Spray-loading: A cryogenic deposition method for diamond anvil cell

Abstract

An efficient loading technique has been developed for flammable, toxic, or explosive gases which can be condensed at liquid nitrogen temperature and ambient pressure in membrane diamond anvil cells (DACs). This cryogenic technique consists in a deposition of small quantities of the desired gas directly into the sample chamber. The deposition is performed using a capillary that reaches the space between the diamond anvils. The DAC is kept under inert gas overpressure during the whole process, in order to avoid contamination from atmospheric O, CO, and HO. This technique provides significant advantages over standard cryo-loading and gas-loading when the condensation of dangerous samples at liquid nitrogen temperature raises safety concerns because it allows dealing with minimum quantities of condensed gases. The whole procedure is particularly fast and efficient. The "spray-loading" has been successfully used in our laboratory to load several samples including acetylene, ammonia, ethylene, and carbon dioxide/water or red phosphorus/NH mixtures.

Novel Calcium sp3 Carbonate CaC2O5-I4̅2d May Be a Carbon Host in Earth’s Lower Mantle

“…The phase purity of the calcite crystals was verified by Raman spectroscopy after heating the samples for 24 h at 120 °C in an oven. CO 2 dry ice was subsequently precipitated into the sample chambers using a custom-built cryogenic loading system built upon an earlier concept …”

“…CO 2 dry ice was subsequently precipitated into the sample chambers using a custom-built cryogenic loading system built upon an earlier concept. 35 Raman Spectroscopy in the Laser-Heated DAC. Highpressure Raman spectroscopy was carried out before and after heating the calcite samples using the double-sided CO 2 -laser heating and Raman system at the Institute of Geosciences at the Goethe Universitaẗ Frankfurt following an earlier routine of the same setup.…”

High-Pressure Synthesis of Cyclic Phosphazenes by Near-UV Photoinduced Reactivity of NH3 and Elemental Phosphorus

“…Amorphous P red powder (from Aldrich, 99.99+% purity) was first loaded in the gasket hole, which was then filled with NH 3 . The black phosphorus sample was prepared by pressurizing P red at ambient temperature above 6.6 GPa. − Gaseous NH 3 was condensed directly between the diamonds, into the gasket hole, by means of the spray-loading technique . The pressure was measured by the ruby fluorescence method. , Reactivity was triggered by focusing the UV multiline emission (≈350 nm) of an Ar ion laser onto the sample with a power of 500 mW in successive irradiations of variable durations (from 1 h to a maximum of 15 h per irradiation).…”

“…4−6 Gaseous NH 3 was condensed directly between the diamonds, into the gasket hole, by means of the spray-loading technique. 35 The pressure was measured by the ruby fluorescence method. 36,37 Reactivity was triggered by focusing the UV multiline emission (≈350 nm) of an Ar ion laser onto the sample with a power of 500 mW in successive irradiations of variable durations (from 1 h to a maximum of 15 h per irradiation).…”

Accessing the Activation Mechanisms of Ethylene Photo-Polymerization under Pressure by Transient Infrared Absorption Spectroscopy

“…Ethylene (99.5% from Sapio) was loaded in the sapphire anvil cell by means of the spray-loading technique. 22 The pressure of the sample was calculated using the pressure shift of a precalibrated ethylene infrared active C−H stretching band as no gauge was used to avoid light-absorbing species within the sample.…”