A simple and convenient pressure calibration method is developed for a newly designed portable wide-access ＇panoramic＇ cell. This cell is adapted to angle-dispersive-mode high-pressure in situ neutron diffraction of...A simple and convenient pressure calibration method is developed for a newly designed portable wide-access ＇panoramic＇ cell. This cell is adapted to angle-dispersive-mode high-pressure in situ neutron diffraction of reactor neutron sources. This pressure calibration method has established a relationship between the cell pressure and the anvil displace- ment （gasket compression） based on the fixed-point calibration technique. By employing TiZr gasket with a thickness of 3 mm and WC anvil with a culet of 4 mm diameter, the average anvil displacements are 1.31 mm and 2.22 mm for Bi phase transitions （2.55 GPa and 7.7 GPa）, and 1.85 mm for Ba phase transitions （5.5 GPa）, respectively. In this pressure range, the pressure increases quickly with decreasing gasket thickness, and undergoes a linear increase with the anvil displacement. By extrapolating the calibration curve, the cell pressure will achieve 10 GPa when the anvil displacement is around 2.5 ram.展开更多
The DIA-type Kawai cell possesses a larger volume and a quasi-hydrostatic pressure environment and has been widely used in materials’ synthesis and x-ray diffraction experiments.However, few high-pressure in situ neu...The DIA-type Kawai cell possesses a larger volume and a quasi-hydrostatic pressure environment and has been widely used in materials’ synthesis and x-ray diffraction experiments.However, few high-pressure in situ neutron diffraction experiments were performed in the DIA-type Kawai cell because there is no wide window for neutron diffraction and the second-stage anvils and guild block material attenuates the neutron signal significantly.In this work, we tentatively modified the normal DIA-type Kawai cell(MA 2-6-8) into a MA 2-8 mode by removing the six first-stage tungsten carbide anvils.As a consequence, the eight tungsten carbide anvils(Kawai cell) are directly driven by the guide blocks.The results of ex situ and in situ pressure calibration show that the cell pressure can reach 5 GPa with small truncation edge lengths(TEL) of 3 mm even at the load of 300 kN.It suggests that this MA 2-8 cell may open a new way for high-pressure and high-temperature in situ neutron diffraction.展开更多
Manipulating metal-insulator transitions in strongly correlated materials is of great importance in condensed matter physics,with implications for both fundamental science and technology.Vanadium dioxide(VO_(2)),as an...Manipulating metal-insulator transitions in strongly correlated materials is of great importance in condensed matter physics,with implications for both fundamental science and technology.Vanadium dioxide(VO_(2)),as an ideal model system,is metallic at high temperatures and shown a typical metal-insulator structural phase transition at 341 K from rutile structure to monoclinic structure.This behavior has been absorbed tons of attention for years.However,how to control this phase transition is still challenging and little studied.Here we demonstrated that to control the Ag nanonet arrays(NAs)in monoclinic VO_(2)(M)could be effective to adjust this metal-insulator transition.With the increase of Ag NAs volume fraction by reducing the template spheres size,the transition temperature(Tc)decreased from 68°C to 51°C.The mechanism of Tc decrease was revealed as:the carrier density increases through the increase of Ag NAs volume fraction,and more free electrons injected into the VO_(2)films induced greater absorption energy at the internal nanometal-semiconductor junction.These results supply a new strategy to control the metal-insulator transitions in VO_(2),which must be instructive for the other strongly correlated materials and important for applications.展开更多
Here,simultaneous in-situ calibration of pressures and temperatures was performed in a hinge-type second-stage cubic large volume press(LVP)up to 15 GPa and 1400 K by an acoustic travel-time approach.Based on the rece...Here,simultaneous in-situ calibration of pressures and temperatures was performed in a hinge-type second-stage cubic large volume press(LVP)up to 15 GPa and 1400 K by an acoustic travel-time approach.Based on the recently reported P-tSand P-T-tP-tSequations for Al2O3buffer rod,the cell pressures and temperatures in the chamber of LVP were insitu determined,in comparison with those by conventional off-line(or fixed-points)pressure calibration method and direct thermocouple measurement,respectively.It is found that the cell pressures of the LVP chamber are significantly reduced after annealing at simultaneous high pressures and high temperatures,owing to the stress relaxation as accumulate in the LVP chamber.This acoustic travel-time method is verified to be a good way for precise determination of thermal(cell)pressures at high temperature conditions,and is of great importance and necessity to conduct in-situ physical property measurements under extreme high P-T conditions,especially when the precious synchrotron x-ray/neutron diffraction beams are not available.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
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
基金supported by the National Natural Science Foundation of China(Grant Nos.91126001,11105128,and 51231002)
文摘A simple and convenient pressure calibration method is developed for a newly designed portable wide-access ＇panoramic＇ cell. This cell is adapted to angle-dispersive-mode high-pressure in situ neutron diffraction of reactor neutron sources. This pressure calibration method has established a relationship between the cell pressure and the anvil displace- ment （gasket compression） based on the fixed-point calibration technique. By employing TiZr gasket with a thickness of 3 mm and WC anvil with a culet of 4 mm diameter, the average anvil displacements are 1.31 mm and 2.22 mm for Bi phase transitions （2.55 GPa and 7.7 GPa）, and 1.85 mm for Ba phase transitions （5.5 GPa）, respectively. In this pressure range, the pressure increases quickly with decreasing gasket thickness, and undergoes a linear increase with the anvil displacement. By extrapolating the calibration curve, the cell pressure will achieve 10 GPa when the anvil displacement is around 2.5 ram.
基金Project supported by the National Natural Science Foundation of China(Grant No.11427810)the National Key Research and Development Program of China(Grant No.2016YFA0401503)the Project for Science and Technology Plan of Sichuan Province,China(Grant No.2015GZ0053)
文摘The DIA-type Kawai cell possesses a larger volume and a quasi-hydrostatic pressure environment and has been widely used in materials’ synthesis and x-ray diffraction experiments.However, few high-pressure in situ neutron diffraction experiments were performed in the DIA-type Kawai cell because there is no wide window for neutron diffraction and the second-stage anvils and guild block material attenuates the neutron signal significantly.In this work, we tentatively modified the normal DIA-type Kawai cell(MA 2-6-8) into a MA 2-8 mode by removing the six first-stage tungsten carbide anvils.As a consequence, the eight tungsten carbide anvils(Kawai cell) are directly driven by the guide blocks.The results of ex situ and in situ pressure calibration show that the cell pressure can reach 5 GPa with small truncation edge lengths(TEL) of 3 mm even at the load of 300 kN.It suggests that this MA 2-8 cell may open a new way for high-pressure and high-temperature in situ neutron diffraction.
基金Project supported by the National Natural Science Foundation of China(Grant Nos.11904299 and U1930124)the Foundation of China Academy of Engineering Physics(Grant No.2018AB02)。
文摘Manipulating metal-insulator transitions in strongly correlated materials is of great importance in condensed matter physics,with implications for both fundamental science and technology.Vanadium dioxide(VO_(2)),as an ideal model system,is metallic at high temperatures and shown a typical metal-insulator structural phase transition at 341 K from rutile structure to monoclinic structure.This behavior has been absorbed tons of attention for years.However,how to control this phase transition is still challenging and little studied.Here we demonstrated that to control the Ag nanonet arrays(NAs)in monoclinic VO_(2)(M)could be effective to adjust this metal-insulator transition.With the increase of Ag NAs volume fraction by reducing the template spheres size,the transition temperature(Tc)decreased from 68°C to 51°C.The mechanism of Tc decrease was revealed as:the carrier density increases through the increase of Ag NAs volume fraction,and more free electrons injected into the VO_(2)films induced greater absorption energy at the internal nanometal-semiconductor junction.These results supply a new strategy to control the metal-insulator transitions in VO_(2),which must be instructive for the other strongly correlated materials and important for applications.
基金supported by the National Natural Science Foundation of China(Grant Nos.12075215,11872198,and U2030110)the National Key Research and Development Program of China(Grant No.2016YFA0401503)。
文摘Here,simultaneous in-situ calibration of pressures and temperatures was performed in a hinge-type second-stage cubic large volume press(LVP)up to 15 GPa and 1400 K by an acoustic travel-time approach.Based on the recently reported P-tSand P-T-tP-tSequations for Al2O3buffer rod,the cell pressures and temperatures in the chamber of LVP were insitu determined,in comparison with those by conventional off-line(or fixed-points)pressure calibration method and direct thermocouple measurement,respectively.It is found that the cell pressures of the LVP chamber are significantly reduced after annealing at simultaneous high pressures and high temperatures,owing to the stress relaxation as accumulate in the LVP chamber.This acoustic travel-time method is verified to be a good way for precise determination of thermal(cell)pressures at high temperature conditions,and is of great importance and necessity to conduct in-situ physical property measurements under extreme high P-T conditions,especially when the precious synchrotron x-ray/neutron diffraction beams are not available.
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.
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.
