh the following components according to the above-mentioned weights: N-(3-mercaptophenyl)acetamide, polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (produced by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#).

[0055] The above-mentioned quantities of N-(3-mercaptophenyl)acetamide, polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) are stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#) are added, and the mixture is accelerated and stirred at 2000 rpm for 3 minutes in a centrifuge to obtain a high-adhesion UV-curable adhesive. Example 8

[0056] The high-adhesion UV-curable adhesive provided in this embodiment is composed of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 11.8g; Polyurethane acrylate polymer (manufactured by Jingshuo Chemical Technology Co., Ltd., product model G-4793): 6.6g; 2,4,6-Trimethylbenzoyl-diphenylphosphine oxide (TPO): 3.3g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 281.94g.

[0057] The method for preparing the high-adhesion UV-curable adhesive in this embodiment includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Jingshuo Chemical Technology Co., Ltd., product model G-4793), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (manufactured by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#).

[0058] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Jingshuo Chemical Technology Co., Ltd., product model G-4793), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (manufactured by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) were stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#) were added, and the mixture was accelerated and stirred at 2000 rpm for 3 minutes in a centrifuge to obtain a high-adhesion UV-curable adhesive.

[0059] Comparative Example 1 The UV-curable adhesive provided in this comparative example consists of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 12.4g; Polyurethane acrylate polymer (manufactured by Guangzhou Runao Chemical Materials Co., Ltd., product model: Lucure8091, functionality 2, hydroxyl value 0): 9g 4-Methylbenzophenone (4-MBP): 5.4g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.1g; Zirconia nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model ZP153): 104.29g.

[0060] The preparation method of the UV-curable adhesive in this comparative example includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Guangzhou Runao Chemical Materials Co., Ltd., product model: Lucure8091), 4-methylbenzophenone (4-MBP), leveling agent (manufactured by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and zirconium oxide nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model: ZP153).

[0061] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Guangzhou Runao Chemical Materials Co., Ltd., product model: Lucure8091), 4-methylbenzophenone (4-MBP), leveling agent (manufactured by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) are stirred evenly. Then, the above-mentioned quantities of zirconium oxide nanoparticle dispersion (manufactured by Nippon Shokubai Co., Ltd., product model: ZP153) are added. The mixture is then accelerated and stirred in a centrifugal mixer at 2000 rpm for 3 minutes to obtain the UV-curable adhesive.

[0062] Comparative Example 2 The UV-curable adhesive provided in this comparative example consists of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 11.8g; Polyurethane acrylate polymer (produced by Guangzhou Runao Chemical Materials Co., Ltd., product model: FSP5520, functionality 4, hydroxyl value 70): 6.6g; 2,4-Diethylthioxanthone (DETX): 3.3g; Leveling agent (manufactured by DIGIC, product model: Flow 370): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 343.61g.

[0063] The preparation method of the UV-curable adhesive in this comparative example includes the following steps: Weigh out the following components according to the above-mentioned weights: o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Guangzhou Runao Chemical Materials Co., Ltd., product model: FSP5520, functionality 4, hydroxyl value 70), 2,4-diethylthioxanthone (DETX), leveling agent (manufactured by DIGIC, product model: Flow 370), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#).

[0064] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (manufactured by Guangzhou Runao Chemical Materials Co., Ltd., product model: FSP5520, functionality 4, hydroxyl value 70), 2,4-diethylthioxanthone (DETX), leveling agent (manufactured by DIGIC, product model: Flow 370), and γ-methacryloyloxypropyltrimethoxysilane (KH570) were stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#) were added, and the mixture was accelerated and stirred in a centrifuge at 2000 rpm for 3 minutes to obtain the UV-curable adhesive.

[0065] Comparative Example 3 The UV-curable adhesive provided in this comparative example consists of the following components by weight: Trimethylolpropane triacrylate (functionality 3): 11.8g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 6.6g; 2,4,6-Trimethylbenzoyl-diphenylphosphine oxide (TPO): 3.3g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.2g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 281.94g.

[0066] The preparation method of the UV-curable adhesive in this comparative example includes the following steps: Weigh the following components according to the above-mentioned mass: trimethylolpropane triacrylate (functionality 3), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (produced by BYK Chemical, product model: BYK310), γ-methacryloyloxypropyltrimethoxysilane (KH570), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#).

[0067] The above-mentioned quantities of trimethylolpropane triacrylate (functionality 3), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) are stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model: OT-RBZ205P7L15-EX103#) are added, and the mixture is stirred at 2000 rpm for 3 minutes in a centrifuge to obtain the UV-curable adhesive.

[0068] Comparative Example 4 The UV-curable adhesive provided in this comparative example consists of the following components by weight: o-Phenylacetyl acrylate (OPPEA): 11.8g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 6.6g; 2,4-Diethylthioxanthone (DETX): 3.3g; Leveling agent (manufactured by DIGIC, product model: Flow 370): 0.1g; Titanium oxide nanoparticle dispersion (manufactured by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#): 343.61g.

[0069] The preparation method of the UV-curable adhesive in this comparative example includes the following steps: Weigh out o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4-diethylthioxanthone (DETX), leveling agent (produced by Digo Corporation, product model: Flow 370), and titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#) according to the above-mentioned mass.

[0070] The above-mentioned quantities of o-phenylphenoxyethyl acrylate (OPPEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 2,4-diethylthioxanthone (DETX), and leveling agent (produced by Digo Corporation, product model: Flow 370) are stirred evenly. Then, the above-mentioned quantities of titanium dioxide nanoparticle dispersion (produced by Nissan Chemical Co., Ltd., product model OT-RBZ205P7L15-EX103#) are added. The mixture is then accelerated and stirred in a centrifuge at 2000 rpm for 3 minutes to obtain a high-adhesion UV-curable adhesive.

[0071] Comparative Example 5 The UV-curable adhesive provided in this comparative example consists of the following components by weight: 2-Phenoxyethyl acrylate (PHEA): 27.2g; Polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380): 20g; 4-Methylbenzophenone (4-MBP): 8.4g; Leveling agent (manufactured by BYK Chemicals, product model: BYK310): 0.1g; γ-Methacryloxypropyltrimethoxysilane (KH570): 0.3g.

[0072] The preparation method of the UV-curable adhesive in this comparative example includes the following steps: Weigh the following components according to the above-mentioned quantities: 2-phenoxyethyl acrylate (PHEA), polyurethane acrylate polymer (produced by Lankeluo New Materials Co., Ltd., product model L1380), 4-methylbenzophenone (4-MBP), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570).

[0073] The UV-curable adhesive can be prepared by mixing the above-mentioned quantities of 2-phenoxyethyl acrylate (PHEA), polyurethane acrylate polymer (produced by Lankel New Materials Co., Ltd., product model L1380), 4-methylbenzophenone (4-MBP), leveling agent (produced by BYK Chemical, product model: BYK310), and γ-methacryloyloxypropyltrimethoxysilane (KH570) in a centrifugal mixer at 2000 rpm for 3 minutes.

[0074] The UV-curable adhesives of Examples 1-8 and Comparative Examples 1-5 were applied to the nanoimprinting process of diffractive waveguides as follows: 1. Prepare an imprint master with a preset grating structure.

[0075] 2. The grating structure of the embossing master is transferred to the soft film substrate through a nanoimprinting process to obtain a soft film plate with an inverse structure of grating structure.

[0076] Specifically, Imprinting adhesive is uniformly spin-coated onto the imprinting master. The soft film substrate is then bonded to the imprinting master. Pressure is applied to fill the grating structure of the imprinting master with the imprinting adhesive, resulting in an inverse structure of the grating structure on the imprinting adhesive. The imprinting adhesive with the inverse structure of the grating structure is then cured and demolded using ultraviolet light and transferred to the soft film substrate to obtain a soft film plate with an inverse structure of the grating structure.

[0077] 3. The inverse structure of the grating structure on the flexible film plate is transferred onto the waveguide substrate using a nanoimprinting process to obtain a diffractive waveguide.

[0078] Specifically, Waveguide substrates (glass wafer substrates and polyurethane substrates) are placed on a spin coater and coated with the UV-curable adhesives of Examples 1-8 and Comparative Examples 1-5 respectively, resulting in a uniform adhesive layer with a nanometer-scale thickness on the waveguide substrate. A soft film plate with a grating structure inverse is pressed onto the adhesive layer, resulting in a grating structure on the adhesive layer. Subsequently, UV light source irradiation is applied to cure the adhesive layer with the grating structure. Then, the soft film plate with the grating structure inverse is separated from the adhesive layer with the grating structure, and demolding is completed to obtain a diffractive waveguide product with a grating structure.

[0079] The following performance tests were performed on the diffractive waveguide products using the UV-curable adhesives of Examples 1-8 and Comparative Examples 1-5: Refractive index test: The refractive index of the adhesive layer of the diffractive waveguide product is tested using an ellipsometer to obtain the refractive index of the adhesive layer under a wavelength of 532nm (it should be noted that the wavelength of 532nm is only an example, and other wavelengths can also be used).

[0080] Adhesion test of adhesive layer on waveguide substrate: According to the national standard GB / T 9286-1998, the adhesive layer of the diffractive waveguide product was subjected to a cross-cut adhesion test. The test result of 3B-5B indicates that the adhesive layer has good adhesion to the waveguide substrate, with 5B indicating the best adhesion. The test result <3B indicates that the adhesive layer has poor adhesion to the waveguide substrate.

[0081] The test results are shown in Table 1 below: Table 1:

[0082] 1. From the test results of Examples 1-8 above, it can be concluded that the UV-curable adhesive prepared by the technical solution of the present invention has a high refractive index (1.7-1.95) and the UV-curable adhesive has very good adhesion to both glass wafer substrates and polyurethane substrates.

[0083] 2. By comparing Example 1 and Comparative Example 1, it can be seen that when the hydroxyl value of the polyurethane acrylate polymer added to the UV-curable adhesive is less than 50, the UV-curable adhesive has poor adhesion to the polyurethane substrate.

[0084] 3. By comparing Example 5 and Comparative Example 2, it can be seen that when the hydroxyl value of the polyurethane acrylate polymer added to the UV-curable adhesive is greater than 50 but the functionality is greater than 3, the adhesion performance of the UV-curable adhesive to the polyurethane substrate is slightly reduced.

[0085] 4. By comparing Example 6 and Comparative Example 3, it can be seen that when the functionality of the UV-curable monomer in the UV-curable adhesive is greater than 1, the adhesion performance of the UV-curable adhesive to the polyurethane substrate decreases.

[0086] 5. By comparing Example 5 and Comparative Example 4, it can be seen that when no silane coupling agent containing acrylate groups or mercapto groups is added to the UV-curable adhesive, the adhesion of the UV-curable adhesive to the glass wafer substrate is poor.

[0087] 6. By comparing Example 3 and Comparative Example 5, it can be seen that when titanium dioxide nanoparticle dispersion is not added to the UV-curable adhesive, the refractive index of the UV-curable adhesive decreases.

[0088] The above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still make modifications or equivalent substitutions to the specific implementation of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention are within the protection scope of the claims of the present invention pending approval.

Claims

1. A UV-curable adhesive with high adhesion performance, characterized in that, By mass percentage, it includes the following components: Oligomers 4-30%; UV-curable monomers: 0-40%; Photoinitiator 0.05-10%; Leveling agent 0.05-10%; Titanium oxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion 30-90%; The oligomer is a polyurethane acrylate polymer; the hydroxyl value of the polyurethane acrylate polymer is ≥50.

2. The high-adhesion UV-curable adhesive according to claim 1, characterized in that, It also includes the following components by weight percentage: Silane coupling agent 0.05-10%; The silane coupling agent is a silane coupling agent containing acrylate groups or mercapto groups.

3. The high-adhesion UV-curable adhesive according to claim 1, characterized in that, The functionality of the polyurethane acrylate polymer is ≤3.

4. The high-adhesion UV-curable adhesive according to claim 1, characterized in that, The functionality of the photocurable monomer is 1.

5. The high-adhesion UV-curable adhesive according to claim 1, characterized in that, The photocurable monomer is an acrylate monomer or a mercapto monomer.

6. The high-adhesion UV-curable adhesive according to claim 1, characterized in that, The photoinitiator is either a pyrolysis-type photoinitiator or a hydrogen abstraction-type photoinitiator.

7. The method for preparing the high-adhesion UV-curable adhesive according to claim 1, characterized in that, Includes the following steps: Weigh the oligomer, photocurable monomer, photoinitiator, and leveling agent according to the stated mass percentage; The oligomer, photocurable monomer, photoinitiator and leveling agent are stirred and mixed evenly, and then titanium oxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion is added and stirred and mixed evenly to obtain a UV-curable adhesive with high adhesion performance.

8. The method for preparing the high-adhesion UV-curable adhesive according to claim 7, characterized in that, Also includes: Weigh 0.05-10% of the silane coupling agent according to the stated mass percentage; The oligomer, photocurable monomer, photoinitiator, silane coupling agent and leveling agent are stirred and mixed evenly, and then titanium oxide nanoparticle dispersion or zirconium oxide nanoparticle dispersion is added and stirred and mixed evenly to obtain a UV-curable adhesive with high adhesion performance.

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