Optical cell for combinatorial in situ Raman spectroscopic measurements of hydrogen storage materials at high pressures and temperatures

Abstract

Articles you may be interested inAn optical cell is described for high-throughput backscattering Raman spectroscopic measurements of hydrogen storage materials at pressures up to 10 MPa and temperatures up to 823 K. High throughput is obtained by employing a 60 mm diameter × 9 mm thick sapphire window, with a corresponding 50 mm diameter unobstructed optical aperture. To reproducibly seal this relatively large window to the cell body at elevated temperatures and pressures, a gold o-ring is employed. The sample holderto-window distance is adjustable, making this cell design compatible with optical measurement systems incorporating lenses of significantly different focal lengths, e.g., microscope objectives and single element lenses. For combinatorial investigations, up to 19 individual powder samples can be loaded into the optical cell at one time. This cell design is also compatible with thin-film samples. To demonstrate the capabilities of the cell, in situ measurements of the Ca(BH 4 ) 2 and nano-LiBH 4 -LiNH 2 -MgH 2 hydrogen storage systems at elevated temperatures and pressures are reported.

Applications of high throughput (combinatorial) methodologies to electronic, magnetic, optical, and energy-related materials

“…The number of samples to be characterized from a given library can vary from 100 to 1000. [311][312][313] However, there are significant challenges to the thin film approach. For example, a phase that can be synthesized through thin film deposition techniques may not be capable of being produced in kilogram quantities using traditional bulk synthesis techniques.…”

“…In-situ high throughput spectroscopy has increasingly become a part of the array of tools used by the hydrogen storage community. 312,341,342 It has been applied to discrete powder arrays as well as to diffusion couple samples. Micro-Raman spectroscopy was used to measure the diffusion of atomic and molecular hydrogen in the borohydride cluster, 341,342 and it was demonstrated, by radioisotopic substitution, that hydrogen was transported almost exclusively by the diffusion of BH 4 À , the exchange of single hydrogen ions occurring at a rate ten orders of magnitude slower.…”

Calcium Borohydride Ca(BH4)2: Fundamentals, Prediction and Probing for High-Capacity Energy Storage Applications, Organic Synthesis and Catalysis

“…Hattrick-Simpers et al described the use of high-throughput backscattering Raman spectroscopic measurements for combinatorial in situ Raman spectroscopy of Ca(BH 4 ) 2 and other RHCs (up to 10 Mpa and 823 K) [71].…”

Generating Information-Rich High-Throughput Experimental Materials Genomes using Functional Clustering via Multitree Genetic Programming and Information Theory

“…The relationship of this property to composition may be governed by any number of chemical and physical attributes, such as phase, crystallinity, microstructure and surface composition etc. While development of HiTp materials characterization − and related analysis techniques , is an active field of research, down-selection of samples from a HiTp screen for performing characterization is generally necessary. For a given composition region, a systematic variation in a materials characterization attribute may lead to a corresponding variation in the performance metric.…”