Hafnium oxide polymer ceramic precursor and preparation method thereof: Fid-Bau Portal

Hafnium oxide polymer ceramic precursor and preparation method thereof

WANG QIAN / GAI KE / ZHAO TONG / LIU WEISEN / YE LI / HAN WEIJIAN

The invention discloses a hafnium oxide polymer ceramic precursor and a preparation method thereof. Comprising the following steps: 1) adding an organic hafnium source into a solvent, and stirring, refluxing and dissolving for 0.5-5 hours; adding a complexing agent mixed solution at the heating temperature of 50-100 DEG C, and continuously stirring, heating and refluxing for 0.5-6 hours; (2) adding a mixed solution into the reaction system obtained in the step (1), and carrying out reflux reaction for 0.5-3 hours after the mixed solution is added; then carrying out atmospheric distillation or reduced pressure distillation to remove the solvent, and cooling to room temperature to obtain a hafnium oxide polymer ceramic precursor; according to the invention, the organic hafnium source is coordinated and stabilized by adopting two complexing agents, and the linear degree and molecular weight of the precursor are improved by adjusting the addition amount, variety and proportion of the two complexing agents, so that the spinning performance of the precursor is improved. The softening point of the obtained ceramic precursor is 120-200 DEG C, the highest ceramic yield is 56%, and the highest molecular weight is 3400.

本发明公开了一种氧化铪聚合物陶瓷前驱体及其制备方法。包括如下步骤：1)将有机铪源加入到溶剂中，搅拌回流溶解0.5～5h；在加热温度50～100℃下，加入络合剂混合溶液，继续搅拌加热回流0.5～6h；2)向步骤1)所得反应体系中加入混合液，加完后回流反应0.5～3h；随后进行常压蒸馏或减压蒸馏除去溶剂，降至室温得到氧化铪聚合物陶瓷前驱体。本发明采用两种络合剂对有机铪源进行配位稳定，通过调节两种络合剂的添加量、种类、比例，提高了前驱体的线性程度及分子量，从而提高前驱体的纺丝性能。得到的陶瓷前驱体的软化点介于120～200℃，陶瓷产率最高为56％，分子量最高达3400。

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