High Pressure Neutron Diffraction Technology and Applications at CMRR
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摘要: 中国绵阳研究堆（CMRR）建有一台专门的高压中子衍射谱仪（凤凰），用于高压科学研究。对聚焦单色器和导管升级后，凤凰谱仪的束流通量大幅度提高。基于凤凰谱仪，建立并发展了一系列高压中子技术，包括：气体压腔、活塞圆筒型压腔、紧固型压腔、标准巴黎-爱丁堡压机（VX4型）、带加热和水冷系统的两面顶压机（HP3-1500）、及压机的调节与定位系统。通过对高温高压样品腔体组装的优化设计，原位中子衍射的温度和压力最高达到34 GPa和1500 ℃。建立的高压中子衍射技术已成功应用于高压溶解度测量、含能材料结构表征、高压聚合反应等方面的研究。Abstract: FENGHUANG diffractometer at CMRR is a neutron diffractometer dedicated for high pressure experiments. After updating the neutron guide and monochromator, now the neutron flux at the sample position can get increased up to 2.84×106 ns–1·cm–2.Based on the FENGHUANG diffractometer, comprehensive high pressure devices and techniques have been developed, such as gas cells, piston cylinders cell, clamp cell, PE press (VX4), opposite anvil press (HP3-1500) along with sample heating and cooling system, and the alignment system for high pressure devices. Moreover, with the modified high pressure and high temperature cell assemblies, the pressure can be up to 34 GPa while the temperature reaches 1500 ℃ at maximum in the angle-dispersive neutron diffraction. Recently, some scientific research have been performed, like the solubility of NaCl at high pressure, the intergranular strain evolution of HMX, and the pressure-induced polymerization. All these experimental experiences from FENGHUANG diffractometer could not only help to promote the development of high pressure techniques on neutron scattering facilities, but also contribute to the users for their high pressure studies.
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Key words:
- high pressure /
- neutron diffraction /
- Paris-Edinburgh press /
- large-volume
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图 2 凤凰谱仪上配备的HP3-1500两面顶压机
Figure 2. HP3-1500 high pressure device for FENGHUANG diffractometer
图 3 不同加载力下NaCl的中子衍射谱
Figure 3. Neutron diffraction patterns of NaCl at different loading forces
图 4 实验与计算的活塞圆筒压腔压力对比
Figure 4. Pressures of piston cylinders cell in the experiment and calculation
图 6 优化的金刚石双凹曲面组装实物图及示意图
Figure 6. Modified DT assembly for the neutron diffraction experiments
图 7 不同压力下Ni的高压中子衍射谱（MgO和金刚石衍射峰分别来自传压介质和压砧）
Figure 7. High pressure neutron diffraction patterns of pure metal Ni at different pressure (Peaks of MgO and diamond come from pressure transmitting medium and anvil, respectively.)
图 8 高温高压中子衍射实验组装
Figure 8. Schematic of high pressure-high temperature assembly for neutron diffraction experiments
图 9 不同温度和压力下MgO的高温高压中子衍射谱（ZrO2和WC衍射峰分别来自传压介质和压砧）
Figure 9. Neutron diffraction patterns of MgO at different pressure and temperature (Peaks of ZrO2 and WC come from pressure transmitting medium and anvil, respectively)
表 1 凤凰谱仪主要的仪器参数
Table 1. Instrumental parameters of FENGHUANG diffractometer
Take-off-angle/(°) Wavelength/Å Scan angle range/(°) 93.8 1.5900−1.5925 −4−153 Maximum beam size/(mm × mm) Flux at sample position/(106 ns−1·cm−2) Minimum resolution/% 30 × 40 0.34−2.84 0.356−0.661 
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