Preparation and performance of hollow ceramic microsphere composites with high-temperature resistance, low thermal conductivity and toughness
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摘要: 在高速飞行的过程中飞行器温度急速上升，飞行器舱段间的密封材料不仅要具有优异的耐高温性能，同时要具有较低的导热系数辅助参与阻隔舱段间的热量传递，并且要具有优异的力学性能使其不被破坏。以中空陶瓷微球为骨料，加入酚醛树脂及磷酸盐固化体系制备有机/无机杂化耐高温韧性复合材料，并对复合材料进行高温处理，研究复合材料在高温处理前后的变化。通过力学性能测试、SEM观察以及XRD和FT-IR测试对复合材料高温处理前后的抗压强度、压缩形变能力、微观结构以及组分变化进行表征，并通过火焰燃烧对复合材料耐高温性能进行测试。结果表明，所制备的复合材料具有较高的抗压强度以及优异的韧性，1000℃高温处理600 s复合材料的宏观形貌未受到影响，具有较高的热稳定性。导热系数测试结果表明，中空陶瓷微珠含量的增加、酚醛树脂的添加以及高温处理均会导致复合材料导热系数降低，最低的导热系数低至0.16 W/(m·K)。Abstract: In the process of high-speed flight, the temperature of the aircraft rises rapidly. The sealing material between the aircraft cabin should not only have excellent high-temperature resistance, but also have a low thermal conductivity to assist in blocking the heat transfer between the cabin, and have excellent mechanical properties to prevent it from being damaged. Used hollow ceramic microspheres as aggregates, added phenolic resin and phosphate curing system to prepare organic/inorganic hybrid high-temperature resistant and tough composites. The composites were subjected to high-temperature treatment to study the changes of the composites before and after the high-temperature treatment. The compressive strength, compression deformation ability, microstructure and composition changes of the composites before and after the high-temperature treatment were characterized by mechanical performance test, SEM observation, XRD and FT-IR. In addition, the high-temperature resistance performance of the composites was tested by flame combustion. The overall results show that the prepared composites have high compressive strength and excellent toughness. The macro morphology of the composites is not affected by the high-temperature treatment at 1000℃ for 600 s, which indicates that the composites have high thermal stability. And the thermal conductivity test results show that the increase in the content of hollow ceramic microbeads, the addition of phenolic resin and the high-temperature treatment all cause the thermal conductivity to decrease, and the lowest thermal conductivity is as low as 0.16 W/(m·K).
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Key words:
- hollow ceramic beads /
- composites /
- high temperature resistance /
- toughness /
- phenolic resin /
- thermal conductivity
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图 1 FA复合材料高温处理前 (a) 和高温处理后 (b) 的XRD图谱
Figure 1. XRD patterns of FA composites before (a) and after (b) high temperature treatment
PF—Phenol-formaldehyde resin; FA—Fly ash; P—Phosphate; 50, 100—Mass fraction of PF
图 2 FA复合材料高温处理前 (a) 和高温处理后 (b) 的FT-IR图谱
Figure 2. FT-IR spectra of FA composites before (a) and after (b) the high-temperature treatment
图 3 FA复合材料高温处理前 (a) 和高温处理后 (b) 的抗压强度
Figure 3. Compressive strength of FA composites before (a) and after (b) the high-temperature treatment
图 4 不同组分FA复合材料高温处理前后最大抗压强度对比
Figure 4. Comparison of maximum compressive strength of FA composites with different components before and after high temperature treatment
图 5 FA复合材料高温处理前 (a) 和高温处理后 (b) 的压缩形变
Figure 5. Compressive deformation of FA composites before (a) and after (b) high temperature treatment
图 6 不同组分制备的FA复合材料不同时间的火焰燃烧测试：((a1)~(a3)) FA∶P=300∶100; ((b1)~(b3)) FA∶P∶PF=300∶100∶50;((c1)~(c3)) FA∶P∶PF=300∶100∶100
Figure 6. Flame combustion test of FA composites prepared by different components in different periods：((a1)-(a3)) FA∶P=300∶100; ((b1)-(b3)) FA∶P∶PF=300∶100∶50; ((c1)-(c3)) FA∶P∶PF=300∶100∶100
图 7 火焰燃烧前 ((a1)~(c1)) 和火焰燃烧后((a2)~(c2)) 测试FA复合材料的宏观形貌：((a1), (a2)) FA∶P=300∶100; ((b1), (b2)) FA∶P∶PF=300∶100∶50; ((c1), (c2)) FA∶P∶PF=300∶100∶100)
Figure 7. Macromorphology of the FA composites before ((a1)-(c1)) and after ((a2)-(c2)) flame combustion test：((a1), (a2)) FA∶P=300∶100; ((b1), (b2)) FA∶P∶PF=300∶100∶50; ((c1), (c2)) FA∶P∶PF=300∶100∶100)
图 8 1000℃处理600 s后FA复合材料的宏观形貌
Figure 8. Macromorphology of the FA composites after 1000℃ treatment for 600 s
图 9 高温处理前FA复合材料SEM图像
((a), (b)) FA∶P=100∶100; ((c), (d)) FA∶P∶PF=100∶100∶50; ((e), (f)) FA∶P∶PF=100∶100∶100
Figure 9. SEM images of FA composites before the high-temperature treatment
图 10 1000℃高温处理后FA复合材料的SEM图像
((a), (b)) FA∶P=100∶100; ((c), (d)) FA∶P∶PF=100∶100∶50; ((e), (f)) FA∶P∶PF=100∶100∶100
Figure 10. SEM images of FA composites after the high-temperature treatment
图 11 FA复合材料高温处理前 (a) 和高温处理后 (b) 的孔隙率变化
Figure 11. Porosity of the FA composites before (a) and after (b) high-temperature treatment
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