静电纺丝法制备钛酸钡纳米纤维的工艺研究

Study on the Preparation of Barium Titanate Nanofibers by Electrospinning

摘要:

本文以乙酸钡和钛酸四丁酯为原料,以聚乙烯吡咯烷酮(PVP, Mw=1300000)为粘性剂,采用溶胶-凝胶法结合静电纺丝技术制备了高长径比的钛酸钡纳米纤维(BaTiO₃ NFs),XRD结果表明,经900^_oC煅烧处理后的BaTiO₃ NFs主相为立方相。首先,分别研究乙酸-乙醇-去离子水、乙酸-N,N-二甲基甲酰胺(DMF)-去离子水和乙酸-DMF-乙酰丙酮三种纺丝溶剂对纤维直径的影响,SEM结果表明,当PVP含量为8.7wt.%时,乙酸-DMF-乙酰丙酮为优化的纺丝溶剂,此时制备的BaTiO₃ NFs直径最小为200nm,长径比最大为100:1；在此基础上,又采用正交试验法,考察了针头到接收器的距离、纺丝液流率和纺丝电压等纺丝参数对BaTiO₃ NFs纤维长径比的影响,结果发现,当针头到接收器的距离为21cm、流率为0.5mL/h以及纺丝电压为21kV是优化的纺丝参数,由此制备的BaTiO₃ NFs形貌较均匀,直径为200nm,长径比最大为125:1。

Abstract:

In this paper, barium acetate and tetrabutyl titanate were used as raw materials, and polyvinylpyrrolidone (PVP, Mw=1300000) was used as the viscous agent. The barium titanate nanoparticle with high aspect ratio was prepared by sol-gel method combined with electrospinning technology. XRD results showed that the main phase of BaTiO₃ NFs was cubic phase after calcination at 900 °C. Firstly, this paper investgated the effects of acetic acid-ethanol-deionized water, acetic acid-DMF-deionized water and acetic acid-DMF-acetylacetone on the fibers diameter. The results of SEM showed that when the PVP content was 8.7wt.%, acetic acid-DMF-acetylacetone was the optimized spinning solvent. The BaTiO₃ NFs prepared at this time had a minimum diameter of 200nm and an aspect ratio of 100:1. On the basis of the orthogonal test method, the influence of the spinning parameters such as the distance from the needle to the receiver, the flow rate and the spinning voltage on the aspect ratio of BaTiO₃ NFs was investigated. It was found that the distance from the needle to the receiver was 21cm, flow rate of 0.5mL/h and spinning voltage of 21kV were optimized spinning parameters. The prepared BaTiO₃ NFs have a uniform morphology, diameter of 200nm and aspect ratio ratio of 125:1.