罗鑫,李禹增,邢欢欢,等.钛酸锂产氚陶瓷前驱体浆料制备及其光固化3D打印成形[J].精密成形工程,2024,16(12):1-13.
LUO Xin,LI Yuzeng,XING Huanhuan,et al.Preparation and Photopolymerization 3D Printing of Li2TiO3 Tritium Breeding Ceramic Precursor Slurry[J].Journal of Netshape Forming Engineering,2024,16(12):1-13. |
| 钛酸锂产氚陶瓷前驱体浆料制备及其光固化3D打印成形 |
| Preparation and Photopolymerization 3D Printing of Li2TiO3 Tritium Breeding Ceramic Precursor Slurry |
| 投稿时间：2024-10-01 |
| DOI：10.3969/j.issn.1674-6457.2024.12.001 |
| 中文关键词: 光固化3D打印 钛酸锂产氚陶瓷 前驱体浆料 流变性能 固化性能 |
| 英文关键词: photopolymerization 3D printing Li2TiO3 ceramic precursor slurry rheological properties curing performance |
| 基金项目:国家自然科学基金(52475387);广东省普通高校重点领域专项(2022ZDZX3017);广东省特支计划(2021TQ05Z151);广东省自然科学基金面上项目(2024A1515010049) |
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| 中文摘要: |
| 目的 通过光固化3D打印技术制备钛酸锂(Li2TiO3)产氚陶瓷前驱体浆料，并分析其流变性能和固化性能，以实现一体化制造工艺的创新。方法 首先采用固相法制备Li2TiO3陶瓷前驱体原料，利用锐钛型TiO2和Li2CO3粉末作为粉源。其次，选择有机树脂体系，包括己二醇二丙烯酸酯(HDDA)和三羟基甲基丙烷三丙烯酸酯(TMPTA)作为光敏树脂，以及分散剂、硅烷偶联剂和光引发剂，制备出性能良好的前驱体浆料。通过正交试验探究了固相含量、分散剂含量和光敏树脂单体比例对浆料流变性能的影响，确定了最佳浆料配方。此外，研究了光引发剂含量对固化性能的影响，并测定了浆料的透射深度和临界曝光强度。通过对单层曝光时间与浆料单线条打印精度和梯度孔打印精度之间的关系进行系统性研究，确定了最佳的曝光时间。最终，利用DLP光固化3D打印机成功打印出形貌良好的Li2TiO3前驱体样件。结果 当固相含量(体积分数)为40%、光敏树脂单体体积比例(TMPTA与HDDA)为1∶1、分散剂含量(质量分数)为5%时，陶瓷前驱体浆料具有高固相、低黏度、良好分散性能的优异性能。此外，测定了前驱体陶瓷浆料的最优光引发剂含量(1.5%，质量分数)以及曝光时间范围(6~14 s)，拟合计算得到陶瓷浆料的透射深度(20.2 µm)与临界曝光强度(0.97 mJ/cm2)。最后，进行打印测试，制备出高精度、无裂纹的前驱体陶瓷素坯。结论 所开发的光固化3D打印工艺为新型钛酸锂产氚陶瓷的一体化制造提供了一种有效的方法，有望解决传统制造工艺中存在的问题，为核聚变反应堆中产氚包层的制备提供了新的技术途径。 |
| 英文摘要: |
| The work aims to prepare lithium titanate (Li2TiO3) tritium breeding ceramic precursor slurry through photopolymerization 3D printing technology and analyze its rheological and curing properties to achieve innovative manufacturing processes. The raw materials of Li2TiO3 ceramic precursor were prepared by the solid-phase method, with anatase TiO2 and Li2CO3 powders. Subsequently, an organic resin system, including hexanediol diacrylate (HDDA) and trimethylol propane triacrylate (TMPTA) as photosensitive resins, as well as dispersants, silane coupling agents, and photoinitiators, was selected to prepare a well-performing precursor slurry. Orthogonal experiments were conducted to explore the effects of solid-phase content, dispersant content, and ratio of photosensitive resin monomers on the rheological properties of the slurry, thus determining the optimal slurry formulation. In addition, the effect of photoinitiator content on curing performance was investigated, and the transmission depth and critical exposure intensity of the slurry were measured. By systematically studying the relationship between single-layer exposure time and the printing accuracy of slurry single lines and gradient holes, the optimal exposure time was determined. Ultimately, well-shaped Li2TiO3 precursor samples were successfully printed by a DLP photopolymerization 3D printer. When the solid-phase content was 40% (volume fraction), the volume ratio of photosensitive resin monomer (TMPTA and HDDA) was 1∶1, and the dispersant content (mass fraction) was 5%, the ceramic precursor slurry had excellent properties of high solid-phase content, low viscosity and good dispersibility. In addition, the optimum photoinitiator content (1.5%, mass fraction) and exposure time range (6-14 s) of precursor ceramic slurry were measured, and the transmission depth (20.2 µm) and critical exposure intensity (0.97 mJ/cm2) of ceramic slurry were obtained by fitting calculation. Finally, the printing test was carried out to prepare the high-precision and crack-free precursor ceramic blank. The developed photopolymerization 3D printing process provides an effective method for the integrated manufacturing of new-type lithium titanate tritium breeding ceramics, which is expected to solve the problems in traditional manufacturing processes and provide a new technical approach for the preparation of tritium breeding blankets in fusion reactors. |
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