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采用苯酚、甲醛、八水氧氯化锆、乙酰丙酮等为原料,乙醇为溶剂,在氢氧化钠催化下制备了可溶于乙醇的锆改性酚醛树脂,用于浸渍裂解工艺制备碳化锆改性碳/碳复合材料;采用FT-IR,XPS,TG对所合成树脂的结构、成分、热性能进行了表征,采用XRD对热处理后的物相进行了分析。结果表明:改性树脂中的锆通过Zr-O或Zr-O-C键与苯环相连,锆的质量分数可达15.92%,树脂的最大热解温度约为580℃。随着锆含量的增加,改性树脂的热解温度降低,热解速率加快,850℃时残碳率为60%;不同锆含量改性树脂1500℃热处理后均转化为ZrO2和ZrC,且随着树脂中锆含量的升高,产物中ZrO2的相对含量有升高的趋势。
Using phenol, formaldehyde, zirconium oxychloride octahydrate and acetylacetone as raw materials and ethanol as solvent, a zirconium-modified phenol resin soluble in ethanol was prepared under the catalysis of sodium hydroxide, which was used to impregnate and pyrolyze to prepare zirconium carbide The structure, composition and thermal properties of the synthesized resin were characterized by FT-IR, XPS and TG. The phase after heat treatment was analyzed by XRD. The results show that the zirconium in the modified resin is connected with the benzene ring through Zr-O or Zr-O-C bonds, the mass fraction of zirconium reaches 15.92% and the maximum pyrolysis temperature of the resin is about 580 ℃. With the increase of zirconium content, the pyrolysis temperature of the modified resin decreased, the pyrolysis rate increased, and the carbon residue rate was 60% at 850 ℃. The modified zirconia resins were transformed to ZrO2 and ZrC after heat treatment at 1500 ℃ With the increase of zirconium content in the resin, the relative content of ZrO2 in the product tends to increase.