Neutron diffraction techniques of large-volume samples at high pressure using compact opposed-anvil cells are developed at a reactor neutron source, China's Mianyang research reactor. We achieve a high-pressure condi...Neutron diffraction techniques of large-volume samples at high pressure using compact opposed-anvil cells are developed at a reactor neutron source, China's Mianyang research reactor. We achieve a high-pressure condition of in situ neutron diffraction by means of a newly designed large-volume opposed-anvil cell. This pressure calibration is based on resistance measurements of bismuth and the neutron diffraction of iron. Pressure calibration experiments are performed at room temperature for a new cell using the tungsten carbide anvils with a tapered angle of 30°, Φ4.5 mm culet diameter and the metal-nonmetal composite gasket with a thickness of 2 mm. Transitions in Bi(Ⅰ–Ⅱ 2.55 GPa, Ⅱ–V 7.7 GPa) are observed at 100 and 300 kN, respectively, by resistance measurements.The pressure measurement results of neutron diffraction are consistent with resistance measurements of bismuth.As a result, pressures up to about 7.7 GPa can routinely and stably be achieved using this apparatus, with the sample volume of 9 mm^3.展开更多
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 ...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.展开更多
We have studied the high-pressure compression behavior of molybdenum up to 60 GPa by synchrotron radial x-ray diffraction(RXRD)in a diamond anvil cell(DAC).It is found that all diffraction peaks of molybdenum undergo ...We have studied the high-pressure compression behavior of molybdenum up to 60 GPa by synchrotron radial x-ray diffraction(RXRD)in a diamond anvil cell(DAC).It is found that all diffraction peaks of molybdenum undergo a split at around 27 GPa,and we believe that a phase transition from a body-centered cubic structure to a rhombohedral structure at room pressure has occurred.The slope of pressure–volume curve shows continuity before and after this phase transition,when fitting the pressure–volume curves of the body-centered cubic structure at low pressure and the rhombohedral structure at high pressure.A bulk modulus of 261.3(2.7)GPa and a first-order derivative of the bulk modulus of 4.15(0.14)are obtained by using the nonhydrostatic compression data at the angleψ=54.7°between the diffracting plane normal and stress axis.展开更多
Tantalum nitride (TAN) compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature (HPHT) method. The crystal structure and atom occupations of WC-type TaN have been investigated...Tantalum nitride (TAN) compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature (HPHT) method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure- volume (P-V) sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B0 = 369(2) GPa with pressure derivatives of B~ = 4 for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result (Bo = 351 GPa), which is close to the recent theoretical calculation result (Bo = 378 GPa). An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta-N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.展开更多
Fe3O4(magnetite), a-Fe2O3(hematite), and Fe O(wu¨ stite) are the three major iron oxides and some of the most fundamental solids in nature. Interest in these systems is due to their abundance as minerals in the E...Fe3O4(magnetite), a-Fe2O3(hematite), and Fe O(wu¨ stite) are the three major iron oxides and some of the most fundamental solids in nature. Interest in these systems is due to their abundance as minerals in the Earth and other telluric planets as well as their interesting electronic and magnetic properties which have been studied for decades. In this article, we review high-pressure studies on these three systems using neutron powder diffraction in the0–14 GPa range with a particular focus on the behavior of magnetism under pressure. Unpublished data on the pressure dependence of the Ne′el temperature in Fe O are presented. This review will give at the same time an introduction into technical aspects and illustrate the potential of high-pressure neutron scattering in the future.展开更多
基金Supported by the National Key Research and Development Program of China under Grant No 2016YFA0401503the Science Challenge Project under Grant No TZ2016001the National Natural Science Foundation of China under Grant No 11427810
文摘Neutron diffraction techniques of large-volume samples at high pressure using compact opposed-anvil cells are developed at a reactor neutron source, China's Mianyang research reactor. We achieve a high-pressure condition of in situ neutron diffraction by means of a newly designed large-volume opposed-anvil cell. This pressure calibration is based on resistance measurements of bismuth and the neutron diffraction of iron. Pressure calibration experiments are performed at room temperature for a new cell using the tungsten carbide anvils with a tapered angle of 30°, Φ4.5 mm culet diameter and the metal-nonmetal composite gasket with a thickness of 2 mm. Transitions in Bi(Ⅰ–Ⅱ 2.55 GPa, Ⅱ–V 7.7 GPa) are observed at 100 and 300 kN, respectively, by resistance measurements.The pressure measurement results of neutron diffraction are consistent with resistance measurements of bismuth.As a result, pressures up to about 7.7 GPa can routinely and stably be achieved using this apparatus, with the sample volume of 9 mm^3.
基金Project supported by the National Natural Science Foundation of China(Grant Nos.10875142,11079040,and 11075175)The 4W2 beamline of BSRF was supported by the Chinese Academy of Sciences(Grant Nos.KJCX2-SW-N20,KJCX2-SW-N03,and SYGNS04)
文摘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.
基金Project supported by the National Natural Science Foundation of China(Grant No.12075163)the Open fund project of Industrial Technology Institute of Sichuan University of Arts and Science,China(Grant No.ZNZZ2101)+1 种基金the Project of Ph.D special research of Sichuan University of Arts and Science,China(Grant No.2019BS006Z)supported by the Chinese Academy of Sciences(Grant Nos.KJCX2-SW-N03 and KJCX2-SW-N20)。
文摘We have studied the high-pressure compression behavior of molybdenum up to 60 GPa by synchrotron radial x-ray diffraction(RXRD)in a diamond anvil cell(DAC).It is found that all diffraction peaks of molybdenum undergo a split at around 27 GPa,and we believe that a phase transition from a body-centered cubic structure to a rhombohedral structure at room pressure has occurred.The slope of pressure–volume curve shows continuity before and after this phase transition,when fitting the pressure–volume curves of the body-centered cubic structure at low pressure and the rhombohedral structure at high pressure.A bulk modulus of 261.3(2.7)GPa and a first-order derivative of the bulk modulus of 4.15(0.14)are obtained by using the nonhydrostatic compression data at the angleψ=54.7°between the diffracting plane normal and stress axis.
基金Project supported by the Research Foundation of Key Laboratory of Neutron Physics(Grant No.2015BB03)the National Natural Science Foundation of China(Grant Nos.11774247)+2 种基金the Science Foundation for Excellent Youth Scholars of Sichuan University(Grant No.2015SCU04A04)the Joint Usage/Research Center PRIUS(Ehime University,Japan)Chinese Academy of Sciences(Grant No.2017-BEPC-PT-000568)
文摘Tantalum nitride (TAN) compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature (HPHT) method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure- volume (P-V) sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B0 = 369(2) GPa with pressure derivatives of B~ = 4 for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result (Bo = 351 GPa), which is close to the recent theoretical calculation result (Bo = 378 GPa). An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta-N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.
文摘Fe3O4(magnetite), a-Fe2O3(hematite), and Fe O(wu¨ stite) are the three major iron oxides and some of the most fundamental solids in nature. Interest in these systems is due to their abundance as minerals in the Earth and other telluric planets as well as their interesting electronic and magnetic properties which have been studied for decades. In this article, we review high-pressure studies on these three systems using neutron powder diffraction in the0–14 GPa range with a particular focus on the behavior of magnetism under pressure. Unpublished data on the pressure dependence of the Ne′el temperature in Fe O are presented. This review will give at the same time an introduction into technical aspects and illustrate the potential of high-pressure neutron scattering in the future.