High-light-transmittance thermosetting composite material and preparation method thereof
By preparing a high-transmittance thermosetting composite material, combined with glass fiber cloth and modified resin, the problems of insufficient strength, durability and environmental adaptability of traditional transparent materials are solved, and the application of high-performance transparent structures is realized.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-05
- Publication Date
- 2026-03-27
AI Technical Summary
Traditional transparent composite materials suffer from problems such as poor weather resistance, easy yellowing, easy interface failure, and insufficient strength in high-end manufacturing fields such as aerospace and electronic equipment, making it difficult to meet the needs of high-performance transparent structures.
A thermosetting composite material with high light transmittance was prepared by using a combination of glass fiber cloth with a volume ratio of 20% to 45% and resin with a volume ratio of 55% to 80% through surface modification and vacuum-assisted molding process. The mechanical properties and environmental adaptability of the material were improved by combining epoxy resin, curing agent, accelerator and light stabilizer.
It has achieved a composite material with high light transmittance, lightweight and high strength, and strong weather resistance, which can meet the high-end manufacturing needs of aerospace and electronic equipment and provides a brand-new transparent structure solution.
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Figure CN121736440A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of composite materials, and in particular to a high-transmittance thermosetting composite material and a preparation method thereof. BACKGROUND
[0002] In the process of continuous development in the modern industrial field, the demand for multifunctional materials is increasing, which not only requires the material to have basic structural properties, but also needs to integrate light transmission, heat insulation, lightweight and other properties. Traditional materials such as glass have good light transmission, but have disadvantages such as fragility, heaviness, and poor formability. While ordinary plastics are lightweight and not easy to break, they have problems such as insufficient strength and easy aging. The United States first developed unsaturated polyester transparent glass steel in 1949, opening up the research of transparent composite materials. Early transparent composite materials mainly used unsaturated polyester and alkali-free glass fiber as basic raw materials and were formed by hand lay-up process, which to some extent realized the combination of light transmission and structural function, but still had problems such as poor weather resistance, easy yellowing, and easy interface failure. Traditional transparent materials have disadvantages such as brittleness, degradation of optical performance, contradiction between lightweight and strength, insufficient scratch and wear resistance, difficulty in forming complex structures, and poor environmental adaptability, which are difficult to meet the needs of high-end manufacturing fields such as aerospace and electronic equipment. SUMMARY
[0003] The present application provides a high-transmittance thermosetting composite material and a preparation method thereof to solve the problems in the background art.
[0004] In a first aspect, the present application provides a high-transmittance thermosetting composite material, the preparation raw materials of the high-transmittance thermosetting composite material include 20% to 45% by volume of glass fiber cloth and 55% to 80% by volume of resin composition. The fiber size of the glass fiber cloth is 5 μm to 30 μm; the resin composition includes 42% to 62% by mass of epoxy resin monomer, 35% to 55% by mass of curing agent, 0.5% to 2.5% by mass of accelerator, and 0.5% to 2.5% by mass of light stabilizer.
[0005] In a second aspect, the present application provides a preparation method of the high-transmittance thermosetting composite material as described above, including: Step 1, surface modification of the glass fiber cloth by immersing it in an epoxy silane coupling agent solution to obtain surface-modified glass fiber cloth; Step 2, mixing the epoxy resin, curing agent, accelerator, and light stabilizer uniformly and then degassing to obtain a resin composition; Step 3, dry the surface modified glass fiber cloth, cut to the required size, then flatten, lay layer by layer into the mold, then assemble the mold according to the vacuum assisted forming process, connect the vacuum system, carry out vacuum detection and check the leakage points until qualified; Step 4, when the mold reaches the injection temperature, start injecting the resin, and when the resin fully impregnates the glass fiber cloth, turn off the vacuum; Step 5, place the mold in the oven, run the curing program according to the process parameters of the resin, take out the mold after curing and disassemble to obtain a high light transmittance thermosetting composite material.
[0006] Further, the solvent of the epoxy silane coupling agent solution in step 1 is ethanol and water, and the mass concentration is 2%~4%; the surface modification time is 0.5h~2h.
[0007] Further, the epoxy resin in step 2 is at least one of aliphatic epoxy resin, bisphenol A type epoxy resin, and bisphenol F type epoxy resin.
[0008] Further, the curing agent in step 2 is at least one of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, and phthalic anhydride.
[0009] Further, the accelerator in step 2 is at least one of 2,4,6-tris(dimethylaminomethyl)phenol, 2-ethyl-4-methylimidazole, triethylamine, and benzyl dimethylamine.
[0010] Further, the light stabilizer in step 2 is a hindered amine light stabilizer.
[0011] Further, the drying temperature in step 3 is 60℃~80℃.
[0012] Further, the injection temperature in step 4 is 50℃~70℃.
[0013] Further, the curing program in step 5 is: first 80℃~100℃ for 40min~80min, then 100℃~120℃ for 100min~150min, and finally 130℃~150℃ for 20min~40min.
[0014] The above technical solutions of the present application have the following advantages: This application provides a high-transmittance thermosetting composite material and its preparation method. This high-performance composite material combines a transparent resin matrix with specially treated glass fibers. While maintaining transparency, the mechanical properties and environmental adaptability of the material are significantly improved through the reinforcement of the glass fibers. Through innovative material design, it overcomes the shortcomings of traditional transparent materials in terms of strength, durability, and environmental adaptability, providing a new solution for high-performance transparent structures in high-end fields such as aerospace and electronic equipment. Furthermore, with advancements in process technology and materials science, and the continuous deepening of research on fiber-resin interface optimization and multifunctionality of composite materials, its application prospects will be even broader. Attached Figure Description
[0015] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0016] Figure 1 This is a schematic diagram of the structure of the high light transmittance thermosetting composite material provided in this application. Detailed Implementation
[0017] To make the technical problems, technical solutions, and beneficial effects of this application clearer, the following detailed description is provided in conjunction with embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.
[0018] In this application, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or multiple items. For example, "at least one of a, b, or c", or "at least one of a, b, and c", can both mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple.
[0019] It should be understood that in the various embodiments of this application, the order of the above processes does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.
[0020] The terminology used in the embodiments of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of this application. The singular forms “a,” “the,” and “the” used in the embodiments of this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.
[0021] The weights of the relevant components mentioned in the embodiments of this application can refer not only to the specific content of each component, but also to the proportional relationship between the weights of the components. Therefore, any scaling up or down of the content of the relevant components according to the embodiments of this application is within the scope disclosed in the embodiments of this application. Specifically, the mass described in the embodiments of this application can be a well-known unit of mass in the chemical industry, such as µg, mg, g, or kg.
[0022] The terms "first" and "second" are used for descriptive purposes only, to distinguish objects, such as substances, from one another, and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. For example, without departing from the scope of the embodiments of this application, "first XX" may also be referred to as "second XX," and similarly, "second XX" may also be referred to as "first XX." Thus, features defined with "first" and "second" may explicitly or implicitly include one or more of that feature.
[0023] The purpose of this application is to provide a high-transmittance thermosetting composite material and its preparation method, which can achieve a balance between optical transparency and mechanical properties, and simultaneously meet the dual requirements of structural load-bearing and light transmission functions. It can be applied to the field of electronic equipment and the protective structure of aviation radar domes.
[0024] The specific embodiments of this application will be described in further detail below with reference to the accompanying drawings and examples. The following examples are used to illustrate this application, but are not intended to limit the scope of this application.
[0025] This application provides a high-transmittance thermosetting composite material, such as... Figure 1 As shown, by volume fraction, the high light transmittance thermosetting composite material comprises: 20%~45% glass fiber cloth and 55%~80% resin composition; the fiber size of the glass fiber cloth is preferably 5μm~30μm, more preferably 7μm~15μm; by mass fraction, the resin composition comprises: 42%~62% epoxy resin monomer, 35%~55% curing agent, 0.5%~2.5% accelerator, and 0.5%~2.5% light stabilizer.
[0026] From a structural and functional perspective, high-transmittance thermosetting composite materials have the following characteristics: (1) High light transmittance. By selecting resins with high light transmittance (modified epoxy resin) and ultra-fine glass fibers (diameter less than 10μm), the material can still maintain more than 90% light transmittance after fiber reinforcement, which is close to the transparency of ordinary glass or transparent polymers.
[0027] (2) Excellent mechanical properties. The presence of glass fiber significantly improves the material’s impact resistance, reduces the risk of cracking or breaking due to external forces, and has tensile and flexural strengths that are much higher than those of traditional transparent materials (such as PMMA or PC), while maintaining lightweight (density of about 1.5-2.0 g / cm³).
[0028] (3) Strong weather resistance. UV stabilizers can be added to the resin matrix to solve the problems of yellowing and aging caused by sun exposure in traditional transparent materials. Furthermore, the cured resin has better resistance to chemicals such as acids, alkalis and solvents than ordinary polymers, thus extending the service life of the material.
[0029] (4) Design flexibility. Resin transfer molding process can customize material properties by adjusting the number of glass fiber cloth layers and the resin ratio, and supports molding of complex shapes.
[0030] This application also provides a method for preparing the high-transmittance thermosetting composite material as described above, comprising the following steps: (1) The glass fiber cloth was impregnated in an epoxy silane coupling agent solution for surface modification to obtain a surface-modified glass fiber cloth; (2) After uniformly mixing epoxy resin with curing agent, accelerator and light stabilizer, degas the mixture to obtain a resin composition; (3) Dry the surface-modified glass fiber cloth obtained in step (1), cut it to the required size, flatten it, lay it layer by layer into the mold, and then assemble the mold in sequence according to the vacuum-assisted molding process, connect it to the vacuum system, perform vacuum testing and check for leaks until it is qualified. (4) When the mold reaches the injection temperature, start injecting resin. After the resin has completely impregnated the glass fiber cloth, turn off the vacuum. (5) Place the mold in the oven and run the curing program according to the resin process parameters. After curing, remove the mold and disassemble it to obtain a high light transmittance thermosetting composite material.
[0031] In some embodiments, the solvent of the epoxy silane coupling agent solution in step (1) is ethanol and water, with a mass concentration of 2% to 4%; the surface modification time is 0.5 h to 2 h.
[0032] In some embodiments, the epoxy resin in step (2) is at least one of alicyclic epoxy resin, bisphenol A type epoxy resin, and bisphenol F type epoxy resin.
[0033] In some embodiments, the curing agent in step (2) is at least one of methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, and phthalic anhydride.
[0034] In some embodiments, the promoter in step (2) is at least one of 2,4,6-tris(dimethylaminomethyl)phenol, 2-ethyl-4-methylimidazol, triethylamine, and benzyldimethylamine.
[0035] In some embodiments, the light stabilizer in step (2) is a hindered amine light stabilizer.
[0036] In some embodiments, the drying temperature in step (3) is 60°C to 80°C.
[0037] In some embodiments, the injection temperature in step (4) is 50°C to 70°C.
[0038] In some embodiments, the curing process in step (5) is as follows: first, cure at 80℃~100℃ for 40min~80min, then cure at 100℃~120℃ for 100min~150min, and then cure at 130℃~150℃ for 20min~40min.
[0039] The following is a description through specific embodiments.
[0040] Example 1 (1) The glass fiber cloth was impregnated in 500g of 2% epoxy silane coupling agent solution for surface modification for 1h, and then dried at 70℃ for 1h to obtain surface modified glass fiber cloth. (2) After mixing 200g of epoxy resin with 160g of curing agent, 3g of accelerator and 5g of light stabilizer evenly, degas the mixture to obtain a resin composition. (3) Cut the surface-modified glass fiber cloth into 200*200mm pieces. 2 After flattening, lay the three layers one by one into the mold, then assemble the mold and connect it to the vacuum system for vacuum testing and leak detection until it passes the test. (4) When the mold reaches 60°C, start injecting resin. After the resin has completely impregnated the glass fiber cloth, turn off the vacuum. (5) Place the mold in an oven and cure it at 80°C for 60 min, then at 120°C for 150 min, and then at 150°C for 30 min to obtain a high-transmittance thermosetting composite material with a glass fiber volume fraction of 21.5% and a thickness of 0.4 mm.
[0041] Example 2 The surface-modified glass fiber cloth from step (3) of Example 1 is cut into 200*200mm pieces. 2After flattening, four layers are laid one by one into the mold. Other processes are the same as in Example 1, resulting in a high-transmittance thermosetting composite material with a glass fiber volume fraction of 31.7% and a thickness of 0.4 mm.
[0042] Example 3 The surface-modified glass fiber cloth from step (3) of Example 1 is cut into 200*200mm pieces. 2 The mixture was then flattened and laid in six layers sequentially into the mold, with the other processes being the same as in Example 1. A high-transmittance thermosetting composite material with a glass fiber volume fraction of 44.7% and a thickness of 0.4 mm was obtained.
[0043] Comparative Example 1 200g of epoxy resin was mixed evenly with 160g of curing agent and 3g of accelerator, and then degassed to obtain a resin composition; untreated fiberglass cloth was cut into 200*200mm pieces. 2 The fiberglass cloth was then laid flat in three layers and placed into the mold. The mold was then assembled and connected to the vacuum system. When the mold reached 60°C, resin was injected. After the resin completely impregnated the fiberglass cloth, the vacuum was turned off. The mold was then placed in an oven and cured at 80°C for 60 minutes, then at 120°C for 150 minutes, and then at 150°C for 30 minutes to obtain a thermosetting composite material with a fiberglass volume fraction of 21.9% and a thickness of 0.4 mm.
[0044] The material test performance of the embodiments and comparative examples in this application is as follows: The high-transmittance thermosetting composite material and its preparation method provided in this application achieve the design goal of integrated structure and function, possessing advantages such as high transmittance, lightweight and high strength, strong weather resistance, and designability, breaking through the limitations of traditional materials in terms of strength, transparency, and function. When the glass fiber volume fraction is 40%, the transmittance of the composite material is higher than 92%, and its optical performance is comparable to that of traditional transparent materials, but its impact resistance and flexural strength are far superior to those of traditional transparent materials. This can meet the demand for lightweight, high-strength, and transparent materials in high-end manufacturing fields such as aerospace and electronic equipment.
[0045] It should be noted that the various embodiments in this specification are described in a progressive manner, and the same or similar parts between the various embodiments can be referred to mutually. Each embodiment focuses on describing the differences from other embodiments. This application is not limited to the specific methods described above and shown in the figures. Furthermore, for the sake of brevity, detailed descriptions of known methods and techniques are omitted here.
[0046] The above-described embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application, and should all be included within the protection scope of this application.
Claims
1. A high-transmittance thermosetting composite material, characterized in that, The raw materials for preparing the high light transmittance thermosetting composite material include 20% to 45% by volume glass fiber cloth and 55% to 80% by volume resin composition. The fiber size of the glass fiber cloth is 5μm to 30μm; the resin composition includes 42% to 62% by mass of epoxy resin monomer, 35% to 55% by mass of curing agent, 0.5% to 2.5% by mass of accelerator and 0.5% to 2.5% by mass of light stabilizer.
2. A method for preparing a high-transmittance thermosetting composite material as described in claim 1, characterized in that, include: Step 1: Impregnate the glass fiber cloth with an epoxy silane coupling agent solution to perform surface modification, and obtain surface-modified glass fiber cloth; Step 2: After uniformly mixing epoxy resin with curing agent, accelerator and light stabilizer, degas the mixture to obtain a resin composition; Step 3: Dry the surface-modified glass fiber cloth, cut it to the required size, flatten it, and lay it layer by layer into the mold. Then, assemble the mold according to the vacuum-assisted molding process, connect it to the vacuum system, perform vacuum testing and check for leaks until it is qualified. Step 4: When the mold reaches the injection temperature, start injecting resin. After the resin has completely impregnated the fiberglass cloth, turn off the vacuum. Step 5: Place the mold in the oven and run the curing program according to the resin's process parameters. After curing, remove the mold and disassemble it to obtain a high-transmittance thermosetting composite material.
3. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, In step 1, the solvent for the epoxy silane coupling agent solution is ethanol and water, with a mass concentration of 2% to 4%; the surface modification time is 0.5 h to 2 h.
4. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, In step 2, the epoxy resin is at least one of alicyclic epoxy resin, bisphenol A type epoxy resin, and bisphenol F type epoxy resin.
5. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, The curing agent in step 2 is at least one of methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, and phthalic anhydride.
6. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, The accelerator in step 2 is at least one of 2,4,6-tris(dimethylaminomethyl)phenol, 2-ethyl-4-methylimidazol, triethylamine, and benzyldimethylamine.
7. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, The light stabilizer in step 2 is a hindered amine light stabilizer.
8. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, The drying temperature in step 3 is 60℃~80℃.
9. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, The injection temperature in step 4 is 50℃~70℃.
10. The method for preparing the high-transmittance thermosetting composite material as described in claim 2, characterized in that, The curing procedure in step 5 is as follows: first, cure at 80℃~100℃ for 40min~80min, then cure at 100℃~120℃ for 100min~150min, and then cure at 130℃~150℃ for 20min~40min.