Preparation method of phosphate reinforced quartz heat insulation tile composite material

Abstract

The invention discloses a preparation method of a phosphate reinforced quartz heat insulation tile composite material, and relates to the field of composite material preparation. The technical problem that a rigid ceramic fiber heat insulation tile is low in strength is solved. The method comprises the following steps: 1, preparing an aluminum dihydrogen phosphate resin solution; 2, preparing the modified heat insulation tile; and 3, dipping in ammonia water to prepare the phosphate reinforced quartz heat insulation tile composite material, thereby completing the preparation. According to the prepared composite material, the excellent heat insulation property is maintained, meanwhile, the mechanical property is greatly improved, and the application range of the composite material in the high-temperature heat insulation field is widened. The phosphate reinforced quartz heat insulation tile composite material prepared by the invention is applied to the field of thermal protection systems.

Description

Technical Field

[0001] The present invention relates to the field of composite material preparation, and in particular to a method for preparing a high-temperature resistant inorganic adhesive reinforced quartz thermal insulation tile composite material. Background Art

[0002] With the increasing frequency of space applications and exploration activities, reusable transportation systems have become an urgent need for space transportation missions of major military powers. Thermal protection materials, as the cornerstone for the development and protection of reusable transportation systems in extreme environments, are the core components for solving the problem of aerodynamic heating thermal barriers. Rigid ceramic fiber insulation tiles are one of the main materials for reusable thermal protection systems, with high temperature resistance, lightweight, and heat insulation properties. However, this material has the system defects of high porosity, low strength, and hard and brittle material. How to achieve a balance between low thermal conductivity and high strength remains the main challenge facing quartz fiber porous ceramics. Summary of the Invention

[0003] In order to solve the technical problem of low strength of rigid ceramic fiber insulation tiles, the present invention provides a preparation method of an inorganic phosphate reinforced quartz insulation tile composite material. This method is completely different from the traditional preparation method of changing raw materials and molding processes. It innovatively uses liquid phosphate resin as a film-forming agent and liquid ammonia water as a curing agent. Under normal temperature conditions, through a two-step impregnation process, an in-situ reaction is achieved on the surface of the quartz fiber skeleton to generate a coating, thereby preparing a high-strength phosphate reinforced quartz insulation tile composite material.

[0004] A method for preparing a phosphate-reinforced quartz thermal insulation tile composite material is specifically carried out according to the following steps:

[0005] 1. diluting aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution, then adding a silane coupling agent and a cosolvent, stirring, and obtaining an aluminum dihydrogen phosphate resin solution;

[0006] 2. Under vacuum conditions, the aluminum dihydrogen phosphate resin solution prepared in step 1 is used to impregnate the quartz insulation tile; then, the quartz insulation tile is dried to obtain the modified insulation tile;

[0007] 3. Under a vacuum environment, the modified thermal insulation tile obtained in step 2 is immersed in ammonia water, and then dried to obtain a phosphate reinforced quartz thermal insulation tile composite material, thereby completing the preparation.

[0008] Furthermore, the mass concentration of the aluminum dihydrogen phosphate solution after dilution in step 1 is 1-20%.

[0009] Furthermore, the silane coupling agent in step 1 is KH550.

[0010] Furthermore, the amount of the silane coupling agent added in step 1 is 1-2% of the mass of the aluminum dihydrogen phosphate solution.

[0011] Furthermore, the cosolvent in step 1 is a surfactant.

[0012] Furthermore, the amount of the additive added in step 1 is 0.05-0.5% of the mass of the aluminum dihydrogen phosphate solution.

[0013] Furthermore, in step 2, the immersion time is controlled to be 3 to 5 hours.

[0014] Furthermore, in step 2, the drying temperature is controlled to be 120-140°C.

[0015] Furthermore, in step three, the immersion time is controlled to be 3 to 5 hours.

[0016] Furthermore, the drying temperature is controlled to be 120~140℃.

[0017] The present invention prepares a high-strength, ultra-thin phosphate coating on the surface of the quartz fiber skeleton. The coating reacts with the fiber skeleton at an interface under high temperature, and has excellent high-temperature resistant mechanical properties.

[0018] Beneficial effects of the present invention:

[0019] The present invention adopts a coating-enhanced modification strategy, utilizing the porous structure of quartz insulation tiles to generate an in-situ phosphate coating on the surface of the quartz fiber skeleton through a secondary impregnation process. When the concentration of the Al(H2PO4)3 solution is 5 wt.%, the coating evenly covers the fiber surface with a thickness of about 4 to 10 nm ( Figure 3 There is no obvious lumps at the fiber nodes, and the thermal conductivity of the composite material remains at 0.09 W·m -1 ·K -1 , with excellent thermal insulation performance. As the concentration of aluminum dihydrogen phosphate solution increases, the room temperature and high temperature compressive strength of the composite material are significantly improved, which is about 7.9 times higher than that of the unmodified sample. The enhancement of mechanical properties is mainly attributed to the formation of phosphate coating and the synergistic effect of colloid at high concentration. At high temperature, the strong interface bonding between the coating and the fiber further improves the material performance. While maintaining excellent thermal insulation, the composite material has greatly improved the mechanical properties, expanding its application in the field of high-temperature thermal insulation.

[0020] The phosphate reinforced quartz thermal insulation tile composite material prepared by the invention is used in the field of thermal protection systems. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is the microscopic morphology of commercially available quartz insulation tiles;

[0022] Figure 2 The microstructure of the phosphate-reinforced quartz thermal insulation tile composite material prepared in Example 2;

[0023] Figure 3 for Figure 2 A partial enlarged view of . DETAILED DESCRIPTION

[0024] Specific embodiment 1: This embodiment is a method for preparing a phosphate reinforced quartz insulation tile composite material, which is specifically carried out in the following steps:

[0025] 1. diluting aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution, then adding a silane coupling agent and a cosolvent, stirring, and obtaining an aluminum dihydrogen phosphate resin solution;

[0026] 2. Under vacuum conditions, the aluminum dihydrogen phosphate resin solution prepared in step 1 is used to impregnate the quartz insulation tile; then, the quartz insulation tile is dried to obtain the modified insulation tile;

[0027] 3. Under a vacuum environment, the modified thermal insulation tile obtained in step 2 is immersed in ammonia water, and then dried to obtain a phosphate reinforced quartz thermal insulation tile composite material, thereby completing the preparation.

[0028] Specific embodiment 2: This embodiment differs from specific embodiment 1 in that the mass concentration of the aluminum dihydrogen phosphate solution after dilution in step 1 is 1-20%. Other aspects are the same as specific embodiment 1.

[0029] Specific embodiment 3: This embodiment differs from specific embodiment 1 or 2 in that the silane coupling agent in step 1 is KH550. Other aspects are the same as specific embodiment 1 or 2.

[0030] Specific embodiment 4: This embodiment differs from specific embodiments 1 to 3 in that the amount of the silane coupling agent added in step 1 is 1-2% of the mass of the aluminum dihydrogen phosphate solution. Other aspects are the same as specific embodiments 1 to 3.

[0031] Specific embodiment 5: This embodiment differs from specific embodiments 1 to 4 in that the cosolvent in step 1 is a surfactant. Other aspects are the same as specific embodiments 1 to 4.

[0032] Specific embodiment 6: This embodiment differs from specific embodiments 1 to 5 in that the amount of the additive added in step 1 is 0.05-0.5% of the mass of the aluminum dihydrogen phosphate solution. Other aspects are the same as specific embodiments 1 to 5.

[0033] Specific embodiment 7: This embodiment differs from specific embodiments 1 to 6 in that the immersion time in step 2 is controlled to be 3 to 5 hours. Other aspects are the same as specific embodiments 1 to 6.

[0034] Specific embodiment 8: This embodiment differs from specific embodiments 1 to 7 in that the drying temperature in step 2 is controlled to be 120-140° C. The rest is the same as specific embodiments 1 to 7.

[0035] Specific embodiment 9: This embodiment differs from specific embodiments 1 to 8 in that the immersion time in step 3 is controlled to be 3 to 5 hours. Other aspects are the same as specific embodiments 1 to 8.

[0036] Specific embodiment 10: This embodiment differs from specific embodiments 1 to 9 in that the drying temperature is controlled to be 120-140° C. The rest is the same as specific embodiments 1 to 9.

[0037] The content of the present invention is not limited to the content of the above-mentioned embodiments. The combination of one or more specific embodiments can also achieve the purpose of the invention.

[0038] Example 1:

[0039] This embodiment provides a method for preparing a phosphate-reinforced quartz thermal insulation tile composite material, which is specifically carried out by the following steps:

[0040] 1. Dilute aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution with a mass concentration of 1% (the dilution solvent is water), then add silane coupling agent KH550 dropwise, stir for 30 minutes, then add anionic polyacrylamide surfactant dropwise, stir for 30 minutes to obtain an aluminum dihydrogen phosphate resin solution; the amount of silane coupling agent added is 1% of the mass of the aluminum dihydrogen phosphate solution; the amount of surfactant added is 0.05% of the mass of the aluminum dihydrogen phosphate solution;

[0041] 2. Under vacuum and room temperature, the aluminum dihydrogen phosphate resin solution prepared in step 1 was used to impregnate the quartz insulation tile for 3 hours; then, the quartz insulation tile was dried in a 120°C oven to remove excess solvent, thereby obtaining a modified insulation tile;

[0042] 3. Under vacuum environment, immerse the modified insulation tile obtained in step 2 in 15% ammonia water for 3 hours, then dry it in a 120°C oven to remove the ammonia water to obtain a phosphate-reinforced quartz insulation tile composite material, thus completing the preparation.

[0043] The phosphate reinforced quartz thermal insulation tile composite material prepared in this example was tested, and the results are as follows:

[0044]

[0045] Example 2:

[0046] This embodiment provides a method for preparing a phosphate-reinforced quartz thermal insulation tile composite material, which is specifically carried out by the following steps:

[0047] 1. Dilute aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution with a mass concentration of 5% (the dilution solvent is water), then add silane coupling agent KH550 dropwise, stir for 30 minutes, then add anionic polyacrylamide surfactant dropwise, stir for 30 minutes to obtain an aluminum dihydrogen phosphate resin solution; the amount of silane coupling agent added is 1% of the mass of the aluminum dihydrogen phosphate solution; the amount of surfactant added is 0.05% of the mass of the aluminum dihydrogen phosphate solution;

[0048] 2. Under vacuum and room temperature, the aluminum dihydrogen phosphate resin solution prepared in step 1 was used to impregnate the quartz insulation tile for 3 hours; then, the quartz insulation tile was dried in a 120°C oven to remove excess solvent, thereby obtaining a modified insulation tile;

[0049] 3. Under vacuum environment, immerse the modified insulation tile obtained in step 2 in 15% ammonia water for 3 hours, then dry it in a 120°C oven to remove the ammonia water to obtain a phosphate-reinforced quartz insulation tile composite material, thus completing the preparation.

[0050] The phosphate reinforced quartz thermal insulation tile composite material prepared in this example was tested, and the results are as follows:

[0051]

[0052] Example 3:

[0053] This embodiment provides a method for preparing a phosphate-reinforced quartz thermal insulation tile composite material, which is specifically carried out by the following steps:

[0054] 1. Dilute aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution with a mass concentration of 10% (the dilution solvent is water), then add silane coupling agent KH550 dropwise, stir for 30 minutes, then add anionic polyacrylamide surfactant dropwise, stir for 30 minutes to obtain an aluminum dihydrogen phosphate resin solution; the amount of silane coupling agent added is 1% of the mass of the aluminum dihydrogen phosphate solution; the amount of surfactant added is 0.05% of the mass of the aluminum dihydrogen phosphate solution;

[0055] 2. Under vacuum and room temperature, the aluminum dihydrogen phosphate resin solution prepared in step 1 was used to impregnate the quartz insulation tile for 3 hours; then, the quartz insulation tile was dried in a 120°C oven to remove excess solvent, thereby obtaining a modified insulation tile;

[0056] 3. Under vacuum environment, immerse the modified insulation tile obtained in step 2 in 15% ammonia water for 3 hours, then dry it in a 120°C oven to remove the ammonia water to obtain a phosphate-reinforced quartz insulation tile composite material, thus completing the preparation.

[0057] The phosphate reinforced quartz thermal insulation tile composite material prepared in this example was tested, and the results are as follows:

[0058]

[0059] Example 4:

[0060] This embodiment provides a method for preparing a phosphate-reinforced quartz thermal insulation tile composite material, which is specifically carried out by the following steps:

[0061] 1. Dilute aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution with a mass concentration of 15% (the dilution solvent is water), then add silane coupling agent KH550 dropwise, stir for 30 minutes, then add anionic polyacrylamide surfactant dropwise, stir for 30 minutes to obtain an aluminum dihydrogen phosphate resin solution; the amount of silane coupling agent added is 1% of the mass of the aluminum dihydrogen phosphate solution; the amount of dispersant added is 0.05% of the mass of the aluminum dihydrogen phosphate solution; the amount of surfactant added is 0.05% of the mass of the aluminum dihydrogen phosphate solution;

[0062] 2. Under vacuum and room temperature, the aluminum dihydrogen phosphate resin solution prepared in step 1 was used to impregnate the quartz insulation tile for 3 hours; then, the quartz insulation tile was dried in a 120°C oven to remove excess solvent, thereby obtaining a modified insulation tile;

[0063] 3. Under vacuum and room temperature conditions, immerse the modified insulation tile obtained in step 2 in 15% ammonia water for 3 hours, then dry it in a 120°C oven to remove the ammonia water to obtain a phosphate-reinforced quartz insulation tile composite material, completing the preparation.

[0064] The phosphate reinforced quartz thermal insulation tile composite material prepared in this example was tested, and the results are as follows:

[0065]

[0066] Figure 1 This is the microscopic morphology of commercially available quartz insulation tiles; Figure 2 The microstructure of the phosphate-reinforced quartz thermal insulation tile composite material prepared in Example 2; Figure 3 for Figure 2 A partial enlarged view of .

[0067] Through testing, it was found that when the concentration of Al(H2PO4)3 solution was 5 wt.%, the coating evenly covered the fiber surface with a thickness of about 4 to 10 nm, and there was no obvious colloid at the fiber nodes. The thermal conductivity of the composite material remained at 0.09 W·m -1 ·K -1 , with excellent thermal insulation properties. As the concentration of aluminum dihydrogen phosphate solution increases, the room temperature and high temperature compressive strength of the composite material are significantly improved, increasing by about 7.9 times compared to the unmodified sample (compressive strength is usually less than 0.5MPa).

Claims

1. A method for preparing a phosphate reinforced quartz thermal insulation tile composite material, characterized in that The method is specifically carried out in the following steps:

1. diluting aluminum dihydrogen phosphate to obtain an aluminum dihydrogen phosphate solution, then adding a silane coupling agent and a cosolvent, stirring, and obtaining an aluminum dihydrogen phosphate resin solution; 2. Under vacuum conditions, the aluminum dihydrogen phosphate resin solution prepared in step 1 is used to impregnate the quartz insulation tile; then, the quartz insulation tile is dried to obtain the modified insulation tile; 3. Under a vacuum environment, the modified thermal insulation tile obtained in step 2 is immersed in ammonia water, and then dried to obtain a phosphate reinforced quartz thermal insulation tile composite material, thereby completing the preparation.

2. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that The mass concentration of the aluminum dihydrogen phosphate solution after dilution in step 1 is 1-20%.

3. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that The silane coupling agent in step 1 is KH550.

4. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that The amount of the silane coupling agent added in step 1 is 1-2% of the mass of the aluminum dihydrogen phosphate solution.

5. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that The cosolvent in step 1 is a surfactant.

6. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that The amount of the additive added in step 1 is 0.05-0.5% of the mass of the aluminum dihydrogen phosphate solution.

7. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that Step 2: Control the immersion time to 3~5h.

8. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that Step 2: Control the drying temperature to 120~140℃.

9. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that Step 3: Control the immersion time to 3~5h.

10. The method for preparing a phosphate reinforced quartz thermal insulation tile composite material according to claim 1, characterized in that Control the drying temperature to 120~140℃.

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