大学化学

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基于微波混合加热的TiO2制备及其性质研究综合实验教学改进

尹艳君1, 马自力2, 张凯迪1, 尹晓杰1, 程乐华1   

  1. 1 巢湖学院化学与材料工程学院, 安徽 合肥 238024;
    2 合肥工业大学材料科学与工程学院, 安徽 合肥 230009
  • 收稿日期:2026-07-13 录用日期:2026-08-28
  • 通讯作者: 马自力 E-mail:zlma@hfut.edu.cn Zili Ma
  • 基金资助:
    安徽省质量工程项目教学研究项目(2025jyxm0366)；巢湖学院教学研究重点项目(x23jyxm05)；巢湖学院教学创新团队(x25jxtd02)

Teaching improvement of a comprehensive experiment on the preparation and property investigation of TiO2 via microwave hybrid heating

Yanjun Yin1, Zili Ma2, Kaidi Zhang1, Xiaojie Yin1, Lehua Cheng1   

  1. 1 School of Chemistry and Material Engineering, Chaohu University, Hefei 238024, Anhui Province, China;
    2 School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009, Anhui Province, China
  • Received:2026-07-13 Accepted:2026-08-28
  • Contact: Zili Ma E-mail:zlma@hfut.edu.cn

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摘要： 溶胶-凝胶法制备纳米TiO2及其光催化性能测试是材料、化学及相关专业常设的综合实验。传统实验通常采用马弗炉对凝胶前驱体进行多温度、长时间热处理，存在升温慢、设备占用时间长、能耗较高和大班教学组织困难等问题。在高校实验室安全分级分类管理背景下，高温设备长时间运行也增加了值守、巡检和过程风险管理压力。针对上述问题，本文将微波混合加热引入TiO2前驱体热处理环节，以石墨粉为辅助吸波体，在家用微波炉中实现快速晶化，并与传统高温炉煅烧样品进行对比。结果表明，微波混合加热可在极短时间内获得锐钛矿相TiO2，其晶型特征与传统高温炉所得样品相近；微波处理十分钟后样品出现明显金红石相特征，与传统高温炉较高温度处理所得样品具有相似的相变趋势。在甲基橙光催化降解实验中，微波短时间处理所得样品的降解率与高温炉处理所得样品的降解率接近。改进实验显著缩短了热处理时间，降低了高温设备长时间运行带来的管理压力和能耗，同时将“能量输入方式-晶化行为-光催化性能”的关联引入教学过程。该实验具有安全绿色、周期短、成本低和探究性强等特点，可为纳米材料制备类本科实验的改进提供参考。

关键词: 教学实验改进, 教学价值, 微波混合加热, 安全绿色, 二氧化钛, 实验室安全管理

Abstract: The sol-gel preparation of nano-TiO2 and the evaluation of its photocatalytic activity constitute a representative comprehensive experiment for undergraduate students majoring in chemistry, materials science, and related fields. In the conventional protocol, gel-derived TiO2 precursors are thermally treated in a high-temperature furnace at multiple temperatures over extended durations. This approach suffers from slow heating rates, prolonged equipment occupancy, high energy consumption, and logistical challenges in organizing large laboratory classes. Moreover, under the current risk-based management framework for university laboratories, the prolonged operation of high-temperature equipment intensifies the burden of onsite supervision, routine inspection, and process risk control. To address these issues, microwave hybrid heating was introduced into the thermal treatment stage of TiO2 precursors, employing graphite powder as a microwave susceptor to achieve rapid crystallization in a domestic microwave oven. The resulting samples were compared with those calcined using a conventional high-temperature furnace. The results showed that microwave hybrid heating produced anatase-phase TiO2 within a very short time, with crystallographic characteristics comparable to those of samples prepared using a conventional high-temperature furnace. After 10 min of microwave treatment, distinct rutile-phase features emerged, indicating a phase-transition trend similar to that observed for samples treated at higher temperatures in a conventional furnace. In the photocatalytic degradation of methyl orange, the sample obtained by short-duration microwave treatment exhibited a degradation efficiency comparable to that of the conventionally heat-treated sample. The improved experiment markedly shortens the thermal treatment time, alleviates the management burden and energy consumption associated with prolonged high-temperature operation, and integrates the relationship among energy input mode, crystallization behavior, and photocatalytic performance into the teaching process. This experiment features safety, greenness, a short cycle, low cost, and strong inquiry orientation, offering a valuable reference for the enhancement of undergraduate experiments involving nanomaterial preparation.

Key words: Improvement of teaching experiments, Educational value, Microwave-assisted hybrid heating, Green and safe chemistry, Titania (TiO2), Laboratory safety management