Containment of fluid samples in the hydrothermal diamond-anvil cell without the use of metal gaskets: Performance and advantages for in situ analysis

Abstract

Metal gaskets (Re, Ir, Inconel, or stainless steel) normally used to contain fluid samples in the hydrothermal diamond-anvil cell (HDAC) are sometimes undesirable due to possible contamination and to gasket deformation at high pressures and temperatures resulting in nonisochoric behavior. Furthermore, in x-ray spectroscopic experiments, metal gaskets may attenuate the incident x-ray beam and emitted fluorescence x-rays, and the interaction of scattered radiation with the gasket may produce fluorescence that interferes with the x-ray spectrum of the sample. New arrangements and procedures were tested for the operation of the HDAC without using the metal gaskets. Distilled, de-ionized water was loaded into the sample chamber, a laser-milled recess 300 ??m in diameter and ???50 ??m deep centered in the 1.0 mm face of the lower diamond anvil, and sealed by pressing the top diamond anvil face directly against the lower one without a metal gasket in between. A maximum sample pressure of 202 MPa at 617 ??C was maintained for a duration of 10 min without evidence of leakage. A small change in fluid density was observed in one experiment where the sample was held at 266 MPa at 708 ??C for 10 min. The gasketless HDAC was also employed in x-ray absorption spectroscopy experiments, where, in addition to the sample chamber in the lower diamond, two grooves were milled at a 90?? angle to each other around the sample chamber to minimize the attenuation of incident and fluorescent x rays. With a minimum distance between the sample chamber and the grooves of 80 ??m, a pressure of 76 MPa at 500 ??C was maintained for 2 h with no change in the original fluid density. ?? 2008 American Institute of Physics.