Thermal protection material based on nano-rare earth doping modification and preparation method thereof

CN119858380BActive Publication Date: 2026-09-18NANTONG INST OF TECH +1
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Patent Information

Application Number
CN202510051806.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-01-13
Publication Date
2026-09-18
Estimated Expiration
2045-01-13

AI Technical Summary

Technical Problem

但由于玻璃纤维脆性较大,服用性能较差,因此,本课题以服用性能较好的芳纶织物替代玻纤织物,将其与铝箔复合作为热防护材料,提升热防护复合材料整体的舒适性能

Benefits of technology

[0021] By adding nano-rare earth powder to organosilicon resin and manually stirring to obtain a uniform solution, the solution is then stirred with a magnetic stirrer at room temperature until it is homogeneous and free of particles, thus obtaining a highly dispersed nano-rare earth thermal insulation resin. This resin is then treated with plasma etching on aluminum foil. Next, a coating machine is used to coat one side of the aluminum foil fabric, which is then adhered to the aluminum foil. A pressure roller is used to press the aramid fabric and aluminum foil together to form an intermediate material. This intermediate material is then placed in an oven for heating and curing, ultimately yielding a nano-rare earth-doped modified thermal protection material. This improves the adhesive strength of the aramid aluminum foil composite material, thereby increasing its thermal protection coefficient.

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Abstract

A thermal protection material based on rare earth doping modification and its preparation method are disclosed, belonging to the technical field of thermal protection materials. The method involves adding rare earth powder to an organosilicon resin, manually stirring to obtain a homogeneous solution, and then stirring the solution at room temperature using a magnetic stirrer until the solution is homogeneous and free of particles, thus obtaining a highly dispersed rare earth thermal insulation resin. The resin is then treated with plasma etching on an aluminum foil. Next, a coating machine is used to coat one side of the aluminum foil fabric, and the same side of the fabric is adhered to the aluminum foil. A pressure roller is used to flatten and press the aramid fabric and aluminum foil together to form an intermediate material. This intermediate material is then placed in an oven for heating and curing, ultimately yielding the rare earth doped thermal protection material. This improves the adhesive strength of the aramid aluminum foil composite material, thereby increasing its thermal protection coefficient.
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Description

Technical Field

[0001] This invention belongs to the field of thermal protection materials technology, specifically relating to a thermal protection material based on nano-rare earth doping modification and its preparation method. Background Technology

[0002] As mentioned in the prior art of patent application CN201210293207.3, aluminum foil-glass fiber fabric composite thermal protection materials have a wide range of applications. However, these materials, which use glass fiber fabric as the base and aluminum foil as the surface composite, possess excellent thermal protection properties. However, due to the high brittleness and poor wearability of glass fiber, this project uses aramid fabric, which has better wearability, to replace glass fiber fabric and composite it with aluminum foil as a thermal protection material, thereby improving the overall comfort performance of the composite material. However, because the surface of aluminum foil is too smooth, the bonding strength between aramid and aluminum foil is low, resulting in a reduced thermal protection coefficient. Therefore, modification is needed to improve the bonding strength of the aramid-aluminum foil composite material to increase the thermal protection coefficient. Summary of the Invention

[0003] To address the shortcomings of existing technologies, this invention proposes a thermal protection material based on nano-rare earth doping modification and its preparation method, which improves the adhesive strength of aramid aluminum foil composite materials, thereby enhancing the thermal protection coefficient.

[0004] The present invention employs the following technical solution.

[0005] A method for preparing a thermal protection material based on rare earth doping modification includes:

[0006] Step 1: Add nano-rare earth powder to the organosilicon resin, stir manually to obtain a mixed solution, and then stir the mixed solution with a magnetic stirrer at room temperature until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano-rare earth heat insulation resin.

[0007] Step 2: Treat the aluminum foil using plasma etching.

[0008] Step 3: Next, use a coating machine to scrape the prepared highly dispersed nano-rare earth heat insulation resin onto one side of the aluminum foil fabric, then attach the same side of the aluminum foil fabric to the aluminum foil, and press the aramid fabric and aluminum foil together with a pressure roller to form an intermediate material.

[0009] Step 4: Place the intermediate material in an oven for heating and curing to finally obtain a nano-rare earth doped and modified thermal protection material.

[0010] Furthermore, the amount of organosilicon resin is 100-200g, and the amount of nano-rare earth powder is 0-20g.

[0011] Furthermore, the mixture was stirred for 30 minutes at a speed of 120 r / min using a magnetic stirrer.

[0012] Furthermore, the aluminum foil weighs 1000–2000g.

[0013] Furthermore, the plasma etching parameters are: processing time of 100–500 s and working power of 100–500 W.

[0014] Furthermore, the distance between the nozzle used in the plasma etching process and the aluminum foil is 1–5 mm.

[0015] Furthermore, the aluminum foil fabric is an aramid fabric, and the aramid fabric weighs 1000-2000g.

[0016] Furthermore, the speed of the pressure roller is 0.8 to 1.2 m / min, and the pressure of the pressure roller is 60 to 120 N.

[0017] Furthermore, the drying temperature for heating and curing in an oven is 80–130°C, and the drying time is 30–60 minutes.

[0018] A thermal protection material based on nano-rare earth doping modification includes:

[0019] The thermal protection material based on rare earth doping modification is prepared according to the preparation method of the thermal protection material based on rare earth doping modification.

[0020] The beneficial effects of the present invention are as follows: Compared with the prior art, the technical effects of the present invention include:

[0021] By adding nano-rare earth powder to organosilicon resin and manually stirring to obtain a uniform solution, the solution is then stirred with a magnetic stirrer at room temperature until it is homogeneous and free of particles, thus obtaining a highly dispersed nano-rare earth thermal insulation resin. This resin is then treated with plasma etching on aluminum foil. Next, a coating machine is used to coat one side of the aluminum foil fabric, which is then adhered to the aluminum foil. A pressure roller is used to press the aramid fabric and aluminum foil together to form an intermediate material. This intermediate material is then placed in an oven for heating and curing, ultimately yielding a nano-rare earth-doped modified thermal protection material. This improves the adhesive strength of the aramid aluminum foil composite material, thereby increasing its thermal protection coefficient. Attached Figure Description

[0022] Figure 1 This is a flowchart of the preparation method of the thermal protection material based on nano-rare earth doping modification in this invention;

[0023] Figure 2This is a schematic diagram illustrating the principle and process of the preparation method of the thermal protection material based on nano-rare earth doping modification in this invention;

[0024] Figure 3 These are SEM images of aluminum foils that have not undergone plasma etching and those that have undergone plasma etching in this invention: Figure 3 (a) is a SEM image of the aluminum foil before plasma etching. Figure 3 (b) is a SEM image of the aluminum foil after plasma etching. Detailed Implementation

[0025] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below in conjunction with the accompanying drawings of the embodiments of this invention. The embodiments described in this application are merely some embodiments of this invention, and not all embodiments. Based on the spirit of this invention, other embodiments obtained by those skilled in the art without creative effort are all within the protection scope of this invention.

[0026] like Figure 1 and Figure 2 As shown, the preparation method of a thermal protection material based on nano-rare earth doping modification according to the present invention includes:

[0027] Generally, material surfaces can be modified through methods such as acid and alkali corrosion, flame burning, mechanical micro-pitting, and plasma treatment. Among these methods, plasma treatment is the only one that does not damage the material's surface structure, and when a suitable gas atmosphere is selected, no waste gas or environmental pollution is generated. Plasma is generally defined as an electrically neutral ionized gas (composed of electrons, ions, metastable states, and LV radiation) on a macroscopic scale. These substances can alter the physical or chemical properties of the material surface depending on the material composition and plasma treatment conditions. The physical or chemical changes on the material surface after plasma treatment depend on the plasma treatment conditions, such as treatment time, power, and plasma treatment gas atmosphere. Plasma modification is a technique for treating material surfaces. On one hand, plasma induces the formation of groups in polymers, which are then subjected to cleavage, oxidation, etc., subsequently forming active groups on the surface of the treated material. On the other hand, plasma can also etch the material to roughen it, forming grooves or very tight cross-linked layers on the surface. The specific preparation method of thermal protection materials based on nano-rare earth doping modification is as follows:

[0028] Step 1: Add nano-rare earth powder to the organosilicon resin, stir manually to obtain a mixed solution, and then stir the mixed solution with a magnetic stirrer at room temperature until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano-rare earth heat insulation resin.

[0029] In a preferred but non-limiting embodiment of the present invention, the amount of organosilicon resin is 100-200g and the amount of nano-rare earth powder is 0-20g.

[0030] In a preferred but non-limiting embodiment of the present invention, the magnetic stirrer is used to stir for 30 minutes at a speed of 120 r / min.

[0031] Step 2: Treat the aluminum foil using plasma etching.

[0032] In a preferred but non-limiting embodiment of the present invention, the aluminum foil weighs 1000–2000g.

[0033] In a preferred but non-limiting embodiment of the present invention, the plasma etching processing parameters are: processing time of 100-500s and working power of 100-500w.

[0034] In a preferred but non-limiting embodiment of the present invention, the distance between the nozzle used in the plasma etching process and the aluminum foil is 1 to 5 mm.

[0035] Step 3: Next, use a coating machine to coat the highly dispersed nano-rare earth heat insulation resin prepared above onto one side of the aluminum foil fabric, then attach the same side of the aluminum foil fabric to the aluminum foil, and press the aramid fabric and aluminum foil together with a pressure roller to form an intermediate material.

[0036] In a preferred but non-limiting embodiment of the present invention, the aluminum foil fabric is an aramid fabric, and the aramid fabric weighs 1000-2000g.

[0037] In a preferred but non-limiting embodiment of the present invention, the speed of the pressure roller is 0.8 to 1.2 m / min, and the pressure of the pressure roller is 60 to 120 N.

[0038] Step 4: Place the above intermediate materials into an oven for heating and curing to finally obtain a nano-rare earth doped and modified thermal protection material.

[0039] In a preferred but non-limiting embodiment of the present invention, the drying temperature for heating and curing in an oven is 80–130°C, and the drying time is 30–60 minutes.

[0040] The present invention discloses a thermal protection material based on nano-rare earth doping modification, comprising:

[0041] The thermal protection material based on rare earth doping modification is prepared according to the preparation method of the thermal protection material based on rare earth doping modification.

[0042] The beneficial effects of the present invention are as follows: Compared with the prior art, the technical effects of the present invention include:

[0043] By adding nano-rare earth powder to organosilicon resin and manually stirring to obtain a uniform solution, the solution is then stirred with a magnetic stirrer at room temperature until it is homogeneous and free of particles, thus obtaining a highly dispersed nano-rare earth thermal insulation resin. This resin is then treated with plasma etching on aluminum foil. Next, a coating machine is used to coat one side of the aluminum foil fabric, which is then adhered to the aluminum foil. A pressure roller is used to press the aramid fabric and aluminum foil together to form an intermediate material. This intermediate material is then placed in an oven for heating and curing, ultimately yielding a nano-rare earth-doped modified thermal protection material. This improves the adhesive strength of the aramid aluminum foil composite material, thereby increasing its thermal protection coefficient.

[0044] Experiments on the preparation method of thermal protection materials based on nano-rare earth doping modification have shown that... Figure 3 (a) is a SEM image of the aluminum foil before plasma etching. Figure 3 (b) is a SEM image of the aluminum foil after plasma etching. The processing parameters were: plasma treatment time of 300s, processing power of 300W, and distance from the plasma nozzle to the aluminum foil of 2.5mm. Figure 3 As can be seen, the surface of the untreated aluminum foil is smooth and without etching marks, while the surface of the aluminum foil treated with plasma has a large number of micron-sized grooves, which increases its specific surface area and thus increases the contact area with the adhesive, making it more conducive to the bonding between the aluminum foil and the adhesive. This improves the bonding strength of the aramid aluminum foil composite material and thus improves the thermal protection coefficient.

[0045] The following specific embodiments further illustrate the present invention:

[0046] Example 1:

[0047] The preparation method of thermal protection materials based on nano-rare earth doping modification includes:

[0048] Step 1: Add nano-rare earth powder to the organosilicon resin, stir manually to obtain a mixed solution, and then stir the mixed solution with a magnetic stirrer at room temperature until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano-rare earth heat insulation resin.

[0049] The amount of organosilicon resin is 100g, and the amount of nano-rare earth powder is 1g.

[0050] Stir with a magnetic stirrer for 30 minutes at a speed of 120 r / min.

[0051] Step 2: Treat the aluminum foil using plasma etching.

[0052] The aluminum foil weighs 1000g.

[0053] The plasma etching parameters are: processing time of 100s and working power of 500w.

[0054] The distance between the nozzle and the aluminum foil used in plasma etching is mm.

[0055] Step 3: Next, use a coating machine to coat the highly dispersed nano-rare earth heat insulation resin prepared above onto one side of the aluminum foil fabric, then attach the same side of the aluminum foil fabric to the aluminum foil, and press the aramid fabric and aluminum foil together with a pressure roller to form an intermediate material.

[0056] The aluminum foil fabric is an aramid fabric, and the aramid fabric weighs 1000g.

[0057] The roller speed is 0.8 m / min and the roller pressure is 6 N.

[0058] Step 4: Place the above intermediate materials into an oven for heating and curing to finally obtain a nano-rare earth doped and modified thermal protection material.

[0059] The drying temperature for curing in an oven is 80℃, and the drying time is 30 minutes.

[0060] Thermal protection materials based on rare earth doping modification include:

[0061] The thermal protection material based on rare earth doping modification is prepared according to the preparation method of the thermal protection material based on rare earth doping modification described in this embodiment.

[0062] Example 2:

[0063] The preparation method of thermal protection materials based on nano-rare earth doping modification includes:

[0064] Step 1: Add nano-rare earth powder to the organosilicon resin, stir manually to obtain a mixed solution, and then stir the mixed solution with a magnetic stirrer at room temperature until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano-rare earth heat insulation resin.

[0065] The amount of organosilicon resin is 150g, and the amount of nano-rare earth powder is 10g.

[0066] Stir with a magnetic stirrer for 30 minutes at a speed of 120 r / min.

[0067] Step 2: Treat the aluminum foil using plasma etching.

[0068] The aluminum foil weighs 1500g.

[0069] The plasma etching parameters are: processing time of 300s and working power of 300w.

[0070] The distance between the nozzle and the aluminum foil used in plasma etching is 3 mm.

[0071] Step 3: Next, use a coating machine to coat the highly dispersed nano-rare earth heat insulation resin prepared above onto one side of the aluminum foil fabric, then attach the same side of the aluminum foil fabric to the aluminum foil, and press the aramid fabric and aluminum foil together with a pressure roller to form an intermediate material.

[0072] The aluminum foil fabric is an aramid fabric, and the aramid fabric weighs 1500g.

[0073] The roller speed is 1.0 m / min and the roller pressure is 90 N.

[0074] Step 4: Place the above intermediate materials into an oven for heating and curing to finally obtain a nano-rare earth doped and modified thermal protection material.

[0075] The drying temperature for curing in an oven is 105℃, and the drying time is 45 minutes.

[0076] Thermal protection materials based on rare earth doping modification include:

[0077] The thermal protection material based on rare earth doping modification is prepared according to the preparation method of the thermal protection material based on rare earth doping modification described in this embodiment.

[0078] Example 3:

[0079] The preparation method of thermal protection materials based on nano-rare earth doping modification includes:

[0080] Step 1: Add nano-rare earth powder to the organosilicon resin, stir manually to obtain a mixed solution, and then stir the mixed solution with a magnetic stirrer at room temperature until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano-rare earth heat insulation resin.

[0081] The amount of organosilicon resin is 200g, and the amount of nano-rare earth powder is 20g.

[0082] Stir with a magnetic stirrer for 30 minutes at a speed of 120 r / min.

[0083] Step 2: Treat the aluminum foil using plasma etching.

[0084] The aluminum foil weighs 2000g.

[0085] The plasma etching parameters are: processing time of 500s and working power of 500w.

[0086] The distance between the nozzle and the aluminum foil used in the plasma etching process is 5 mm.

[0087] Step 3: Next, use a coating machine to coat the highly dispersed nano-rare earth heat insulation resin prepared above onto one side of the aluminum foil fabric, then attach the same side of the aluminum foil fabric to the aluminum foil, and press the aramid fabric and aluminum foil together with a pressure roller to form an intermediate material.

[0088] The aluminum foil fabric is an aramid fabric, and the aramid fabric weighs 2000g.

[0089] The roller speed is 1.2 m / min and the roller pressure is 120 N.

[0090] Step 4: Place the above intermediate materials into an oven for heating and curing to finally obtain a nano-rare earth doped and modified thermal protection material.

[0091] The drying temperature for curing in an oven is 130℃, and the drying time is 60 minutes.

[0092] Thermal protection materials based on rare earth doping modification include:

[0093] The thermal protection material based on rare earth doping modification is prepared according to the preparation method of the thermal protection material based on rare earth doping modification described in this embodiment.

[0094] Subsequently, three nano-rare earth thermal protection composite materials that had not undergone plasma etching treatment were obtained using existing techniques as corresponding control groups, namely control group 1, control group 2, and control group 3. The thermal protection coefficients of the nano-rare earth thermal protection composite materials from Examples 1, 2, and 3 were then tested, and the results are shown in Table 1.

[0095] Table 1

[0096]

[0097] Table 1 shows the thermal protection performance of nano-rare earth thermal protection composite materials without plasma treatment and after plasma treatment, with the rare earth addition amount being 10g in both cases.

[0098] Table 1 shows that the thermal protection coefficients of the untreated nano-rare earth thermal protective composite materials are 443.76 kW·s / m², 446.29 kW·s / m², and 445.73 kW·s / m², respectively, while those of the plasma-treated nano-rare earth thermal protective composite materials are 508.65 kW·s / m², 511.29 kW·s / m², and 516.52 kW·s / m². As can be seen from Table 1, the thermal protection performance of the plasma-treated nano-rare earth thermal protective composite materials is significantly greater than that of the untreated ones. This is because plasma treatment creates numerous grooves on the surface of the aluminum foil, resulting in a stronger bond between the adhesive and the aluminum foil. It also enhances the mechanical interlocking force at the interfaces, making the overall bonding of the aluminum foil aramid composite material more compact. Therefore, compared to the untreated aluminum foil aramid composite material, the thermal protection performance of the plasma-treated aluminum foil aramid composite material is significantly greater.

[0099] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of the present invention without departing from the spirit and scope of the present invention. Any modifications or equivalent substitutions should be covered within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing a thermal protection material based on nano-rare earth doping modification, characterized in that, include: Step 1: Add nano-rare earth powder to the organosilicon resin, stir manually to obtain a mixed solution, and then stir the mixed solution with a magnetic stirrer at room temperature until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano-rare earth heat insulation resin. Step 2: Treat the aluminum foil using plasma etching. Step 3: Next, use a coating machine to coat the prepared highly dispersed nano-rare earth heat insulation resin onto one side of the aramid fabric, then attach the same side of the aramid fabric to the aluminum foil, and press the aramid fabric and aluminum foil together with a pressure roller to form an intermediate material. Step 4: Place the intermediate material back into the oven for heating and curing to finally obtain the nano-rare earth doped and modified thermal protection material; In step 1, the amount of organosilicon resin is 100~200g and the amount of nano-rare earth powder is 1~20g; Stir with a magnetic stirrer for 30 minutes at a speed of 120 r / min; The plasma etching parameters are: processing time of 100~500 s and working power of 100~500w; The distance between the nozzle and the aluminum foil used in plasma etching is 1~5 mm.

2. The method for preparing the thermal protection material based on nano-rare earth doping modification according to claim 1, characterized in that, The speed of the pressure roller is 0.8~1.2m / min, and the pressure of the pressure roller is 60~120N.

3. The method for preparing the thermal protection material based on nano-rare earth doping modification according to claim 2, characterized in that, The drying temperature for curing in an oven is 80~130℃, and the drying time is 30~60 minutes.

4. A thermal protection material based on nano-rare earth doping modification, characterized in that, include: The thermal protection material based on rare earth doping modification prepared according to any one of claims 1 to 3.

Citation Information

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