| 题名 | KDP/DKDP晶体生长关键技术研究 |
| 作者 | 谢晓义 |
| 文献子类 | 博士 |
| 导师 | 邵建达 |
| 关键词 | KDP/DKDP晶体 KDP/DKDP crystals 快速生长 Rapid growth 连续过滤 Continuous filtration 监控系统 Monitoring system 性能研究 Performance study |
| 其他题名 | Study on key technologies of KDP/DKDP crystal growth |
| 英文摘要 | KDP/DKDP晶体作为性能良好的非线性和电光晶体，拥有透过波段宽、易生长大尺寸等优点，也是目前唯一可用于惯性约束核聚变中的晶体材料。但目前国内晶体，尤其是DKDP晶体的性能仍然不能满足装置的需求。鉴于晶体损伤机理研究的复杂性和缺陷探测比较困难，本文从减少引起损伤的缺陷源头方面着手，主要围绕KDP/DKDP晶体快速生长过程中涉及到的关键技术进行研究。具体开展的工作如下： 采用自主研制的带有连续过滤系统的生长设备，结合软件模拟的指导，快速生长了透亮、无可见缺陷的小尺寸Z向/横向KDP晶体、大尺寸Z向/横向KDP晶体，以及小尺寸横向70%氘化率DKDP晶体。实验测定了70%DKDP晶体的溶解度曲线，分析了溶质析出过程中D和H元素的交换，并根据KDP/DKDP晶体的溶解度公式，首创性地采用“称重法”测定生长溶液的饱和温度，通过实验证明了其可靠性。 理论分析了连续过滤技术在晶体生长中的必要性，并实验证实了连续过滤技术在不影响溶液稳定性的同时有效减少了溶液中颗粒物的浓度及粒径大小。实验分析了过滤方式、过滤流量对连续过滤效果的影响，发现过滤孔径越小、过滤级次越多、过滤流量适宜时，过滤效果最佳，这为晶体生长过程中过滤参数的选择提供了实验依据。 针对以往晶体生长过程中尺寸变化只能依赖人眼辨认的问题，自主研发了一套全自动晶体生长监控系统。该系统不仅能够持续采集晶体的生长参数，记录设备的工作状态，还能实时拍摄晶体的照片，建立三维模型，获得晶体的尺寸，从而能计算出实时的溶质消耗量，有助于精确调整降温速率，控制晶体外形，促进晶体的稳定生长。 开展了连续过滤快速生长的KDP/DKDP晶体的性能研究，对其氘化率测试、透过率、拉曼光谱、热学分析、缺陷损伤以及辐照性能进行了细致分析。重点研究了KDP/DKDP晶体的损伤性质，测量了晶体不同区域的杂质种类、含量与体内散射点分布，研究了不同晶体的损伤阈值，证实了连续过滤技术对晶体的损伤性能有所改善，但还需进一步优化过滤参数，提升过滤能力；实验验证了红外光谱法测定溶液氘化率的可靠性，关于晶体光学性能、热学性质以及辐照性能的研究对其发展和应用也有着重要的参考价值。; KDP/DKDP crystals, as non-linear and electro-optical crystals with good performance, have the advantages of being easy to grow to large size, wide band width, and are currently the only crystalline materials that can be used in Inertial Confinement Fusion. However, the performance of local-made crystals, especially DKDP crystals, still cannot meet the requirements of the device. In view of the complexity and difficulty of the research on the mechanism of crystal damage and detection of defects, this thesis starts with the purpose of reducing the source of defects that cause damage, mainly focusing on the key technologies involved in the rapid growth of KDP/DKDP crystals. The specific work carried out is as follows： Under the guidance of software simulation about the flow field and using self-developed growth equipment with continuous filtration system, we rapidly grew transparent small and large size Z-/horizontal KDP crystals, and small scale horizontal 70% deuterated DKDP crystals without visible defects. The solubility curve of 70% DKDP crystals was determined experimentally. And the exchange of D and H elements was analyzed during solute precipitation process. According to the KDP/DKDP crystal solubility formula, the “weighing method” was used to measure the saturation temperature of growth solution. The reliability of the formula was proved by experiments. The necessity of continuous filtration technology in crystal growth was theoretically analyzed, and it was confirmed that the continuous filtration technology can effectively reduce the concentration and size of the particles in the solution without affecting the stability of the solution. The effects of filtration method and flow rate on the continuous filtration effect were analyzed experimentally. It was found that the smaller the filtration pore size, the more filtration grades, and the appropriate filtration flux, the best filtration effect would be obtained. These results provide experimental basis for the selection of filtration parameters in the crystal growth process. Aiming at the problem that the size change during crystal grow in the past can only rely on the ability of human eyes to distinguish, we independently developed a fully automatic crystal growth monitoring system. The system can not only continuously acquire the crystal growth parameters, record the working status of the equipment, but also can take pictures of crystals in real time, establish a three-dimensional model, and obtain the crystal size, so that real-time solute consumption can be calculated, which helps to accurately adjust the cooling rate, control crystal shape, and promote crystal growth stably. The performance of rapidly growing KDP/DKDP crystals with continuous filtration was carefully studied, such as the deuteration rate, transmittance, Raman analysis, thermal properties, defect damage, and irradiation performance. The damage properties of KDP/DKDP crystals were analyzed in detail. The species and concentration of impurities and distribution of scattering points in different regions of the crystal were measured, and the damage thresholds of different crystals were studied. It was confirmed that the continuous filtration technique has improved the damage performance of crystals, but it is necessary to further optimize the filtration parameters and improve the filtration capacity. The infrared spectroscopy was verified experimentally to be reliable to determine the the deuteration rate of the solution. The investigations on optical properties, thermal properties and irradiation performance also have important reference significance for the development and application of crystals. |
| 学科主题 | 材料学 |
| 内容类型 | 学位论文 |
| 源URL | [http://ir.siom.ac.cn/handle/181231/31072]  |
| 专题 | 中国科学院上海光学精密机械研究所 |
| 作者单位 | 中国科学院上海光学精密机械研究所 |
| 推荐引用方式 GB/T 7714 | 谢晓义. KDP/DKDP晶体生长关键技术研究[D]. |
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