A thermal-gradient approach to variable-temperature measurements resolved in space.

Autor: O'Nolan D; Department of Chemistry, Stony Brook University, 100 Nicolls Road, Stony Brook, New York 11794, USA., Huang G; Department of Materials Science and Engineering, University of Michigan, Ann Arbor, Michigan 48109, USA., Kamm GE; Department of Chemistry, Stony Brook University, 100 Nicolls Road, Stony Brook, New York 11794, USA., Grenier A; Department of Chemistry, Stony Brook University, 100 Nicolls Road, Stony Brook, New York 11794, USA., Liu CH; Department of Materials Science and Engineering, Columbia University, New York, New York 10027, USA., Todd PK; Department of Chemistry, Colorado State University, Fort Collins, Colorado 80523, USA., Wustrow A; Department of Chemistry, Colorado State University, Fort Collins, Colorado 80523, USA., Thinh Tran G; Department of Chemistry, Colorado State University, Fort Collins, Colorado 80523, USA., Montiel D; Department of Materials Science and Engineering, University of Michigan, Ann Arbor, Michigan 48109, USA., Neilson JR; Department of Chemistry, Colorado State University, Fort Collins, Colorado 80523, USA., Billinge SJL; Department of Materials Science and Engineering, Columbia University, New York, New York 10027, USA., Chupas PJ; Department of Chemistry, Stony Brook University, 100 Nicolls Road, Stony Brook, New York 11794, USA., Thornton KS; Department of Materials Science and Engineering, University of Michigan, Ann Arbor, Michigan 48109, USA., Chapman KW; Department of Chemistry, Stony Brook University, 100 Nicolls Road, Stony Brook, New York 11794, USA.
Jazyk: angličtina
Zdroj: Journal of applied crystallography [J Appl Crystallogr] 2020 Apr 23; Vol. 53 (Pt 3), pp. 662-670. Date of Electronic Publication: 2020 Apr 23 (Print Publication: 2020).
DOI: 10.1107/S160057672000415X
Abstrakt: Temperature is a ubiquitous environmental variable used to explore materials structure, properties and reactivity. This article reports a new paradigm for variable-temperature measurements that varies the temperature continuously across a sample such that temperature is measured as a function of sample position and not time. The gradient approach offers advantages over conventional variable-temperature studies, in which temperature is scanned during a series measurement, in that it improves the efficiency with which a series of temperatures can be probed and it allows the sample evolution at multiple temperatures to be measured in parallel to resolve kinetic and thermodynamic effects. Applied to treat samples at a continuum of tem-peratures prior to measurements at ambient temperature, the gradient approach enables parametric studies of recovered systems, eliminating temperature-dependent structural and chemical variations to simplify interpretation of the data. The implementation of spatially resolved variable-temperature measurements presented here is based on a gradient-heater design that uses a 3D-printed ceramic template to guide the variable pitch of the wire in a resistively heated wire-wound heater element. The configuration of the gradient heater was refined on the basis of thermal modelling. Applications of the gradient heater to quantify thermal-expansion behaviour, to map metastable polymorphs recovered to ambient temperature, and to monitor the time- and temperature-dependent phase evolution in a complex solid-state reaction are demonstrated.
(© International Union of Crystallography 2020.)
Databáze: MEDLINE
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