Structural Studies of Boron Nitride Compounds Under Extreme Conditions

Title: Structural Studies of Boron Nitride Compounds Under Extreme Conditions
Authors: Sterling, Spencer
Date: 2021-10-27
Abstract: This document will present the work done on BN under high pressure conditions, both at room temperatures and at high temperatures under laser heating conditions. These experiments are performed to identify possible phase transitions within the BN system and characterize the materials present under the given conditions using a mixture of X-ray diffraction and Raman and infrared spectroscopies are employed. A review of the background and motivations for studies of BN under extreme conditions, as well as the techniques employed, is given as an introduction. A phase transition from hexagonal boron nitride (hBN) to wurtzite boron nitride (wBN) is observed beginning at 9 GPa and room temperature, with coexistence of the two phases until 14 GPa for hydrostatic conditions and to above 20 GPa for non-hydrostatic conditions. This transition is partially reversible below 2 GPa. The formed wBN has a high concentration of defects. For recovered samples, defects couple with the 532.18 nm excitation laser producing a heating effect, observed as a Raman downshift with increasing laser power. The bulk modulus B0 and pressure derivative of the bulk modulus B0′ of hBN are estimated to be 30.6 ± 0.5 GPa and 8.7 ± 0.7, respectively. The bulk modulus of wBN is estimated to be 392 ± 5 GPa, leading to a Vickers hardness of 68 ± 1 GPa. Extra diffraction lines are observed for hBN samples loaded with N2, indicating a potential new structure arising from a reaction of N2 with hBN, but Raman spectroscopy fails to corroborate this finding. The crystallinity of the hBN samples and the choice of pressure transmitting medium are shown to have little to no effect on the estimated physical properties of hBN. Laser heating is performed on hBN with various sample assemblies. The effectiveness of different assemblies is discussed. NaCl is used as a pressure and temperature gauge local to the X-ray probe to contrast the stationary ruby pressure gauge and the non-local black body temperature measurement. A large contrast between the two temperature measurements yields doubt that the intended temperatures of around 2000 K are produced in the sample. Observation of the proposed high-pressure high-temperature transition to body-centered tetragonal BN or intercalated BN cannot be confirmed, likely due to insufficient heating. The prospects for studying Li-BN intercalation compounds under extreme conditions is discussed. An initial experiment on the system studied with X-ray diffraction is unable to confirm heating of the material nor the presence of intercalation compounds.
CollectionThèses, 2011 - // Theses, 2011 -

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