Pressure Distribution Investigation in Silicon Oil Compressed in Diamond Anvil Cell
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摘要: 金刚石压腔是被广泛使用的静高压装置之一，具有压力范围宽，光学适用性优良以及使用便利等优点，对高压科学的发展起到了巨大的推动作用。然而，压力较高时，传压介质固化等因素可能造成压腔内静水压环境失衡，从而产生压力梯度。采用皮秒超声技术测量压腔内各处的声学信号，通过声学数据分析获得了高压下样品腔内硅油的压力分布，结果显示：压力梯度随压强的升高而增大，从1 GPa时的1.3×10−4 GPa/μm增长为30 GPa时的5.3×10−2 GPa/μm。该方法不仅克服了以往实验技术在信号测量连续性、样品选择等方面的限制，还可在普通实验室搭建和使用。此外，还结合原位拉曼光谱技术，分析了加压过程中硅油中压力标准差的异常波动，该波动可能与硅油在经历了玻璃化转变之后发生固-固相变有关。Abstract: Diamond anvil cell (DAC) is a kind of widely used static-high-pressure device. Benefitting from its wide pressure range, excellent optical applicability and convenience of use, DAC provides a tremendous boost to the development of high-pressure science. However, at high pressures, factors like solidification of pressure transmitting medium may cause destruction of the hydrostatic pressure condition in the DAC sample chamber, leading to the generation of pressure gradients. In this work, a new method of using the technique of picosecond ultrasonics to investigate acoustic signal distribution at various locations within the sample chamber was proposed, which can analyze the pressure distribution via the acoustic observations. Limitations in the continuity of signal acquisition, sample selection, etc. can be overcome in this experimental technique, which could be built and manipulated in an ordinary laboratory. Here, pressure gradient in silicon oil was carried out under compression using this technique, and the results revealed that the pressure gradient in the sample chamber increased from 1.3×10−4 GPa/μm at 1 GPa to 5.3×10−2 GPa/μm at 30 GPa. In addition, the anomalous change of standard deviation of the pressure distribution was analyzed by combining it with in-situ Raman spectroscopy, then the possible phase transitions of silicone oil at high pressures were discussed.
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Key words:
- diamond anvil cell /
- pressure gradient /
- picosecond ultrasonics /
- silicone oil /
- phase transition
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图 1 (a) 皮秒超声实验装置（PBS为偏振分束器，λ/4为1/4波片，λ/2为1/2波片，AOM为声光调制器，DBP为二向色分束器，PD为光电探测器）；(b) 放大的金刚石压腔（Transducer为光声换能介质（钨箔），样品腔的剩余空间由硅油填充，图中还注明了泵浦光和探测光的光路及声波的传播路径）
Figure 1. (a) Schematic of the picosecond ultrasonics experiment setup (PBS represents polarization beam splitter, λ/4 represents quarter waveplate, λ/2 represents half wave plate, AOM is acousto-optic modulator, DBP is dichroic beam splitter, and PD is photodetector); (b) enlarged diagram of the diamond anvil cell (transducer stands for the opto-acoustic transducer (tungsten foil), optical paths of pump and probe beams, as well as propagation of sound waves are shown as well in the figure)
图 2 (a) 显微镜下DAC（最外圈的亮色圆环（直径为300 μm）对应金刚石台面，中间的浅色圆片为钨箔，图中标出了测量点1、2和3以及红宝石的位置）；(b) 4.1 GPa时点1处采集的超声原始信号；(c) 去除热背底后的布里渊振荡信号；(d) 将(c)进行快速傅里叶变化后得到的频域信号
Figure 2. (a) Image inside the DAC observed under microscope (The outermost bright-colored circular region stands for the culet area with diameter of 300 μm. The middle-most light-colored circular plate are the tungsten foil, measuring positions 1, 2, and 3, aswell as the location of ruby are labeled.); (b) raw signal of picosecond ultrasonics collected at pressure of 4.1 GPa at Position 1;(c) Brillouin oscillations after subtraction of the thermal background; (d) frequency spectrum after Fourier transformation of (c)
图 3 (a) 高压下点1、2和3处的压力分布及其误差；(b) 各点与点3之间的压力差（点3设为参照，其压强均设置为零）
Figure 3. (a) Pressure distribution at measuring positions 1, 2 and 3; (b) corresponding pressure gradient(the pressure gradient at point 3 is set to zero)
图 4 高压下各测量点位间压力的标准差
Figure 4. Standard deviation of the pressures measured at different measuring positions at different pressures
表 1 高压下3个测量点处采集的布里渊振荡频率和由红宝石标定的压强
Table 1. Brillouin oscillation frequencies collected at the three measuring positions and pressures calibrated by ruby at different pressure steps
No. Frequency/GHz Pressure on ruby/GPa Position 1 Position 2 Position 3 1 13.07(6) 13.04(6) 13.04(6) 1.0 2 21.56(12) 21.51(12) 21.43(12) 4.1 3 25.52(14) 25.42(14) 25.36(14) 7.0 4 29.38(18) 29.18(18) 28.99(18) 10.2 5 33.17(17) 33.09(17) 33.01(17) 13.8 6 38.10(20) 37.74(20) 37.50(20) 20.2 7 41.98(22) 41.67(22) 41.30(22) 25.0 8 45.79(24) 45.58(24) 45.05(24) 30.0 
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