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European Microscopy Congress 2016: Proceedings || Graphite-to-diamond (13C) direct transition in a diamond anvil high-pressure cell
摘要： As the hardest material in nature, diamond is of great importance and interest for scientific studies. However, formation of a diamond is complicated process and requires extreme conditions. Bundy and Kasper (1967) for the first time synthesized a new form of carbon—hexagonal diamond – under conditions of static pressure exceeding about 13 GPa and temperature greater than about 1000°C [1]. At room temperature the crystal structure of graphite is stable up to pressure 15 GPa and loses some of the graphite features at higher pressure, forming metastable graphitic or amorphous phases [2]. Transition of polycrystalline graphite to diamond occurs after hydrostatic pressure treatment near 70 GPa [3]. The development of solid-state phase transitions, including those at the stage of nucleation and development of a new phase practically always is connected with the relaxation of elastic stress [4], and in case of graphite-diamond transformation the latter can play main role. The goal of the present work is the formation of diamond from graphite in direct phase transition in a diamond anvil high-pressure cell, where the relaxation of elastic stress can be realized by means of plastic deformation of the sample. The experiment was performed at room temperature without a catalyst.13С was subjected to the shear deformation under pressure of 25 GPa. The structure studies of the obtained material were made by transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). In order to prevent the confusion of the diamond obtained in the experiment with one of the diamond anvils we used graphite composed of 13C carbon isotope atoms as a precursor. The diamond anvils consisted of conventional 12C diamond. Before TEM examination of each sample a Raman spectroscopy was used to verify that it contains only 13 C (diamond) and no 12C. TEM and EELS were carried out using JEOL JEM-2010 high-resolution transmission electron microscope. TEM analysis has shown that the samples obtained in the series of our experiments contain several phases of carbon simultaneously. After the high pressure treatment in shear diamond anvil cell (SDAC) there were observed some fragments of the sample, which contained both hexagonal and rhombohedral graphite (significant amounts of the last one), and also diamond and lonsdaleite. Fig. 1 shows the fragment, where the rhombohedral graphite presents. Fig. 2a shows the diamond structure fragment with {111}-planes composing 70o. Interplanar distances are 0.206 nm. Fig. 2b shows the EELS-spectrum which can be unambiguously attributed to a diamond. Thus, it was shown that 13С-graphite directly transforms into 13С-diamond (at least particularly) without a catalyst at room temperature after treatment in SDAC under pressure of 25 GPa.
关键词： EELS,high pressure,shear diamond anvil cell,HRTEM
更新于2025-09-23 15:23:52
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An exploration of surface enhanced Raman spectroscopy (SERS) for in situ detection of sulfite under high pressure
摘要： In this work, silver nanoparticles film was directly fabricated on the surface of the diamond anvil as SERS active substrate for the first time by using a simple and convenient method. With this approach, the SERS spectrum of sulfite was obtained with a detection limit of 5 μmol/L in diamond anvil cell (DAC) at ～50 MPa. The SERS signal intensity of the two main vibration modes, νsymSeO and δsymOeSeO, showed good linearity with the Na2SO3 concentrations in the range from 5 to 40 μmol/L under high pressure. The linear correlation coefficients were 97.67% and 96.08%, respectively. The effects of pressure on the SERS intensity and Raman shift of the two modes were also studied. The SERS intensity dropped with the increase of pressure and the two main vibration modes shifted to high wave-number when the pressure increased in the pressures ranging from 54 MPa to 330 MPa. The experiments indicate that this method is rapid, convenient and sensitive in detecting sulfite at high pressures. It can be developed as an effect in situ method to detect sulfite in the process of high pressure reaction.
关键词： SERS,In situ,High pressure,Diamond-anvil cell,Sulfite
更新于2025-09-23 15:23:52
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Simple imaging for the diamond anvil cell: Applications to hard-to-reach places
摘要： The employment of high-pressure gases as a pressure-transmitting medium, sample, or reactant for diamond anvil cell experiments is widespread. As a pressure transmitter, high-pressure gases are crucial to forming quasi-hydrostatic compression atmospheres for samples inside the uniaxially driven cell. We describe an optical design for forming high-resolution images of the gasket and sample chamber of the diamond anvil cell under high gas pressures in a gas loading apparatus. Our design is simple, is of low-cost, and may be easily adapted to suit gas loading apparatus of any design, as well as other common hard-to-reach environments in diamond anvil cell experiments, i.e., those with large stand-off distances, such as cryostats.
关键词： optical design,high-pressure gases,gas loading apparatus,diamond anvil cell,imaging
更新于2025-09-23 15:21:21
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Temperature measurement in double-sided laser-heated diamond anvil cell and reaction of carbon
摘要： In this work, a double-sided laser-heated diamond anvil cell facility for studies at extreme conditions of pressure and temperature that has been developed is described in detail. Phase transitions occurring at extreme conditions can be mapped by accurate measurements of pressure and temperature. Micrometer-sized diamond crystals having regular facets have been synthesized at a pressure of 18 GPa and temperature 1785 K, which is con?rmed by visual inspection, micro-Raman and ?eld emission scanning electron micrograph measurements. A low-temperature gradient is observed across the sample surface during the formation of micrometer-sized diamond crystals. Our observation restricts the use of steel gasket as it can react with carbon (C) transported from the diamond anvil. The reaction of C with one of the potential thermal insulating medium Al2O3 is observed in the X-ray diffraction measurements.
关键词： Laser-heated diamond anvil cell,High pressure,Reaction of carbon
更新于2025-09-23 15:19:57
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Table-top nuclear magnetic resonance system for high-pressure studies with <i>in situ</i> laser heating
摘要： High pressure Nuclear Magnetic Resonance (NMR) is known to reveal the behavior of matter under extreme conditions. However, until now, significant maintenance demands, space requirements, and high costs of superconducting magnets render its application unfeasible for regular modern high pressure laboratories. Here, we present a table-top NMR system based on permanent Halbach magnet arrays with a diameter of 25 cm and height of 4 cm. At the highest field of 1013 mT, 1H-NMR spectra of ice VII have been recorded at 25 GPa and ambient temperature. The table-top NMR system can be used together with double sided laser heating setups. Feasibility of high-pressure high-temperature NMR was demonstrated by collecting 1H-NMR spectra of H2O at 25 GPa and 1063(50) K. The change in the signal intensity in a laser-heated NMR diamond anvil cell has been found to yield a convenient way for temperature measurements.
关键词： diamond anvil cell,laser heating,Halbach magnet,Nuclear Magnetic Resonance,high-pressure
更新于2025-09-16 10:30:52
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Laser heating setup for diamond anvil cells for <i>in situ</i> synchrotron and in house high and ultra-high pressure studies
摘要： The diamond anvil cell (DAC) technique combined with laser heating is one of the major methods for studying materials at high pressure and high temperature conditions. In this work, we present a transferable double-sided laser heating setup for DACs with in situ temperature determination. The setup allows precise heating of samples inside a DAC at pressures above 200 GPa and could be combined with synchrotron beamline equipment. It can be applied to X-ray diffraction and X-ray transmission microscopy experiments. In the setup, we use high-magnification and low working distance infinity corrected laser focusing objectives that enable us to decrease the size of the laser beam to less than 5 μm and achieve the maximum optical magnification of 320 times. All optical components of the setup were chosen to minimize chromatic and spatial aberrations for accurate in situ temperature determination by multiwavelength spectroscopy in the 570–830 nm spectral range. Flexible design of our setup allows simple interchange of laser sources and focusing optics for application in different types of studies. The setup was successfully tested in house and at the high-pressure diffraction beamline ID15B at the European Synchrotron Radiation Facility. We demonstrate an example of application of the setup for the high pressure–high temperature powder diffraction study of PdH and X-ray transmission microscopy of platinum at 22(1) GPa as a novel method of melting detection in DACs.
关键词： high pressure,diamond anvil cell,X-ray transmission microscopy,X-ray diffraction,synchrotron,laser heating,high temperature
更新于2025-09-16 10:30:52
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Raman spectroscopy of poly (methyl methacrylate) under laser shock and static compression
摘要： Time-resolved Raman spectroscopy for visualizing molecular fingerprint snapshots at nanosecond time scale is a useful tool for detailed understanding of in situ shock behaviour of materials. This technique was applied to study the changes in molecular vibrations of poly (methyl methacrylate) (PMMA) under laser driven shock compression up to ~1.9 GPa in a confinement geometry. A layered target configuration is used to enhance the shock pressure. The vibrational modes are measured as a function of dynamic shock and static compression. The Grüneisen parameters and bond anharmonicities in PMMA are determined using compression behaviour of Raman modes. The deduced shock velocity (~3.5 ± 0.4 km/s) in PMMA based on the time evolution of shocked Raman mode at 1.9 GPa is in agreement with the one calculated (~3.7 km/s) from 1-D radiation hydrodynamic simulations. A comparative study on shock experiment and static high pressure Raman spectroscopic measurements is done. Static pressure measurement up to ~16 GPa show rapid blue shifting of C–H stretching modes.
关键词： Raman spectroscopy,PMMA,confinement geometry,Raman shift,laser shock,diamond anvil cell (DAC),static experiment
更新于2025-09-16 10:30:52