High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction(XRD) in diamond anvil cells(DACs) using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF(Beijing Synchrotron Radiation Facility) and some results are also presented.     

铝的等温状态方程

 采用原位高压同步辐射X射线衍射技术,利用金刚石对顶砧（DAC）装置产生高压,选用高纯NaCl粉末作为传压介质与标压物质,在室温下、21.5 GPa的压力范围内,测定了铝的等温状态方程。利用Murnaghan方程对实验结果进行了数值拟合,得到铝的零压体弹模量及其一级压力导数分别为B₀=(77±2) GPa,B₀′=4.8±0.3。该结果同相关文献资料报导的值在误差范围内符合得很好,略显得较大,这是由于传压介质NaCl的非静水压效应所致。在实验所达到的压力范围内,未发现明显的相变迹象。     

纳米硫化锌球壳的高压相变研究

 采用同步辐射能量色散X射线衍射（EDEX）技术和金刚石对顶砧高压装置,对纳米硫化锌球壳进行了原位高压X射线衍射实验。最高压力达33.3 GPa。常压下纳米硫化锌球壳为纤锌矿结构和闪锌矿结构共存的混相结构。压力达到11.2 GPa时,纳米硫化锌空心球中的纤锌矿结构全部转变为闪锌矿结构。压力达到16.0 GPa时,发生了由闪锌矿结构向岩盐矿结构的相变,在17.5 GPa和21.0 GPa时分别出现未知峰,33.3 GPa时基本完全转变为岩盐矿结构。两个相变均为可逆相变。     

室温高压下天然锡石状态方程研究

 利用金刚石压腔同步辐射X射线就位衍射技术,在室温、最高压力达13 GPa条件下,对采自云南个旧锡矿的天然锡石做了X衍射测量。结果表明,在实验压力范围内锡石未发生相变,其晶胞参数随压力增大而逐渐减小。与前人合成锡石实验结果相比,本次实验测定的晶胞参数偏大。由Birch状态方程对实验结果p-V进行最小二乘法拟合,得出锡石的K_T(0)＝228 GPa。分析认为,在天然矿物晶体中,Zr对Sn的类质同象置换是晶胞参数偏大的主要原因。     

Structural stability of ultra-high temperature refractory material MoSi_2 and Mo_5Si_3 under high pressure

In-situ angle dispersive x-ray diffraction(ADXRD) with synchrotron radiation source is performed on an ultra-high temperature refractory of MoSi_2 and Mo_5Si_3 by using a diamond anvil cell(DAC) at room temperature. While the pressureinduced volume reduction is almost constant, the value of the bulk modulus increases with the decrease of molybdenum content in the system. According to the Brich–Murnaghan equation, the bulk modulus 222.1(2.1) GPa with its pressure derivative 4 of MoSi_2, and the bulk modulus 308.4(7.6) GPa with its pressure derivative 0.7(0.1) of Mo_5Si_3 are obtained.The experimental data show that MoSi_2 has distinct anisotropic behavior, Mo_5Si_3 is less anisotropic than MoSi_2. The result shows that MoSi_2 and Mo_5Si_3 have the structural stabilities under high pressure. When the pressure reaches up to 41.1 GPa, they can still maintain their body-cantered tetragonal structures.     

振动压路机的滑膜控制研究

振动压实中的跳振现象在压实过程中时有发生,跳振现象将造成路基压实质量难以保证,也会对振动压路机操作人员的身心健康产生不利影响。因此,本文从控制“振动压路机-土”系统动力学模型的减振系统阻尼力的角度进行分析,通过研究模糊PID控制和滑模控制对振动控制产生的影响,得到相较于模糊比例积分微分（proportional integral differential,PID）控制,滑模控制可消除系统抖振的影响,更有利于保证路基压实过程中的振动控制,为振动压实的施工作业提供理论支持。     

A new cell for X-ray absorption spectroscopy study under high pressure

X-ray absorption fine structure （XAFS） spectroscopy is a powerful technique for the investigation of the local environment around selected atoms in condensed matter. XAFS under pressure is an important method for the synchrotron source. We design a cell for a high pressure XAFS experiment. Sintered boron carbide is used as the anvils of this high pressure cell in order to obtain a full XAFS spectrum free from diffraction peaks. In addition, a hydraulic pump was adopted to make in-suit pressure modulation. High quality XAFS spectra of ZrH2 under high pressure （up to 13 GPa） were obtained by this cell.     

Pressure-induced phase transition of wulfenite

The in-situ high-pressure structures of wulfenite have been investigated by means of angular dispersive X-ray diffraction with diamond anvil cell and synchrotron radiation. In the pressure up to 22.9 GPa, a pressure-induced scheelite-to-fergusonite transition is observed at about 10.6 GPa. The pressure dependence for the lattice parameters of wulfenite is reported, and the axial compression coefficients Ka₀=－1.36×10^－3 GPa^－1 and Kc₀= －2.78×10^－3 GPa^－1 are given. The room-temperature isothermal bulk modulus is also obtained by fitting the P-V data using the Murnaghan equation of state.     

The Phase Transition of Eu2O3 under High Pressures

Pressure-induced phase transition of cubic Eu2 03 is studied by angle-dispersive x-ray diffraction （ADXD） up to 42.3 GPa at room temperature. A structural transformation from a cubic phase to a hexagonal phase is observed, which starts at 5.0 GPa and finishes at about 13.1 GPa. The phase transition leads to a volume collapse of 9.0% at 8.6 GPa. The hexagonal phase of Eu2 03 maintains stable up to the highest experiment pressure. After re/ease of pressure, the high-pressure phase transforms to a monoclinic phase. The pressure-volume data are fitted with the Birch-Murnaghan equation of state. The bulk moduli obtained upon compression from the fitting are 145（2） GPa and 151（6） OPa for the cubic and hexagonal phases, respectively, when their first pressure derivatives are fixed at 4.     

High-Pressure and High-Temperature Behaviour of Gallium Oxide

High-temperature and high-pressure behaviours of β-Ga2O3 powder are studied by energy-dispersive x-ray diffrac- tion in a diamond anvil cell （DAC）. It is found that the phase transition from the monoclinic β-Ga2O3 to the trigonal α-Ga2O3 occurs at around 19.2 GPa under cold compression. By heating the powder to 2000 K at 30 GPa, we confirm that α-Ga2O3 is the most stable structure at the high pressure. Furthermore, the structural transition from β-Ga2O3 to α-Ga2O3 is irreversible. After laser heating, the recrystallized Ga2O3 has a preferable （012） orientation. This interesting behaviour is also discussed.