静电悬浮激光脉冲局部温度梯度触发形核实验技术
doi: 10.11728/cjss2025.06.2024-0095 cstr: 32142.14.cjss.2024-0095
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王艳秋 1987年7月出生于河北省承德市, 现为中国科学院国家空间科学中心高级工程师, 博士研究生, 主要研究方向为静电悬浮无容器实验技术研究、空间科学实验技术研究及仪器研制. E-mail: wangyanqiu@nssc.ac.cn -
孙志斌 1978年4月出生于山西省运城市, 中国科学院国家空间科学中心研究员, 博士生导师, 主要研究方向为信息光电子学、空间科学实验技术和空间光电子测量仪器研制. E-mail: zbsun@nssc.ac.cn
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Local Temperature Gradient Laser Pulse Triggered Nucleation Experimental Technology under Electrostatic Levitation
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摘要: 通过激光脉冲在样品表面局部区域形成温度梯度, 引起实验样品内部结构起伏和能量起伏概率加大, 程度加深, 使晶体从熔融的液相亚稳态相变为固相, 实现静电悬浮下高质量可控深过冷激光脉冲触发形核. 通过有限元模拟仿真方法研究不同加热激光束斑直径, 功率为9 W, 功率密度为$ 2.86\times {10}^{8}\;\mathrm{W} \cdot {\mathrm{m}}^{-2} $和$ 1.146\times {10}^{7}\;\mathrm{W} \cdot {\mathrm{m}}^{-2} $的激光对温度梯度场的影响, 得到不同激光束斑直径下熔融样品局部温度梯度场分布结果. 采用直径为2 mm锆材料样品, 研究在较小激光束斑直径下, 不同的激光脉冲宽度与过冷度熔融材料样品触发形核时间尺度变化. 基于经典形核理论, 通过16组不同过冷度, 每组20次自发形核的数据统计分析, 得到锆材料样品在不同过冷度下从母相熔体的亚稳态向固相移动所需时间的变化关系. 在此基础上, 开展激光脉冲束斑直径为0.2 mm的波长为936 nm, 样品为锆材料激光脉冲触发形核实验研究. 实验结果表明, 锆材料在过冷度为195 K±3 K, 样品形核凝固过程中所需的时间比自发形核所需时间降低3/4, 高质量可控地使熔融样品在不同过冷度下触发形核.Abstract: The containerless and solidification method of electrostatically suspended deep subcooled samples is of great significance for materials science research and materials preparation, and this paper proposes to realize the experimental study of triggered nucleation and solidification and measurement of materials under deep subcooling based on the local temperature gradient field of the laser pulse. By triggering the laser pulse to generate a local temperature, a temperature gradient is formed around the sample, and the temperature gradient triggers convection to increase the probability of structural and energy undulation inside the experimental sample and deepen the degree, so that the crystals change from a molten liquid phase to a solid phase, realizing high-quality and controllable deep-subcooling laser pulse-triggered nucleation under electrostatic levitation. By means of finite element simulation methods, the effect of laser heating with different spot diameters and a power of 9 W, a power density of $ 2.86\times {10}^{8}\;\mathrm{W} \cdot {\mathrm{m}}^{-2} $ and $ 1.146\times {10}^{7}\;\mathrm{W} \cdot {\mathrm{m}}^{-2} $ on the temperature gradient field was investigated. The distribution results of the local temperature gradient field in the molten sample under different laser spot diameters were obtained. A zirconium sample with a diameter of 2 mm was used in the experiment to study the time scale of triggered nucleation of molten samples with different laser pulse widths and subcooling degrees under smaller laser beam spot diameters. Based on the classical nucleation theory, the time required for the zirconium samples to move from the substable state of the mother phase melt to the solid phase under different supercooling degrees was obtained by statistically analyzing the data from 16 groups of 20 spontaneous nucleations at different supercooling degrees. On this basis, the experimental study of laser pulse triggered nucleation was carried out at a wavelength of 936 nm with a laser pulse spot diameter of 0.2 mm and a sample of zirconium material. The experimental results show that the time required for nucleation and solidification of zirconium material at a low subcooling of 195 K ± 3 K is 3/4 times lower than that required for spontaneous nucleation, and that high quality and controllable nucleation can be triggered for molten samples at different subcooling levels.
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图 2 静电悬浮控制单元原理
Figure 2. Schematic diagram of control unit of electrostatic levitation
图 5 激光光束半径为0.2 mm时不同时刻样品温度分布
Figure 5. Temperature distribution inside the sample at different times when the laser beam diameter is 0.2 mm
图 6 平均温度1800±10 K的横截面温度场分布
Figure 6. Temperature distribution in the cross section of the sample with 1800±10 K average temperature under the thermal equilibrium state
图 7 样品内的温度梯度仿真结果. (a)最大温度梯度, (b)平均温度梯度
Figure 7. Simulated temperature gradient in the sample during heating. (a) Maximum temperature gradient, (b) average temperature gradient
图 8 热趋于稳定状态下样品最大温度变化
Figure 8. Maximum temperature variation of the sample under thermal nearby equilibrium state
图 9 过冷态下样品锆的温度及激光总功率随时间的变化
Figure 9. Variation of sample zirconium temperature and total laser power with time during undercooling
图 10 不同过冷度下自发形核凝固时间拟合曲线
Figure 10. Fitted curves of solidification time of spontaneous nucleation at different supercooling degrees
图 11 不同脉冲激光宽度锆的形核温度及时间
Figure 11. Nucleation temperature and time of zirconium with different pulse laser width
图 12 锆样品过冷保持时间与激光脉冲触发形核时间比值
Figure 12. Ratio of supercooling holding time and laser pulse-triggered nucleation time of zirconium samples
图 13 样品锆在245 K过冷度下凝固时的表面固液界面迁移情况 (暗色部分为过冷的液态锆, 明亮色部分为再辉凝固后的固态锆. 高速相机拍摄速率为200 kframe·s–1)
Figure 13. Surface solid-liquid interface migration situation of zirconium under 245 K undercooling (The dark parts of the picture are liquid zirconium that is supercooled, and the bright white parts are solid zirconium that has recized. Shooting rate of high-speed camera is 200 kframe·s–1)
图 14 锆样品激光脉冲触发形核凝固固液界面迁移速度
Figure 14. Migration velocity of solid-liquid interface for laser pulse-triggered nucleation solidification of zirconium samples
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