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

Abstract

The invention relates to a thermal protection material based on nano rare earth doping modification and a preparation method thereof, and belongs to the technical field of thermal protection materials.The preparation method comprises the steps that nano rare earth powder is added into organic silicon resin and manually stirred to be uniform, a mixed solution is obtained, then the mixed solution is stirred through a magnetic stirrer at the room temperature till the mixed solution is uniform and free of particles, and the thermal protection material is obtained; treating an aluminum foil by using a plasma etching treatment method, so as to obtain the high-dispersity nano rare-earth heat-insulating resin; then blade-coating one surface of an aluminum foil fabric with the prepared high-dispersity nano rare earth heat-insulating resin by using a coating machine, adhering the surface of the aluminum foil fabric to an aluminum foil, flatly pressing the aramid fabric and the aluminum foil by using a compression roller, and bonding to form an intermediate material; putting the intermediate material into a drying oven, heating and curing to finally obtain the nano rare earth doped and modified thermal protection material, so that the bonding strength of the aramid fiber aluminum foil composite material is improved, and the thermal protection coefficient is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of thermal protection materials, and in particular relates to a thermal protection material based on nano rare earth doping modification and a preparation method thereof. Background Art

[0002] As mentioned in the prior art of patent application number CN201210293207.3, the aluminum foil glass fiber fabric composite thermal protection material has a wide range of uses. On the other hand, the aluminum foil glass fiber fabric composite thermal protection material is a thermal protection material with glass fiber fabric as the base fabric and aluminum foil composited on the surface, and has excellent thermal protection performance. However, due to the large brittleness of glass fiber and poor wearability, this project replaces glass fiber fabric with aramid fabric with better wearability, and composites it with aluminum foil as a thermal protection material to improve the overall comfort performance of the thermal protection composite material. However, since the surface of the aluminum foil is too smooth, there is a problem of low bonding strength when composited with aramid and aluminum foil, which reduces the thermal protection coefficient. Therefore, it is necessary to modify it, so as to improve the bonding strength of the aramid aluminum foil composite material to improve the thermal protection coefficient. Summary of the invention

[0003] In order to address the defects in the prior art, the present invention proposes a thermal protection material based on nano rare earth doping modification and a preparation method thereof, which improves the bonding strength of the aramid aluminum foil composite material to improve the thermal protection coefficient.

[0004] The present invention utilizes the following technical solutions.

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

[0006] Step 1: Add nano rare earth powder to the silicone resin, stir it 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 thermal insulation resin;

[0007] Step 2: treating the aluminum foil using a plasma etching method;

[0008] Step 3: Then use a coating machine to scrape the prepared high-dispersion nano rare earth thermal insulation resin onto one side of the aluminum foil fabric, and then adhere the side of the aluminum foil fabric to the aluminum foil, and use a pressure roller to flatten and press the aramid fabric and the aluminum foil together to form an intermediate material;

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

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

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

[0012] Furthermore, the aluminum foil is 1000-2000g.

[0013] Furthermore, the plasma etching processing parameters are: processing time is 100 to 500 seconds, and working power is 100 to 500W.

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

[0015] Furthermore, the aluminum foil fabric is an aramid fabric, and the aramid fabric has a weight of 1000 to 2000 g.

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

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

[0018] A thermal protection material based on nano rare earth doping modification, comprising:

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

[0020] The beneficial effects of the present invention are that, compared with the prior art, the technical effects of the present invention include:

[0021] Nano rare earth powder is added to silicone resin, and the mixture is stirred manually to obtain a mixed solution. The mixed solution is then stirred at room temperature by a magnetic stirrer until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano rare earth thermal insulation resin, and the aluminum foil is treated by a plasma etching method; then a coating machine is used to scrape the prepared highly dispersed nano rare earth thermal insulation resin onto one side of the aluminum foil fabric, and then the side of the aluminum foil fabric is adhered to the aluminum foil, and the aramid fabric and the aluminum foil are flattened and pressed together by a pressing roller to form an intermediate material; the intermediate material is then placed in an oven for heating and curing, and finally a nano rare earth doped and modified thermal protection material is obtained, thereby improving the bonding strength of the aramid aluminum foil composite material to improve the thermal protection coefficient. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a flow chart of the preparation method of the thermal protection material based on nano rare earth doping modification in the present invention;

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

[0024] Figure 3 The SEM images of the aluminum foils that have not been treated with plasma etching and those that have been treated with plasma etching in the present invention are as follows: Figure 3 (a) is the SEM image of aluminum foil that has not been treated by plasma etching. Figure 3 (b) is the SEM image of aluminum foil after plasma etching. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solution and advantages of the present invention clearer, the following will be combined with the drawings in the embodiments of the present invention to clearly and completely express the technical solution of the present invention. The embodiments expressed in this application are only some embodiments of the present invention, not all embodiments. According to the spirit of the present invention, other embodiments obtained by ordinary technicians in this field without creative work are all within the protection scope of the present invention.

[0026] like Figure 1 and Figure 2 As shown, the method for preparing a thermal protection material based on nano rare earth doping modification described in the present invention comprises:

[0027] Generally, the surface of materials can be modified by methods such as acid and alkali corrosion, flame burning, mechanical micro-pitting and plasma treatment. Among these methods, plasma treatment is the only method that will not damage the surface structure of the material, and the selection of a suitable gas atmosphere to treat the material will not produce any waste gas and environmental pollution. Plasma is usually defined as an ionized gas (composed of electrons, ions, metastable states and LV radiation) that is electrically neutral on a macroscopic scale. These substances will change the physical or chemical properties of the material surface according to the material composition and plasma treatment conditions. The physical or chemical changes on the surface of the material after plasma treatment depend on the plasma treatment conditions, such as treatment time, power, plasma treatment gas atmosphere, etc. Plasma modification is a technology for treating the surface of a material. On the one hand, plasma induces the formation of polymer groups, which are then cracked, oxidized, etc., and then active groups are formed on the surface of the treated material. On the other hand, plasma can also etch the material to make it rough, form grooves on the surface or form a very tight cross-linked layer. The 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 silicone resin, stir it 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 thermal insulation resin;

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

[0030] In a preferred but non-limiting embodiment of the present invention, the magnetic stirrer stirs for 30 minutes and its rotation speed is 120 r / min.

[0031] Step 2: treating the aluminum foil using a plasma etching method;

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

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

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

[0035] Step 3: Then, use a coating machine to scrape the highly dispersed nano rare earth thermal insulation resin prepared above onto one side of the aluminum foil fabric, and then adhere the side of the aluminum foil fabric onto the aluminum foil, and use a pressure roller to flatten and press the aramid fabric and the aluminum foil together 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 roller speed is 0.8-1.2 m / min, and the roller pressure is 60-120 N.

[0038] Step 4: Place the intermediate material in an oven for heating and curing, and 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 curing in an oven is 80 to 130° C., and the drying time is 30 to 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 nano rare earth doping modification is prepared according to the preparation method of the thermal protection material based on nano rare earth doping modification.

[0042] The beneficial effects of the present invention are that, compared with the prior art, the technical effects of the present invention include:

[0043] Nano rare earth powder is added to silicone resin, and the mixture is stirred manually to obtain a mixed solution. The mixed solution is then stirred at room temperature by a magnetic stirrer until the mixed solution is uniform and free of particles, thereby obtaining a highly dispersed nano rare earth thermal insulation resin, and the aluminum foil is treated by a plasma etching method; then a coating machine is used to scrape the prepared highly dispersed nano rare earth thermal insulation resin onto one side of the aluminum foil fabric, and then the side of the aluminum foil fabric is adhered to the aluminum foil, and the aramid fabric and the aluminum foil are flattened and pressed together by a pressing roller to form an intermediate material; the intermediate material is then placed in an oven for heating and curing, and finally a nano rare earth doped and modified thermal protection material is obtained, thereby improving the bonding strength of the aramid aluminum foil composite material to improve the thermal protection coefficient.

[0044] Through the test of the preparation method of thermal protection material based on nano rare earth doping modification, it can be found that Figure 3 (a) is the SEM image of aluminum foil that has not been treated by plasma etching. Figure 3 (b) is a SEM image of aluminum foil after plasma etching. The processing parameters are: plasma treatment time is 300s, treatment power is 300W, and the distance from the plasma nozzle to the aluminum foil is 2.5mm. Figure 3 It can be seen that the surface of the aluminum foil without plasma treatment is smooth and has no traces of etching, while the surface of the aluminum foil after plasma treatment produces a large number of micron-sized grooves, and its specific surface area increases, which also increases the contact area with the adhesive, which is more conducive to the bonding between the aluminum foil and the adhesive, thereby improving the bonding strength of the aramid aluminum foil composite material and improving the thermal protection coefficient.

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

[0046] Embodiment 1:

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

[0048] Step 1: Add nano rare earth powder to the silicone resin, stir it 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 thermal insulation resin;

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

[0050] The magnetic stirrer was stirred for 30 min at a speed of 120 r / min.

[0051] Step 2: treating the aluminum foil using a plasma etching method;

[0052] Aluminum foil is 1000g.

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

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

[0055] Step 3: Then, use a coating machine to scrape the highly dispersed nano rare earth thermal insulation resin prepared above onto one side of the aluminum foil fabric, and then adhere the side of the aluminum foil fabric onto the aluminum foil, and use a pressure roller to flatten and press the aramid fabric and the aluminum foil together to form an intermediate material;

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

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

[0058] Step 4: Place the intermediate material in an oven for heating and curing, and finally obtain a nano rare earth doped and modified thermal protection material.

[0059] The drying temperature for heating and curing in an oven is 80°C and the drying time is 30 minutes.

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

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

[0062] Embodiment 2:

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

[0064] Step 1: Add nano rare earth powder to the silicone resin, stir it 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 thermal insulation resin;

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

[0066] The magnetic stirrer was stirred for 30 min at a speed of 120 r / min.

[0067] Step 2: treating the aluminum foil using a plasma etching method;

[0068] The aluminum foil is 1500g.

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

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

[0071] Step 3: Then, use a coating machine to scrape the highly dispersed nano rare earth thermal insulation resin prepared above onto one side of the aluminum foil fabric, and then adhere the side of the aluminum foil fabric onto the aluminum foil, and use a pressure roller to flatten and press the aramid fabric and the aluminum foil together to form an intermediate material;

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

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

[0074] Step 4: Place the intermediate material in an oven for heating and curing, and finally obtain a nano rare earth doped and modified thermal protection material.

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

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

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

[0078] Embodiment 3:

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

[0080] Step 1: Add nano rare earth powder to the silicone resin, stir it 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 thermal insulation resin;

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

[0082] The magnetic stirrer was stirred for 30 min at a speed of 120 r / min.

[0083] Step 2: treating the aluminum foil using a plasma etching method;

[0084] The aluminum foil is 2000g.

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

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

[0087] Step 3: Then, use a coating machine to scrape the highly dispersed nano rare earth thermal insulation resin prepared above onto one side of the aluminum foil fabric, and then adhere the side of the aluminum foil fabric onto the aluminum foil, and use a pressure roller to flatten and press the aramid fabric and the aluminum foil together to form an intermediate material;

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

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

[0090] Step 4: Place the intermediate material in an oven for heating and curing, and finally obtain a nano rare earth doped and modified thermal protection material.

[0091] The drying temperature for heating and curing in an oven is 130°C and the drying time is 60 minutes.

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

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

[0094] Subsequently, three nano rare earth thermal protection composite materials that have not been treated by plasma etching were obtained by the method of the prior art 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 of Example 1, Example 2 and Example 3 were tested, and the results are shown in Table 1:

[0095] Table 1

[0096]

[0097] Table 1 shows the thermal protection properties of nano rare earth thermal protection composite materials without plasma treatment and after plasma treatment, where the rare earth addition amount is 10g.

[0098] It can be found from Table 1 that the thermal protection coefficients of the nano rare earth thermal protection composite materials without plasma treatment are 443.76kw·s / m2, 446.29kw·s / m2, and 445.73kw·s / m2, respectively, while the thermal protection coefficients of the nano rare earth thermal protection composite materials treated with plasma are 508.65kw·s / m2, 511.29kw·s / m2, and 516.52kw·s / m. It can be seen from Table 1 that the thermal protection performance of the nano rare earth thermal protection composite materials treated with plasma is significantly greater than that of the untreated ones. The reason is that after the aluminum foil is treated with plasma, a large number of grooves are formed on the surface, and the adhesive and the aluminum foil are more firmly bonded. At the same time, the mechanical bite force between the interfaces is also enhanced, making the aluminum foil aramid composite materials more densely bonded as a whole. Therefore, compared with the untreated aluminum foil aramid composite materials, the thermal protection performance of the aluminum foil aramid composite materials treated with plasma is significantly greater than the former.

[0099] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the present invention can still be modified or replaced by equivalents, and any modifications or equivalent replacements that do not depart from the spirit and scope of the present invention 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 silicone resin, stir it 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 thermal insulation resin; Step 2: treating the aluminum foil using a plasma etching method; Step 3: Then use a coating machine to scrape the prepared high-dispersion nano rare earth thermal insulation resin onto one side of the aluminum foil fabric, and then adhere the side of the aluminum foil fabric to the aluminum foil, and use a pressure roller to flatten and press the aramid fabric and the aluminum foil together to form an intermediate material; Step 4: Place the intermediate material in an oven for heating and curing, and finally obtain a nano rare earth doped and modified thermal protection material.

2. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 1, characterized in that: The organic silicon resin is 100-200g, and the nano rare earth powder is 0-20g.

3. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 1, characterized in that: The magnetic stirrer was stirred for 30 min at a speed of 120 r / min.

4. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 1, characterized in that: The weight of the aluminum foil is 1000 to 2000 g.

5. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 1, characterized in that: The plasma etching processing parameters are: processing time is 100 to 500 seconds, and working power is 100 to 500W.

6. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 5, characterized in that: The distance between the nozzle used for plasma etching and the aluminum foil is 1 to 5 mm.

7. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 6, characterized in that: The aluminum foil fabric is an aramid fabric, and the aramid fabric is 1000-2000g.

8. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 7, characterized in that: The pressure roller speed is 0.8-1.2 m / min, and the pressure roller pressure is 60-120 N.

9. The method for preparing a thermal protection material based on nano rare earth doping modification according to claim 8, characterized in that: The drying temperature for heating and curing in an oven is 80 to 130° C., and the drying time is 30 to 60 minutes.

10. A thermal protection material based on nano rare earth doping modification, characterized in that: include: A thermal protection material based on nano rare earth doping modification prepared by the preparation method of thermal protection material based on nano rare earth doping modification according to any one of claims 1 to 9.

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