聚乙酰丙酮合锆甩丝法制备氧化锆纤维棉

Preparation of Zirconia Fibers Cotton by Centrifugal Spinning of Polyacetylacetonatozirconium Spinning Solution

采用氧氯化锆、乙酰丙酮等原料合成聚乙酰丙酮合锆纺丝液,经离心甩丝和水蒸汽气氛热处理,成功制备出长度1～10 cm、直径4～15μm、洁白柔韧的ZrO2纤维棉。通过FT-IR和1H-NMR测试,推测了聚乙酰丙酮合锆的链状分子结构。初步研究了高温煅烧后ZrO2纤维的微观结构变化情况,结果表明:直接经1650℃/24 h煅烧,纤维晶粒发生明显长大,同时纤维柔韧性也显著下降;而先经1900℃/10 min快速超高温烧结预处理,再经1650℃保温120 h煅烧,纤维晶粒未发生明显长大,纤维仍可保持较好的柔韧性,表明快速超高温烧结预处理是提高ZrO2纤维高温结构稳定性的有效手段。

Zirconia fibers cotton were prepared by using zirconium oxychloride and acetylacetone as raw materials to synthesize the spinning solution of polyacetylacetonatozirconium（PAZ）,followed by centrifugal spinning and heat-treating under steam atmosphere.The as-prepared zirconia fibers are flexible,with 1-10 cm in length and 4-15 μm in diameter.The molecular structure of PAZ was derived from the characterizations of FT-IR and 1H-NMR.The microstructure changing of the zirconia fibers after calcinated at high-temperature were also investigated.The results showed that when the fibers were directly calcinated at 1650 ℃ for 24 h,obvious grain coarsening was observed along with the decrease of the fibers flexibility.However,when the fibers were pre-sintered at 1900 ℃ for 10 min,then calcinated at 1650 ℃ for 120 h,no pronounced grain growth was observed and the flexibility of the obtained fibers was good.It indicates that fast sintering at ultra-high-temperature is effective for improving the high temperature structural stability of zirconia fibers.