A method and apparatus for forming a polymer-based composite

By controlling the polymerization process of polymer monomers using aluminum molding molds and a lifting platform, the problem of volume shrinkage in the preparation of polymer-based composite materials has been solved, realizing an efficient molding method and device, and improving the yield and mechanical properties of composite materials.

CN116353108BActive Publication Date: 2025-10-21SHENZHEN TAOTAO TECH CO LTD
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Patent Information

Application Number
CN202310232191.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-01
Publication Date
2025-10-21
Estimated Expiration
2043-03-01

AI Technical Summary

Technical Problem

During the preparation of polymer-based composite materials, the volume shrinkage of polymer monomers can cause deformation or damage to the framework substrate, affecting the mechanical and optical properties of the composite material.

Method used

An aluminum molding mold is used for thermal initiation and prepolymerization reaction. The polymer monomer is slowly introduced into the curing device via a lifting platform to control the polymerization process. Uncured polymer monomers are used to fill the cured area to compensate for volume shrinkage. Pulsed ultrasonic and directional annealing are used to improve the polymerization effect.

Benefits of technology

It effectively avoids the defect of volume shrinkage after molding of polymer-based composite materials, improves yield and mechanical properties, and reduces production costs.

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Abstract

The application relates to a forming method of a polymer-based composite material, comprising the following steps: S1: placing a frame substrate in a forming mold, the forming mold being matched with the shape of the frame substrate, and the forming mold being provided with an impregnation solution; the impregnation solution comprising a polymer monomer and an initiator; S2: placing the forming mold provided with the frame substrate and the impregnation solution in a heating device, and performing a thermal initiation and a prepolymerization reaction at a first temperature to obtain an intermediate; S3: placing the obtained intermediate and the forming mold on a lifting platform, and driving the forming mold to slowly enter a solidification device at a speed of 1mm / h-5mm / h until the forming mold is completely placed in the solidification device; and then, heat preservation is carried out at a second temperature, so that the polymer monomer is completely polymerized to obtain a polymer-based composite material. The application controls the shrinkage direction of the polymer monomer polymerization, and avoids the volume shrinkage defect of the polymer-based composite material after forming.
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Description

Technical Field

[0001] The present invention relates to the technical field of composite materials, and in particular to a molding method and a molding device for a polymer-based composite material. Background Art

[0002] The preparation method of the polymer-based composite material includes the following process route: first, a frame substrate is prepared, and then the obtained frame substrate is impregnated in a polymer or polymer monomer solution, so that the polymer or polymer monomer penetrates into the frame substrate to fill the frame substrate, wherein the polymer monomer is suitable for a frame substrate with a smaller pore structure; then the frame substrate filled with the polymer or polymer monomer is cured to finally obtain a polymer-based composite material.

[0003] However, during the curing process, the polymer or polymer monomer will shrink in volume, which will cause the frame substrate 4 to deform or be damaged. In particular, the curing process of the polymer monomer is accompanied by a polymerization reaction. When the polymer monomer polymerizes, numerous covalent bonds are formed, which means a greater volume shrinkage. Taking polymethyl methacrylate (PMMA) as an example, there is a 20% volume shrinkage from the monomer methyl methacrylate (MMA) to the polymerization of polymethyl methacrylate. When the frame substrate is made of ceramic material, since ceramic is a relatively rigid material, it cannot deform along with the shrinkage of the polymer. Therefore, the volume shrinkage generated during the polymer polymerization process will leave defects in the composite material. When the bonding force between ceramic and polymer is strong, forced deformation of the polymer may even cause the frame substrate to break. And as the volume of the polymer-based composite material increases, the defects caused by the shrinkage of the polymer increase, seriously affecting the mechanical and optical properties of the composite material. Therefore, it is extremely important to obtain a molding method that can avoid the defects of volume shrinkage generated after the polymer-based composite material is molded. Summary of the Invention

[0004] The object of the present invention is to solve the above problems and provide a composite material forming method and forming device.

[0005] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows:

[0006] A method for forming a polymer-based composite material comprises the following steps:

[0007] S1: placing the frame substrate in a forming mold, the forming mold being in conformity with the shape of the frame substrate, and the forming mold being provided with an impregnation solution; the impregnation solution comprising a polymer monomer and an initiator; the forming mold being made of aluminum material, and having a thickness of 0.5-2 mm;

[0008] S2: placing the forming mold containing the frame substrate and the impregnation solution in a heating device, and performing thermal initiation and prepolymerization reaction at a first temperature to obtain an intermediate;

[0009] In step S2, the entire polymerization reaction has been completed by 70%-80% at the first temperature, but the polymer has not yet solidified and retains a certain fluidity, with a viscosity of 1-100 mPa·s to ensure smooth progress of the next polymerization step;

[0010] S3: The intermediate obtained is placed together with the molding die on a lifting platform, and the lifting platform drives the molding die to slowly enter the curing device at a speed of 1mm / h-5mm / h until the molding die is completely placed in the curing device. The heating temperature of the curing device is the second temperature, and the second temperature is 35-60°C; then, the temperature is kept at the second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material.

[0011] Preferably, in step S1, before placing the frame substrate in the forming mold, the step further includes performing a surface modification step on the frame substrate: immersing the frame substrate in a silane coupling agent solution, and then drying the frame substrate.

[0012] Preferably, the preparation of the silane coupling agent solution comprises the steps of: dissolving the silane coupling agent in an alcohol-water mixture, adjusting the pH value to 2-4, and stirring for 1-1.5 hours; the mass ratio of alcohol to water in the alcohol-water mixture is 9:1; and the silane coupling agent comprises one or both of silane coupling agent KH-570 and silane coupling agent KH-550.

[0013] Preferably, the temperature rise curve of the drying treatment is: from room temperature to 60-70°C, keeping warm for 1-2 hours; from 60-70°C to 120-130°C, keeping warm for 1.5-2 hours; to ensure that the silane coupling agent reacts completely while drying the alcohol aqueous solution.

[0014] Preferably, in step S1, the frame substrate is a frame substrate having a porous structure; the frame substrate includes one of a rigid organic frame substrate, a ceramic frame substrate or a glass fiber frame substrate.

[0015] Preferably, in step S3, the curing device includes one of a heat curing device, a cold curing device, a light curing device or a chemical curing device.

[0016] Preferably, in step S3, the curing device is a heat curing device, and the heat curing device is a water bath heating device;

[0017] Step S3 also includes simultaneously applying pulsed ultrasound to the water bath heating device; the ultrasound frequency is 40-80 Hz, the ultrasound on time is 1-2 minutes, and the ultrasound off time is 5-10 minutes.

[0018] Preferably, after step S3, the obtained polymer-based composite material is further subjected to directional annealing treatment, and the directional annealing treatment includes the steps of: drying the polymer-based composite material at 85-95°C for 2-2.5h, and then placing the polymer-based composite material still in a high temperature state on a metal plate at room temperature.

[0019] Preferably, the frame substrate is a frame substrate having a through-hole structure.

[0020] The present invention also relates to a molding device used in the molding method of the polymer-based composite material; the molding device comprises a molding die and a lifting platform for driving the molding die to move.

[0021] The beneficial effects produced by the present invention include at least:

[0022] The present invention discloses a molding method and molding device for a polymer-based composite material. An intermediate obtained by thermal initiation and prepolymerization reaction is loaded into a molding mold and slowly enters a curing device at a certain speed, so that the polymer monomer is directionally polymerized. The polymer intermediate that has not undergone polymerization reaction is used to fill the polymerized and cured portion, thereby achieving compensation and offset of the structure after polymerization and curing. Furthermore, the shrinkage direction of the polymer monomer polymerization is controlled, thereby avoiding the defect of volume shrinkage caused by the molding of the polymer-based composite material, and providing a new idea for the preparation of the polymer-based composite material.

[0023] The forming mold of the present invention is made of aluminum with a thickness of 0.5-2 mm. Aluminum is a good conductor of heat, which improves thermal conductivity and enhances the fluidity of the polymer monomer. The forming mold is detachable and reusable, reducing production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the working state of the molding device of the present invention;

[0025] Among them, 1 is the forming mold, 2 is the lifting platform, 3 is the curing device, and 4 is the frame base material. DETAILED DESCRIPTION

[0026] To facilitate understanding of the present invention, the present invention will be described more fully below with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the accompanying drawings. However, the present invention may be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and comprehensive understanding of the present disclosure.

[0027] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in this specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0028] In the present invention, descriptions such as “first”, “second”, etc. are only used for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of the indicated technical features.

[0029] Example 1

[0030] The inventive concept of the present invention is as follows: In the initial stage of the prepolymerization reaction, polymer monomers polymerize to form dispersed, elongated micelles. Since the polymerization reaction releases a large amount of heat, it disturbs and slows the diffusion of the monomers, causing the elongated micelles to gradually connect and fuse with each other, spreading out to form a layered adhesive. Under the guidance of thermal diffusion from the aluminum molding mold, the layered adhesive moves toward the frame substrate. When the frame substrate is a ceramic substrate, and the ceramic substrate has a porous layered structure, the layered adhesive forms an angle of 0-5° with the ceramic layer, and the pores in the ceramic substrate not filled with polymer are also basically arranged parallel to the layered adhesive. At this point, the layered adhesive is an intermediate.

[0031] The intermediate further solidifies as the molding die descends. The solidification shrinkage is centered on the polymer itself. The intermediate, which originally had a rectangular cross-section, shrinks to form a spherical structure with an arc-shaped outer surface, providing a smooth channel for the intermediate adjacent to the spherical structure that still has a certain fluidity to be fully polymerized and the polymer monomer to be polymerized. The pores formed by solidification shrinkage are completely filled with sufficient supply.

[0032] A method for forming a polymer-based composite material comprises the following steps:

[0033] S1: placing the frame substrate 4 in a forming mold 1, wherein the forming mold 1 matches the shape of the frame substrate 4, and an impregnation solution is provided in the forming mold 1; the impregnation solution includes a polymer monomer and an initiator;

[0034] In the present invention, there is no specific limitation on the order of placing the impregnation solution. The impregnation solution may be placed before the frame substrate is provided or after the frame substrate is placed in the forming mold 1 .

[0035] S2: The forming mold 1 containing the frame substrate 4 and the impregnation solution is placed in a heating device, and a thermal initiation and prepolymerization reaction is carried out at a first temperature to obtain an intermediate; preferably, the first temperature is 80°C-95°C, and the time of the thermal initiation and prepolymerization reaction is 20-30 minutes; of course, the time of the thermal initiation and prepolymerization reaction is set according to the specific size of the reactants. During step S2, the initiator (for example: BPO or AIBN) is activated to initiate the polymerization reaction of the polymer monomer (for example: MMA). During the polymer polymerization process, new chemical bonds are continuously formed between the monomers, and the polymer chain length gradually increases. Therefore, the viscosity of the impregnation solution gradually increases while releasing heat. Preferably, in the present invention, when the impregnation solution reaches the viscosity of glycerol (triglyceride), the forming mold containing the frame substrate and the impregnation solution is removed from the heating device to obtain the intermediate.

[0036] S3: The intermediate product and the forming mold 1 are placed on a lifting platform 2. The lifting platform 2 slowly drives the forming mold 1 into the curing device 3 at a speed of 1 mm / h-5 mm / h until the forming mold 1 is completely placed in the curing device 3. The intermediate product is then kept at a second temperature to allow the polymer monomer to completely polymerize, thereby obtaining a polymer-based composite material. Preferably, the second temperature is 35-60°C, and the holding time is 3-28 hours.

[0037] The molding method of the polymer-based composite material described in the present invention is as follows: the frame substrate 4 is placed in the molding mold 1, and then the intermediate obtained after thermal initiation and pre-polymerization treatment is slowly placed into the curing device 3 together with the molding mold 1, so that the polymer monomer that penetrates into the frame matrix gradually solidifies from the area close to the curing device 3 to the area far away from the curing device 3 in the order in which the molding mold 1 is placed into the curing device 3. During this process, the uncured polymer monomer flows into the polymerized and cured structure, fills the cured area, compensates for and reduces the volume shrinkage generated during the polymerization and curing process, overcomes the structural defects of the polymer-based composite material caused by the polymerization of the polymer monomer, avoids the damage to the frame substrate 4 caused by the force of the cured polymer on the frame matrix during the polymerization and curing process, and improves the yield of the polymer-based composite material preparation.

[0038] In step S1, the forming mold 1 is made of aluminum with a thickness of 0.5-2 mm. Aluminum is a good conductor of heat, which improves thermal conductivity and enhances the fluidity of the polymer monomer. The forming mold 1 is removable and reusable, reducing production costs. The thin thickness of the forming mold 1 ensures that the subsequently applied pulsed ultrasonic wave can be transmitted into the forming mold 1, acting on the frame substrate and the impregnation solution.

[0039] Before placing the frame substrate 4 in the molding die 1 in step S1, the frame substrate 4 is subjected to a surface modification step by immersing the frame substrate 4 in a silane coupling agent solution and then drying the silane coupling agent solution. Furthermore, preferably, the frame substrate 4 can be immersed in the silane coupling agent solution under a vacuum environment of 1-5 Pa.

[0040] The silane coupling agent solution is prepared by dissolving the silane coupling agent in an alcohol-water mixture, adjusting the pH to 2-4, and stirring for 1-1.5 hours to allow the silane coupling agent to fully dissolve or hydrolyze. The alcohol-water mixture has a mass ratio of alcohol to water of 9:1. The silane coupling agent rapidly hydrolyzes in an acidic aqueous solution to produce ionic groups, which react chemically with the ceramic surface and covalently bond to the surface of the frame substrate. Using an alcohol-water solution rather than an aqueous solution promotes hydrolysis and increases the reaction rate. The silane coupling agent includes one or both of silane coupling agent KH-570 and silane coupling agent KH-550. The chemical name of silane coupling agent KH-570 is γ-methacryloyloxypropyl; the chemical name of silane coupling agent KH550cas:919-30-2 is γ-aminopropyltriethoxysilane. Preferably, the pH is adjusted to 2-4 using acetic acid or citric acid.

[0041] The drying process has a heating curve of: from room temperature to 60-70°C, holding for 1-2 hours; then from 60-70°C to 120-130°C, holding for 1.5-2 hours. The temperature in the first stage is within the range of 60-70°C, which is lower than the lowest boiling point of the alcohol-water mixture, allowing the alcohol-water mixture to volatilize but not boil. This ensures that the alcohol-water mixture is completely evaporated, avoiding uneven distribution of the silane coupling agent caused by boiling of the alcohol-water mixture. After the alcohol-water mixture is completely evaporated, the drying temperature is increased to improve the efficiency of the drying process.

[0042] In step S1, the frame substrate 4 is a frame substrate 4 having a porous structure; the frame substrate 4 includes one of a rigid organic frame substrate 4 such as carbon fiber, a ceramic frame substrate 4, or a glass fiber frame substrate 4. Preferably, the frame substrate 4 is a ceramic frame substrate having a through-hole structure. Furthermore, if the frame substrate has a conformationally anisotropic structure, the descending direction of the lifting platform is parallel to the axial direction of the pores of the frame substrate. For example, if the ceramic frame substrate has a porous layered structure, the layered structure inclination angle should be less than or equal to 60°.

[0043] In step S3 , the curing device 3 includes one of a heat curing device 3 , a cold curing device 3 , a light curing device 3 or a chemical curing device 3 .

[0044] In step S3, the curing device 3 is a thermal curing device 3, which is a water bath heating device. When the temperature is maintained at the second temperature, the liquid level is completely cured at a point 2-3 mm below the curing device. Specifically, starting from the liquid level when the upper end of the forming mold is completely immersed in the water bath, the polymer is completely cured when the upper end of the forming mold descends 2-3 mm, and the curing reaction process ends. In the present invention, the first temperature is the initiation temperature of the thermal initiator, and the second temperature is the polymerization temperature of the polymer. In step S3, as the lifting platform descends, the portion that first contacts the water bath undergoes polymerization, and the polymer gradually solidifies. The heat generated by polymerization is absorbed by the water bath, and the volume shrinkage that occurs is filled by the fluid intermediate polymer that has not yet undergone polymerization. In conventional water bath polymerization processes, the entire solution is immersed in the water bath. If the polymerization temperature is maintained at a higher level, the heat generated during the polymerization process is difficult to release. The generated heat accelerates the polymerization reaction, generating more heat, which leads to implosion. The product produced by implosion has poor mechanical and optical properties. Therefore, in conventional polymerization methods, the second temperature is generally much lower than the first temperature. When the molding device of the present invention is used, even if a higher temperature is used for polymerization, the amount of polymerization reaction occurring per unit time and the rapid heat dissipation of the aluminum mold can be controlled by changing the lifting and lowering rates, making the heat release of the entire reaction more controllable and avoiding explosion, thereby achieving a high-temperature polymerization reaction.

[0045] The process of carrying out the curing reaction in the curing device 3 at the second temperature also includes applying pulsed ultrasound to the water bath heating device; the ultrasonic frequency is 40-80Hz, the ultrasonic on time is 1-2min, and the ultrasonic intermittent time is 5-10min. Optionally, the number of pulsed ultrasounds is set according to the specific actual operating conditions. In the present invention, applying pulsed ultrasound during the curing reaction can degas the reaction system and remove the gas generated by the initiator; increase the polymerization rate of the polymer monomer and improve production efficiency; improve the fluidity of the polymer monomer, so that the shrinkage generated by the polymer monomer during the polymerization process is more uniform; compared with uninterrupted ultrasonic treatment, the use of pulsed ultrasound is more energy-saving and environmentally friendly.

[0046] Furthermore, after step S3, the obtained polymer-based composite material is subjected to a directional annealing treatment, wherein the directional annealing treatment comprises the steps of drying the polymer-based composite material at 85-95° C. for 2-2.5 hours, and then placing the polymer-based composite material still in a high-temperature state on a metal plate at room temperature. The metal plate is preferably an aluminum metal plate.

[0047] The present invention also relates to a molding device for use in the aforementioned method for molding a polymer-based composite material. The molding device comprises a molding die 1 and a lifting platform 2 for driving the molding die 1. When the curing device 3 is a water bath heating device, the molding device further comprises a lifting frame disposed within the water bath heating device for mounting the lifting platform 2. During use, the molding die 1 is placed on the lifting platform 2, and the lifting frame drives the lifting platform 2 toward or away from the water bath heating device, driving the molding die 1 up and down.

[0048] Example 2

[0049] In this embodiment, the polymer-based composite material to be prepared is a PMMA / ceramic composite material, and the ceramic content is 60% by mass. The frame substrate 4 is a zirconia ceramic frame substrate, and the ceramic frame substrate includes a lamellar frame structure parallel to each other. The dimensions of the ceramic frame substrate are length * width * height = 20mm * 20mm * 10mm, and the porosity of the ceramic frame substrate is 40%. It should be noted that the dimensions of the ceramic frame involved in this embodiment are not the only dimensions of the frame substrate 4 described in the present invention. In other embodiments, the dimensions of the frame substrate 4 can be adaptively adjusted according to actual needs.

[0050] The molding method of the polymer-based composite material described in this embodiment includes the following steps:

[0051] The ceramic frame substrate 4 is placed in a forming mold 1 that matches its shape. The forming mold 1 is provided with an impregnation solution. In this embodiment, the impregnation solution includes an MMA monomer solution and an initiator.

[0052] Placing the forming mold 1 containing the ceramic frame substrate and the impregnation solution in a heating device, and performing thermal initiation and prepolymerization reactions at a first temperature to obtain an intermediate; the heating device is a water bath heating device, the first temperature is 80-95° C., and the thermal initiation and prepolymerization reaction time is 20 minutes;

[0053] The obtained intermediate is placed together with the forming mold 1 on a lifting platform 2, and the lifting platform 2 drives the forming mold 1 to slowly enter the curing device 3 at a speed of 3 mm / h until the forming mold 1 is completely placed in the curing device 3; then the temperature is kept at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, i.e., the water bath temperature, is 35°C, and the insulation time is 28h.

[0054] Example 3

[0055] Compared with Example 2, the difference of this embodiment is that in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the molding mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the molding mold 1 to slowly enter the curing device 3 at a speed of 3 mm / h until the molding mold 1 is completely placed in the curing device 3; then keep warm at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 45°C, and the insulation time is 6 hours.

[0056] Example 4

[0057] Compared with Example 2, the difference of this embodiment is that in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the molding mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the molding mold 1 to slowly enter the curing device 3 at a speed of 1 mm / h until the molding mold 1 is completely placed in the curing device 3; then the temperature is kept at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 60°C, and the insulation time is 10 hours.

[0058] Example 5

[0059] Compared with Example 2, the difference of this embodiment is that in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the molding mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the molding mold 1 to slowly enter the curing device 3 at a speed of 2 mm / h until the molding mold 1 is completely placed in the curing device 3; then the temperature is kept at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 60°C, and the insulation time is 6 hours.

[0060] Example 6

[0061] Compared with Example 2, the difference of this embodiment is that in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the molding mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the molding mold 1 to slowly enter the curing device 3 at a speed of 3 mm / h until the molding mold 1 is completely placed in the curing device 3; then the temperature is kept at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 60°C, and the insulation time is 4 hours.

[0062] Example 7

[0063] Compared with Example 2, the difference of this embodiment is that in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the molding mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the molding mold 1 to slowly enter the curing device 3 at a speed of 4 mm / h until the molding mold 1 is completely placed in the curing device 3; then the temperature is kept at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 60°C, and the insulation time is 3h.

[0064] Example 8

[0065] Compared with Example 2, the difference of this embodiment is that in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the molding mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the molding mold 1 to slowly enter the curing device 3 at a speed of 5 mm / h until the molding mold 1 is completely placed in the curing device 3; then keep warm at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 60°C, and the insulation time is 3h.

[0066] Example 9

[0067] Compared with Example 2, the difference of this embodiment is that the frame substrate 4 is an alumina ceramic frame substrate; in the preparation method of the polymer-based composite material of this embodiment: the obtained intermediate and the forming mold 1 are placed together on the lifting platform 2, and the lifting platform 2 drives the forming mold 1 to slowly enter the curing device 3 at a speed of 3 mm / h until the forming mold 1 is completely placed in the curing device 3; then keep warm at a second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material; the curing device 3 is preferably a water bath heating device, the second temperature, that is, the water bath temperature is 60°C, and the insulation time is 3h.

[0068] Comparative Example 1

[0069] In Comparative Example 1, the obtained intermediate and the molding die 1 were directly and completely placed in a water bath heating device at a water bath temperature of 35° C. and reacted for 28 hours.

[0070] Comparative Example 2

[0071] In Comparative Example 2, the obtained intermediate and the molding die 1 were directly and completely placed in a water bath heating device at a water bath temperature of 45° C. and reacted for 6 hours.

[0072] Comparative Example 3

[0073] In Comparative Example 3, the obtained intermediate and the molding die 1 were directly and completely placed in a water bath heating device at a water bath temperature of 60° C. and reacted for 3 hours.

[0074] Test Case

[0075] The porosity, hardness, and strength tests were performed on the polymer-based composite materials obtained in Examples 2-9 and Comparative Examples 1-3. The test results are shown in the table below. The porosity refers to the porosity of the polymer phase in the obtained polymer-based composite material, and the porosity is measured using a water displacement method. The porosity testing method comprises the steps of first measuring the porosity of the frame substrate and then measuring the porosity of the obtained polymer-based composite material, where the porosity = the porosity of the obtained polymer-based composite material - the porosity of the frame substrate. The hardness is Vickers hardness.

[0076]

[0077] The porosity of the polymer-based composite materials prepared in Examples 2-9 is smaller than that of the polymer-based composite materials prepared in Comparative Examples 1-3 due to polymer infiltration, indicating that the preparation method of the polymer-based composite materials described in the present invention compensates for the structural defects caused by the polymerization and curing of the polymer monomers and overcomes the defect of volume shrinkage caused by the molding of the polymer-based composite materials.

[0078] The hardness and strength of the polymer-based composite materials obtained in Examples 2, 3, and 7-9 of the present invention are greater than those of the corresponding Comparative Examples 1, 2, and 3, indicating that the polymer-based composite materials obtained by the polymer-based composite material molding method and molding device described in the present invention have better mechanical properties than the prior art.

[0079] The technical features of the above embodiments can be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0080] The above embodiments merely represent preferred embodiments of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent. It should be noted that a person skilled in the art would be able to make various modifications and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. A method for forming a polymer-based composite material, comprising the steps of: S1: placing the frame substrate in a forming mold, the forming mold being in conformity with the shape of the frame substrate, and the forming mold being provided with an impregnation solution; the impregnation solution comprising a polymer monomer and an initiator; the forming mold being made of aluminum material, and having a thickness of 0.5-2 mm; S2: placing the forming mold containing the frame substrate and the impregnation solution in a heating device, and performing thermal initiation and prepolymerization reaction at a first temperature to obtain an intermediate; S3: The intermediate obtained is placed together with the molding die on a lifting platform, and the lifting platform drives the molding die to slowly descend at a speed of 1mm / h-5mm / h into the curing device until the molding die is completely placed in the curing device. The heating temperature of the curing device is the second temperature, and the second temperature is 35-60°C; then the temperature is kept at the second temperature to allow the polymer monomer to be completely polymerized to obtain a polymer-based composite material.

2. The method for forming a polymer-based composite material according to claim 1, wherein: In step S1, before placing the frame substrate in the forming mold, the step of surface modification of the frame substrate is further included: the frame substrate is immersed in a silane coupling agent solution and then dried.

3. The method for forming a polymer-based composite material according to claim 2, wherein: The preparation of the silane coupling agent solution comprises the following steps: dissolving the silane coupling agent in an alcohol-water mixture, adjusting the pH value to 2-4, and stirring for 1-1.5 hours; The mass ratio of alcohol to water in the alcohol-water mixture is 9:1; the silane coupling agent includes one or both of silane coupling agent KH-570 and silane coupling agent KH-550.

4. The method for forming a polymer-based composite material according to claim 2, wherein: The temperature rise curve of the drying treatment is: heating from room temperature to 60-70° C., keeping warm for 1-2 hours; heating from 60-70° C. to 120-130° C., keeping warm for 1.5-2 hours.

5. The method for forming a polymer-based composite material according to claim 1, wherein: In step S1, the frame substrate is a frame substrate having a porous structure; the frame substrate includes one of a rigid organic frame substrate, a ceramic frame substrate or a glass fiber frame substrate.

6. The method for forming a polymer-based composite material according to claim 1, wherein: In step S3, the curing device includes one of a heat curing device, a cold curing device or a light curing device.

7. The method for forming a polymer-based composite material according to claim 1, wherein: In step S3, the curing device is a heat curing device, and the heat curing device is a water bath heating device; step S3 also includes simultaneously applying pulsed ultrasound to the water bath heating device; The ultrasonic frequency is 40-80 Hz, the ultrasonic on time is 1-2 minutes, and the ultrasonic intermittent time is 5-10 minutes.

8. The method for forming a polymer-based composite material according to claim 1, wherein: After step S3, the obtained polymer-based composite material is subjected to directional annealing treatment, which includes the steps of drying the polymer-based composite material at 85-95°C for 2-2.5 hours, and then placing the polymer-based composite material still in a high-temperature state on a metal plate at room temperature.

9. The method for forming a polymer-based composite material according to claim 1, wherein: The frame substrate is a frame substrate with a through-hole structure.

10. A molding device, characterized in that: Used in the molding method of the polymer-based composite material according to any one of claims 1 to 9; the molding device includes a molding die and a lifting platform for driving the molding die to move.

Citation Information

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