Wide-angle field-of-view AR (Augmented Reality) imaging nanocomposite and preparation process thereof
By compounding the organic polymer matrix with nano-optical functional particles and optimizing the preparation process, the problem of poor optical matching of wide-angle field of view AR imaging materials was solved, the large-scale clear imaging effect of AR equipment was achieved, and the optical properties and mechanical strength of the material were improved.
Patent Information
- Application Number
- CN202511011967.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-22
- Publication Date
- 2025-10-10
AI Technical Summary
The poor optical matching of existing wide-angle field of view AR imaging nano-composites leads to image distortion and limited field of view, which cannot meet the AR device's requirements for clear imaging over a large range.
An organic polymer matrix is compounded with specific nano-optical functional particles, and a preparation process combining hydrothermal synthesis and step-by-step modification is adopted. A silane coupling agent is used to modify the surface of the nanoparticles, and a plasticizer is added to optimize the optical properties and molding properties of the material.
The coordinated optimization of the optical performance of composite materials under wide-angle field of view is achieved, which solves the problems of imaging distortion and limited field of view, meets the needs of AR devices for clear imaging over a large range, and improves the uniformity of the optical performance and mechanical strength of the material.
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Figure CN120758020A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of composite materials, and in particular to a wide-angle field-of-view AR imaging nanocomposite material and a preparation process thereof. Background Art
[0002] Wide-angle field of view AR imaging nanocomposites are a key material used in augmented reality devices. Their core function is to achieve a wider field of view and clearer imaging effects by regulating the propagation and refraction characteristics of light. They have important application value in AR terminal devices such as smart glasses and head-mounted displays. Such materials usually need to take into account good optical transparency, mechanical stability and compatibility with AR optical systems to meet the requirements of imaging quality and equipment durability in actual use.
[0003] In the existing technology, composite materials used for wide-angle AR imaging mostly use a single organic polymer matrix, or simply mix nanoparticles that have not been designed for performance matching. This solution often makes it difficult to achieve precise control of optical parameters because the refractive index matching of the material under wide-angle field of view is low and light scattering is severe, which in turn causes distortion and blurred edges in the imaging image. Therefore, the field of view angle range is significantly limited and cannot meet the actual needs of AR devices for large-scale clear imaging. Summary of the Invention
[0004] In response to the shortcomings of the existing technology, the present invention provides a wide-angle field of view AR imaging nanocomposite material and its preparation process, which solves the problem that a single polymer or unmodified nanoparticle combination leads to poor optical matching and cannot meet the actual needs of AR devices for large-scale clear imaging.
[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: A wide-angle field of view AR imaging nanocomposite material, comprising the following raw materials in parts by weight: 60-80 parts of an organic polymer matrix, 10-30 parts of nano-optical functional particles, and 5-15 parts of a plasticizer;
[0006] The nano-optical functional particles are prepared from core functional raw materials and structure regulators;
[0007] The plasticizer is dibutyl phthalate or tributyl citrate.
[0008] Preferably, the organic polymer matrix is a mixture of one or more of polymethyl methacrylate, polystyrene or polyurethane.
[0009] Preferably, the core functional raw materials include 1.2-1.8 parts of zinc oxide target, 2.0-3.5 parts of zinc nitrate hexahydrate, and 0.5-1.2 parts of titanium tetrachloride, and the structure regulating agent is 1.0-2.0 parts of hexamethylenetetramine.
[0010] Preferably, the nano-optical functional particles are a combination of one or more of titanium dioxide nanoparticles or zinc oxide nanoparticles formed by reaction of a core functional material, the nano-optical functional particles have a particle size of 10-50 nm, and the titanium dioxide nanoparticles are surface-modified using a surface modifier, the surface modifier being a silane coupling agent.
[0011] A preparation process of a wide-view field AR imaging nanocomposite material, the preparation process comprising the following steps:
[0012] S1, dissolving zinc nitrate hexahydrate and titanium tetrachloride in deionized water to prepare a mixed solution with a total metal ion concentration of 0.1-0.3 mol / L, then adding hexamethylenetetramine to the mixed solution to adjust the pH of the solution to 8-10 to form a precursor solution;
[0013] S2, transferring the precursor solution to a high-pressure reaction kettle and reacting at 120-180℃ for 6-12 hours; after the reaction is completed, cooling to room temperature, collecting the precipitate by centrifugal separation, washing with deionized water and anhydrous ethanol for 3-5 times, and vacuum drying at 60-80℃ for 12-24 hours to obtain titanium dioxide or zinc oxide composite nanoparticles;
[0014] S3, dispersing the dried nanoparticles in anhydrous ethanol to form a suspension with a mass fraction of 5%-10%, adding a silane coupling agent at 1%-5% of the mass of the nanoparticles, and stirring and reacting at 50-80℃ for 2-6 hours; after the reaction is completed, centrifugal separation and vacuum drying are performed to obtain surface-modified nano-optical functional particles;
[0015] S4, heating the organic polymer matrix to a molten state, then adding the surface-modified nano-optical functional particles and a plasticizer, mixing under mechanical stirring for 10-30 minutes, and then forming by extrusion, injection molding or calendering process to obtain the composite material.
[0016] Preferably, in S2, the molar ratio of zinc nitrate hexahydrate to titanium tetrachloride is controlled to be 1:1 to 3:1 to adjust the ratio of zinc oxide to titanium dioxide in the composite nanoparticles.
[0017] Preferably, in S3, the silane coupling agent is γ-aminopropyl triethoxysilane or γ-methacryloyloxypropyl trimethoxysilane, and 0.1%-1% of a catalyst dibutyltin dilaurate is added to the reaction system.
[0018] Preferably, in said S4, after adding the nano-optical functional particles and before adding the plasticizer, ultrasonic wave is introduced to assist dispersion, the ultrasonic wave frequency is 20-40 kHz, the power is 100-300 W, and the dispersion time is 5-15 minutes.
[0019] Preferably, the zinc oxide target is pretreated before use, specifically comprising the following steps:
[0020] The zinc oxide target is crushed into powder with a particle size of ≤100 μm;
[0021] Calcination at 400-600°C for 2-4 hours;
[0022] Then add it into titanium tetrachloride solution and disperse it by ultrasonic for 30-60 minutes.
[0023] Preferably, in S4, the molding process of the composite material is extrusion molding, and the temperature of each zone of the extruder is set to: 160-180°C in zone 1, 180-200°C in zone 2, 200-220°C in zone 3, 210-230°C in the die, and the screw speed is 50-120rpm.
[0024] The present invention provides a wide-angle field of view AR imaging nanocomposite material and its preparation process. It has the following beneficial effects:
[0025] 1. The present invention achieves synergistic optimization of the optical performance of the composite material in wide-angle AR imaging scenarios by compounding an organic polymer matrix with specific nano-optical functional particles. Compared with the existing solutions that use a single polymer or unmodified nanoparticle combination, which leads to poor optical matching, this solution solves the core defects of imaging distortion and limited field of view, thereby meeting the actual needs of AR devices for clear imaging over a wide range.
[0026] 2. The present invention adopts a technical solution of surface modification of nano-optical functional particles using a silane coupling agent, thereby achieving uniform dispersion of nanoparticles in a polymer matrix. Compared with the solution in the prior art in which nanoparticles agglomerate due to insufficient compatibility, this solution solves the core defects of composite materials, such as fluctuations in optical properties and decreased mechanical strength.
[0027] 3. The present invention achieves controllable growth and structural stability of nano-optical functional particles through a preparation process technology scheme that combines hydrothermal synthesis with step-by-step modification. Compared with the existing scheme of simple mixing preparation that leads to uneven particle size, it solves the core defect of poor consistency of optical parameters of composite materials.
[0028] 4. The present invention adopts a technical solution of using a specific plasticizer and controlling its addition ratio, thereby achieving a balance between the forming performance and optical properties of the composite material. Compared with the solution in the prior art where improper selection of plasticizers leads to a decrease in the light transmittance of the material, this solution solves the core defects of difficult forming and processing and insufficient imaging clarity. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1 The figure is a schematic flow chart of a preparation process of a wide-angle field AR imaging nanocomposite material according to the present invention. DETAILED DESCRIPTION
[0030] The following will clearly and completely describe the technical solution of the present invention in conjunction with the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0031] Please see the attached Figure 1 The embodiment of the present invention provides a wide-angle field of view AR imaging nanocomposite material, comprising the following raw materials in parts by weight: 60-80 parts of an organic polymer matrix, 10-30 parts of nano-optical functional particles, and 5-15 parts of a plasticizer;
[0032] Nano-optical functional particles are prepared from core functional raw materials and structure regulators;
[0033] The plasticizer is dibutyl phthalate or tributyl citrate.
[0034] Specifically, the organic polymer matrix provides the basic structure and stability of the material, and the appropriate ratio range ensures that the material has good mechanical properties and optical transparency; the nano-optical functional particles improve the optical properties of the material and achieve high-quality imaging under wide-angle field of view, and their ratio determines the degree of optical performance improvement; the plasticizer enhances the flexibility of the material and optimizes the performance of the material in different environments;
[0035] The core functional raw materials and structure regulators work together to ensure that nano-optical functional particles can be effectively formed and have the required properties;
[0036] Titanium dioxide and zinc oxide have specific refractive indices that can adjust the material's optical parameters, such as transmittance and refractive index, to expand the imaging field of view and avoid image blur. The combination of the two particles can synergistically regulate optical properties to meet the precise light transmission and refraction requirements of AR devices. Titanium dioxide and zinc oxide nanoparticles can be used in combination or alone. Surface modification of titanium dioxide nanoparticles can enhance their compatibility with organic polymer matrices and improve the integrity of the material.
[0037] Plasticizers are inserted between organic polymer molecular chains to reduce intermolecular forces, lower the glass transition temperature of the polymer matrix, improve the flexibility and processing fluidity of the material, and facilitate molding into complex-shaped AR optical components through extrusion, injection molding and other processes without significantly affecting the material's transmittance and mechanical strength.
[0038] The organic polymer matrix is a mixture of one or more of polymethyl methacrylate, polystyrene or polyurethane.
[0039] Specifically, polymethyl methacrylate has high light transmittance, ensuring the clarity of AR imaging; polystyrene has good processing fluidity and is easy to shape; and polyurethane has good flexibility, which improves the impact resistance of the material.
[0040] The core functional raw materials include 1.2-1.8 parts of zinc oxide target, 2.0-3.5 parts of zinc nitrate hexahydrate, 0.5-1.2 parts of titanium tetrachloride, and the structure regulator is 1.0-2.0 parts of hexamethylenetetramine.
[0041] Specifically, zinc oxide target, zinc nitrate hexahydrate and titanium tetrachloride are the material basis for synthesizing nano-optical functional particles. The zinc oxide target and zinc nitrate hexahydrate provide zinc sources, which react to generate zinc oxide nanoparticles; titanium tetrachloride provides titanium sources to generate titanium dioxide nanoparticles. The three together determine the chemical composition and optical activity of the nanoparticles, ensuring that the particles have the basis for adjusting the optical properties of the composite material.
[0042] During the nanoparticle synthesis process, the growth direction and morphology of the nanoparticles are controlled by adjusting the pH value and reaction rate of the reaction system to avoid excessive agglomeration of particles or excessive particle size, and to ensure uniform dispersion, thereby stably exerting optical functions.
[0043] The nano-optical functional particles are a combination of one or more of titanium dioxide nanoparticles and zinc oxide nanoparticles formed by the reaction of core functional raw materials. The particle size of the nano-optical functional particles is 10-50 nanometers, and the titanium dioxide nanoparticles are surface-modified using a surface modifier, which is a silane coupling agent.
[0044] Specifically, the two ends of the silane coupling agent's molecule are respectively bonded to the surface of titanium dioxide nanoparticles and the organic polymer matrix, eliminating the interfacial tension between the two through chemical bonds, preventing the nanoparticles from agglomerating in the matrix, improving the dispersion stability of the particles, and ensuring the uniformity and long-term effectiveness of the optical properties of the composite material.
[0045] A preparation process for a wide-angle field of view AR imaging nanocomposite material, the preparation process comprising the following steps:
[0046] S1. Dissolving zinc nitrate hexahydrate and titanium tetrachloride in deionized water to prepare a mixed solution with a total metal ion concentration of 0.1-0.3 mol / L, then adding hexamethylenetetramine to the mixed solution and adjusting the pH of the solution to 8-10 to form a precursor solution;
[0047] S2. Transfer the precursor solution to a high-pressure reactor and react at 120-180° C. for 6-12 hours; after the reaction, cool to room temperature, collect the precipitate by centrifugation, wash with deionized water and anhydrous ethanol 3-5 times in sequence, and vacuum dry at 60-80° C. for 12-24 hours to obtain titanium dioxide or zinc oxide composite nanoparticles;
[0048] S3, dispersing the dried nanoparticles in anhydrous ethanol to form a suspension with a mass fraction of 5%-10%, adding a silane coupling agent at a rate of 1%-5% of the mass of the nanoparticles, stirring and reacting at 50-80° C. for 2-6 hours, and after the reaction, centrifuging and vacuum drying to obtain surface-modified nano-optical functional particles;
[0049] S4. The organic polymer matrix is heated to a molten state, and then the surface-modified nano-optical functional particles and the plasticizer are added, mixed under mechanical stirring for 10-30 minutes, and then formed by extrusion, injection molding or calendering to obtain a composite material.
[0050] Specifically, zinc nitrate hexahydrate and titanium tetrachloride are dissolved in deionized water to avoid interference of impurity ions in the reaction. The total metal ion concentration is then controlled because too high a concentration will lead to too fast a particle generation rate and easy agglomeration, while too low a concentration will result in low reaction efficiency. After adding hexamethylenetetramine, the ammonia produced by its slow hydrolysis will gradually increase the alkalinity of the solution pH. At this time, the metal ions will form hydroxide or oxyhydroxide precursors, providing a stable reaction starting point for the subsequent generation of nanoparticles. The hydrolysis reaction formula of hexamethylenetetramine is: (CH2)6N4+6H2O→6HCHO+4NH3·H2O, slowly releasing NH3·H2O and gradually increasing the pH.
[0051] Afterwards, a high-temperature and high-pressure environment is provided by a high-pressure reactor to put the precursor solution in a subcritical or supercritical state, accelerating ion diffusion and crystal growth, and promoting the crystallization and morphology improvement of nanoparticles. After the reaction is completed, cooling can avoid the destruction of the particle structure caused by a sudden drop in temperature. Centrifugal separation uses centrifugal force to quickly separate the nanoparticle precipitation; deionized water washing removes residual water-soluble impurities, and anhydrous ethanol washing can replace the moisture on the surface of the particles, facilitating subsequent drying. Further early vacuum drying is carried out at low temperature to remove the solvent to avoid particle agglomeration caused by high temperature. At the same time, the vacuum environment can prevent particle oxidation. The reaction formula of zinc ions to generate zinc oxide is: Zn 2+ +2OH - →ZnO↓+H2O, under alkaline conditions, zinc ions combine with hydroxide to form zinc oxide crystals, and titanium oxide ions form titanium dioxide. The reaction formula is:
[0052] TiO 2+ +H2O→TiO2↓+2H +, titanium oxide ions hydrolyze to form titanium dioxide crystals, releasing hydrogen ions;
[0053] Anhydrous ethanol is used as a dispersion medium to dissolve the silane coupling agent and evenly disperse the nanoparticles, preventing hydroxyl group agglomeration during aqueous phase dispersion, balancing dispersion efficiency and reaction concentration, ensuring full contact between the particles and the coupling agent. The coupling agent can cover the active sites on the particle surface, avoiding excess free coupling agent residue. Heating can accelerate the hydrolysis of the coupling agent and the reaction rate with the particle surface, while stirring can promote uniform mixing of the system. After the reaction is completed, centrifugation is performed to remove unreacted coupling agent, and vacuum drying is performed to remove residual ethanol to obtain pure surface-modified particles.
[0054] Heating to a molten state can enhance the mobility of the molecular chains of the organic polymer matrix, transforming it into a viscous flow state, providing space for the dispersion of nanoparticles and plasticizers; after adding surface-modified nanoparticles, they have good compatibility with the matrix and can be evenly dispersed under stirring; the addition of plasticizers further reduces the viscosity of the system and promotes uniform mixing. Mechanical stirring can achieve uniform distribution of each component at both the macro and micro levels. Extrusion, injection molding or calendering processes process the molten mixture into sheets, plates or complex components according to the product shape requirements, and finally cool and shape them into composite materials.
[0055] In S2, the ratio of zinc oxide to titanium dioxide in the composite nanoparticles is adjusted by controlling the molar ratio of zinc nitrate hexahydrate to titanium tetrachloride to be 1:1 to 3:1.
[0056] Specifically, the molar ratio of zinc nitrate hexahydrate to titanium tetrachloride directly determines the ratio of zinc ions to titanium ions in the reaction system. Under the same reaction conditions, the two ions will be converted into zinc oxide and titanium dioxide nanoparticles in proportion. By adjusting this ratio, the relative content of the two particles can be precisely controlled, and then the refractive index of the composite material can be adjusted to match the optical path design of the AR optical system and achieve low-light-loss imaging under a wide-angle field of view.
[0057] In S3, the silane coupling agent is γ-aminopropyltriethoxysilane or γ-methacryloxypropyltrimethoxysilane, and 0.1%-1% of the catalyst dibutyltin dilaurate is added to the reaction system.
[0058] Specifically, the amino group of γ-aminopropyltriethoxysilane can react with active hydrogen-containing polymers such as polyurethane, and the double bond of γ-methacryloxypropyltrimethoxysilane can undergo free radical copolymerization with polymethyl methacrylate, polystyrene, etc. The two coupling agents are respectively adapted to different types of polymer matrices. Dibutyltin dilaurate serves as an ester exchange reaction catalyst, which can reduce the activation energy of the hydrolysis and condensation reactions of the silane coupling agent, accelerate the reaction rate, shorten the time to reach reaction equilibrium, and improve the modification efficiency.
[0059] In S4, after adding the nano-optical functional particles and before adding the plasticizer, ultrasonic wave is introduced to assist dispersion, with an ultrasonic wave frequency of 20-40 kHz, a power of 100-300 W, and a dispersion time of 5-15 minutes.
[0060] Specifically, ultrasonic-assisted dispersion uses the cavitation effect generated by high-frequency mechanical vibration to form tiny bubbles in the liquid and burst them instantly, generating a strong impact force that can break up the weak agglomerates between nanoparticles. This process is carried out before the plasticizer is added to avoid the lubricating effect of the plasticizer reducing the cavitation effect and ensuring the dispersion effect; the combination of specific frequency, power and time can achieve the best dispersion effect without destroying the particle structure, further improving the optical uniformity of the composite material.
[0061] The zinc oxide target is pretreated before use, which includes the following steps:
[0062] The zinc oxide target is crushed into powder with a particle size of ≤100 μm;
[0063] Calcination at 400-600°C for 2-4 hours;
[0064] Then add it into titanium tetrachloride solution and disperse it by ultrasonic for 30-60 minutes.
[0065] Specifically, after pulverization, the specific surface area of the target material can be increased, the dissolution rate and reaction activity of the subsequent reaction can be improved, and then calcination can remove adsorbed water, organic impurities and lattice defects on the surface of the target material, thereby improving the purity and crystallinity of zinc oxide. After adding titanium tetrachloride solution, ultrasonic dispersion can be carried out. The vibration effect of ultrasound can be used to evenly disperse the target material powder in the solution to avoid sedimentation, while promoting its initial reaction with the titanium tetrachloride solution, thereby providing a uniform zinc source for the subsequent generation of nanoparticles.
[0066] In S4, the molding process of the composite material is extrusion molding, and the temperature of each zone of the extruder is set as follows: 160-180°C in zone 1, 180-200°C in zone 2, 200-220°C in zone 3, 210-230°C in the die head, and the screw speed is 50-120 rpm.
[0067] Specifically, the first zone is preheated to soften the material, the second zone is heated to promote melting, the third zone is kept warm to completely plasticize the material, and the slightly higher temperature of the die head ensures smooth extrusion of the material, ultimately making the performance of the extruded composite material uniform and stable.
[0068] The following is an introduction with reference to specific embodiments:
[0069] Example 1:
[0070] The wide-view field AR imaging nanocomposite provided by the embodiment comprises the following raw material weight parts: 60 parts of polymethyl methacrylate, 30 parts of nano optical functional particles and 10 parts of dibutyl phthalate.
[0071] The nano optical functional particles are prepared from 1.2 parts of zinc oxide target material, 2.0 parts of zinc nitrate hexahydrate, 1.2 parts of titanium tetrachloride and 1.0 parts of hexamethylenetetramine, the titanium dioxide nanoparticles are modified by gamma-aminopropyl triethoxysilane, and 0.1% of a catalyst dibutyl tin dilaurate is added to the reaction system;
[0072] The molar ratio of the zinc nitrate hexahydrate to the titanium tetrachloride is 1:1, and the particle size of the nano optical functional particles is 10 nanometers.
[0073] The preparation process of the wide-view field AR imaging nanocomposite comprises the following steps:
[0074] S1, dissolving the zinc nitrate hexahydrate and the titanium tetrachloride in deionized water to prepare a mixed solution with a total metal ion concentration of 0.1 mol / L, adding hexamethylenetetramine, adjusting the pH of the solution to 8 to form a precursor solution;
[0075] S2, transferring the precursor solution to a high-pressure reaction kettle, reacting at 120℃ for 12 hours; after the reaction is completed, cooling to room temperature, collecting the precipitate by centrifugal separation, washing with deionized water and anhydrous ethanol for 3 times, vacuum drying at 60℃ for 24 hours to obtain titanium dioxide and zinc oxide composite nanoparticles;
[0076] S3, dispersing the dried nanoparticles in anhydrous ethanol to form a suspension with a mass fraction of 5%, adding gamma-aminopropyl triethoxysilane at 1% of the mass of the nanoparticles, stirring and reacting at 50℃ for 6 hours, after the reaction is completed, centrifugal separation and vacuum drying to obtain surface-modified nano optical functional particles;
[0077] S4, heating the polymethyl methacrylate to a molten state, adding the surface-modified nano optical functional particles, dispersing by ultrasonic wave at 20 kHz and 100 W for 5 minutes, then adding dibutyl phthalate, mixing under mechanical stirring for 10 minutes, and then forming by injection molding to obtain the composite material.
[0078] Embodiment two:
[0079] The wide-view field AR imaging nanocomposite provided by the embodiment comprises the following raw material weight parts: 60 parts of polymethyl methacrylate, 30 parts of nano optical functional particles and 10 parts of dibutyl phthalate.
[0080] Among them, the nano-optical functional particles are prepared from 1.5 parts of zinc oxide target, 2.8 parts of zinc nitrate hexahydrate, 0.9 parts of titanium tetrachloride and 1.5 parts of hexamethylenetetramine. The titanium dioxide nanoparticles are modified with γ-methacryloxypropyltrimethoxysilane, and 0.5% of the catalyst dibutyl tin dilaurate is added to the reaction system.
[0081] The molar ratio of zinc nitrate hexahydrate to titanium tetrachloride is 2:1, the mass ratio of polystyrene to polyurethane is 1:1, and the particle size of the nano-optical functional particles is 25 nanometers.
[0082] The preparation process of the wide-angle field AR imaging nanocomposite material comprises the following steps:
[0083] S1. Dissolve zinc nitrate hexahydrate and titanium tetrachloride in deionized water to prepare a mixed solution with a total metal ion concentration of 0.2 mol / L, add hexamethylenetetramine, and adjust the solution pH to 9 to form a precursor solution;
[0084] S2. The precursor solution was transferred to a high-pressure reactor and reacted at 150° C. for 9 hours. After the reaction was completed, the mixture was cooled to room temperature, and the precipitate was collected by centrifugation. The precipitate was washed four times with deionized water and anhydrous ethanol, and dried under vacuum at 70° C. for 18 hours to obtain titanium dioxide and zinc oxide composite nanoparticles.
[0085] S3, dispersing the dried nanoparticles in anhydrous ethanol to form a suspension with a mass fraction of 8%, adding γ-methacryloxypropyltrimethoxysilane at a mass fraction of 3% of the nanoparticles, and stirring at 65° C. for 4 hours. After the reaction is completed, centrifugation and vacuum drying are performed to obtain surface-modified nano-optical functional particles;
[0086] S4. Heat the mixture of polystyrene and polyurethane to a molten state, add surface-modified nano-optical functional particles, disperse them by 30kHz, 200W ultrasonic wave for 10 minutes, then add tributyl citrate, mix them under mechanical stirring for 20 minutes, and then form them by extrusion process. The temperatures of each zone of the extruder are set to: 160°C in zone 1, 180°C in zone 2, 200°C in zone 3, 210°C in the die, and the screw speed is 80rpm to obtain the composite material.
[0087] Example 3:
[0088] The present invention provides a wide-angle field of view AR imaging nanocomposite material, which comprises the following raw materials in parts by weight: 80 parts of polyurethane, 10 parts of nano-optical functional particles, and 10 parts of tributyl citrate.
[0089] Among them, the nano-optical functional particles are prepared from 1.8 parts of zinc oxide target, 3.5 parts of zinc nitrate hexahydrate, 0.5 parts of titanium tetrachloride and 2.0 parts of hexamethylenetetramine. The titanium dioxide nanoparticles are modified with γ-methacryloxypropyltrimethoxysilane, and 1% of the catalyst dibutyltin dilaurate is added to the reaction system.
[0090] The molar ratio of zinc nitrate hexahydrate to titanium tetrachloride is 3:1, and the particle size of the nano-optical functional particles is 50 nanometers.
[0091] The preparation process of the wide-angle field AR imaging nanocomposite material comprises the following steps:
[0092] S1. Dissolve zinc nitrate hexahydrate and titanium tetrachloride in deionized water to prepare a mixed solution with a total metal ion concentration of 0.3 mol / L, add hexamethylenetetramine, and adjust the solution pH to 10 to form a precursor solution;
[0093] S2. The precursor solution was transferred to an autoclave and reacted at 180° C. for 6 hours. After the reaction, the mixture was cooled to room temperature, and the precipitate was collected by centrifugation. The mixture was washed with deionized water and anhydrous ethanol five times, and vacuum-dried at 80° C. for 12 hours to obtain titanium dioxide and zinc oxide composite nanoparticles.
[0094] S3, dispersing the dried nanoparticles in anhydrous ethanol to form a 10% suspension by mass, adding γ-methacryloxypropyltrimethoxysilane at a rate of 5% by mass of the nanoparticles, and stirring at 80° C. for 2 hours. After the reaction is completed, centrifugation and vacuum drying are performed to obtain surface-modified nano-optical functional particles;
[0095] S4. Heat the polyurethane to a molten state, add the surface-modified nano-optical functional particles, disperse them by 40kHz, 300W ultrasonic wave for 15 minutes, then add tributyl citrate, mix them under mechanical stirring for 30 minutes, and then form them by calendering process to obtain the composite material.
[0096] Table 1: Performance index effect comparison table
[0097]
[0098]
[0099] According to Table 1, compared with the prior art, the three embodiments of the present invention have obvious advantages in key performance indicators such as field of view, transmittance, refractive index, tensile strength and impact resistance. The prior art has the problem that a single polymer or a combination of unmodified nanoparticles leads to poor optical matching and cannot meet the actual needs of AR devices for large-scale clear imaging. The present invention effectively solves these defects through a reasonable raw material ratio and an optimized preparation process. Among them, Example 2 has the best comprehensive optical performance, and Examples 1 and 3 respectively perform outstandingly in mechanical strength and impact resistance, fully demonstrating the innovation and practicality of the present invention.
[0100] Field of view angle (°) in Table 1: Using the optical system measurement method, an optical test platform simulating AR imaging was built. The composite material was made into an optical waveguide lens assembly. By adjusting the angle of the incident light, the maximum angle range that can produce a clear image was recorded. This range is the field of view angle. The existing technology also uses optical software simulation methods, etc. The present invention uses the actual measurement method, which is closer to actual application scenarios and can intuitively reflect the field of view performance of the material in actual AR equipment.
[0101] The transmittance (%) in Table 1 was measured using a UV-visible spectrophotometer. The composite material was prepared into standard specimens of uniform thickness, and the transmittance of the specimens was measured at a wavelength of 550 nm, a value representative of the visible light range. While integrating sphere methods are available in the prior art, the UV-visible spectrophotometer method was chosen in this paper for its ease of operation and ability to accurately measure transmittance at specific wavelengths, which aligns with AR imaging's focus on visible light transmittance.
[0102] The refractive indices in Table 1 were measured using an Abbe refractometer. At a constant temperature of 25°C, the composite material sample was placed in close contact with the prism of the refractometer, and the refractive index value was read by adjusting the instrument. Interferometry is also available in the prior art, but the Abbe refractometer method is used in this paper, which is convenient to operate and highly accurate, meeting the general requirements for composite material refractive index measurement.
[0103] Tensile strength (MPa) in Table 1: Tested using a universal testing machine. The composite material was formed into a standard dumbbell-shaped specimen and stretched at a rate of 5 mm / min. The maximum tensile force at specimen breakage was recorded, and the tensile strength was calculated based on the specimen's cross-sectional area. This rate is selected in the present invention to consistently reflect the material's tensile properties.
[0104] Impact resistance (kJ / m 2) : Testing is performed using an Izod impact tester. Standard V-notched specimens of the composite material are prepared. The impact energy absorbed upon fracture is measured at a specified impact energy. The impact resistance is then calculated based on the specimen dimensions. While other methods exist in the prior art, such as the simply supported beam impact test, the present invention utilizes the Izod method, which is applicable to both brittle and ductile materials and provides a good indicator of the composite material's impact resistance.
[0105] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A wide-angle field of view AR imaging nanocomposite material, characterized in that: The invention comprises the following raw materials in parts by weight: 60-80 parts of organic polymer matrix, 10-30 parts of nano-optical functional particles, and 5-15 parts of plasticizer; The nano-optical functional particles are prepared from core functional raw materials and structure regulators; The plasticizer is dibutyl phthalate or tributyl citrate.
2. The wide-angle field AR imaging nanocomposite material according to claim 1, characterized in that: The organic polymer matrix is a mixture of one or more of polymethyl methacrylate, polystyrene or polyurethane.
3. The wide-angle field AR imaging nanocomposite material according to claim 1, characterized in that: The core functional raw materials include 1.2-1.8 parts of zinc oxide target material, 2.0-3.5 parts of zinc nitrate hexahydrate, and 0.5-1.2 parts of titanium tetrachloride, and the structure regulating agent is 1.0-2.0 parts of hexamethylenetetramine.
4. The wide-angle field AR imaging nanocomposite material according to claim 1, characterized in that: The nano-optical functional particles are a combination of one or more of titanium dioxide nanoparticles and zinc oxide nanoparticles formed by reacting the core functional raw materials. The particle size of the nano-optical functional particles is 10-50 nanometers, and the titanium dioxide nanoparticles are surface-modified using a surface modifier, which is a silane coupling agent.
5. A preparation process for wide-angle field AR imaging nanocomposite material, characterized in that: A wide-angle field AR imaging nanocomposite material according to any one of claims 1 to 4, wherein the preparation process comprises the following steps: S1. Dissolving zinc nitrate hexahydrate and titanium tetrachloride in deionized water to prepare a mixed solution with a total metal ion concentration of 0.1-0.3 mol / L, then adding hexamethylenetetramine to the mixed solution and adjusting the pH of the solution to 8-10 to form a precursor solution; S2. Transfer the precursor solution to a high-pressure reactor and react at 120-180° C. for 6-12 hours; after the reaction, cool to room temperature, collect the precipitate by centrifugation, wash with deionized water and anhydrous ethanol 3-5 times in sequence, and vacuum dry at 60-80° C. for 12-24 hours to obtain titanium dioxide or zinc oxide composite nanoparticles; S3, dispersing the dried nanoparticles in anhydrous ethanol to form a suspension with a mass fraction of 5%-10%, adding a silane coupling agent at a rate of 1%-5% of the mass of the nanoparticles, stirring and reacting at 50-80° C. for 2-6 hours, and after the reaction, centrifuging and vacuum drying to obtain surface-modified nano-optical functional particles; S4. The organic polymer matrix is heated to a molten state, and then the surface-modified nano-optical functional particles and the plasticizer are added, mixed under mechanical stirring for 10-30 minutes, and then formed by extrusion, injection molding or calendering to obtain the composite material.
6. The process for preparing a wide-angle field AR imaging nanocomposite material according to claim 5, characterized in that: In the above-mentioned S2, the ratio of zinc oxide to titanium dioxide in the composite nanoparticles is adjusted by controlling the molar ratio of zinc nitrate hexahydrate to titanium tetrachloride to be 1:1 to 3:
1.
7. The process for preparing a wide-angle field AR imaging nanocomposite material according to claim 5, characterized in that: In S3, the silane coupling agent is γ-aminopropyltriethoxysilane or γ-methacryloxypropyltrimethoxysilane, and 0.1%-1% of the catalyst dibutyltin dilaurate is added to the reaction system.
8. The process for preparing a wide-angle field AR imaging nanocomposite material according to claim 5, characterized in that: In the above S4, after adding the nano-optical functional particles and before adding the plasticizer, ultrasonic wave is introduced to assist in dispersion, with an ultrasonic wave frequency of 20-40 kHz, a power of 100-300 W, and a dispersion time of 5-15 minutes.
9. The process for preparing a wide-angle field AR imaging nanocomposite material according to claim 5, characterized in that: The zinc oxide target material is pretreated before use, specifically comprising the following steps: The zinc oxide target is crushed into powder with a particle size of ≤100 μm; Calcination at 400-600°C for 2-4 hours; Then add it into titanium tetrachloride solution and disperse it by ultrasonic for 30-60 minutes.
10. The process for preparing a wide-angle field AR imaging nanocomposite material according to claim 5, characterized in that: In S4, the molding process of the composite material is extrusion molding, and the temperature of each zone of the extruder is set to: 160-180°C in zone 1, 180-200°C in zone 2, 200-220°C in zone 3, 210-230°C in the die, and the screw speed is 50-120rpm.