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Title: Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

Abstract

Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-delta crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that ismore » of interest for magnetocaloric applications.« less

Authors:
ORCiD logo [1];  [2];  [3];  [1];  [4];  [3];  [5];  [1];  [3]
  1. Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA
  2. Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Laboratory of Mathematics, Physics and Electrical Engineering, Halmstad University, P.O. Box 823, SE-301 18 Halmstad, Sweden
  3. Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden
  4. Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA
  5. X-ray Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
Swiss National Science Foundation (SNSF); Swedish Research Council (SRC); USDOE; USDOE Office of Science - Office of Basic Energy Sciences - Materials Sciences and Engineering Division
OSTI Identifier:
1419952
DOE Contract Number:
AC02-06CH11357
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 88; Journal Issue: 12
Country of Publication:
United States
Language:
English

Citation Formats

Willa, K., Diao, Z., Campanini, D., Welp, U., Divan, R., Hudl, M., Islam, Z., Kwok, W. -K., and Rydh, A. Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature. United States: N. p., 2017. Web. doi:10.1063/1.5016592.
Willa, K., Diao, Z., Campanini, D., Welp, U., Divan, R., Hudl, M., Islam, Z., Kwok, W. -K., & Rydh, A. Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature. United States. doi:10.1063/1.5016592.
Willa, K., Diao, Z., Campanini, D., Welp, U., Divan, R., Hudl, M., Islam, Z., Kwok, W. -K., and Rydh, A. 2017. "Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature". United States. doi:10.1063/1.5016592.
@article{osti_1419952,
title = {Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature},
author = {Willa, K. and Diao, Z. and Campanini, D. and Welp, U. and Divan, R. and Hudl, M. and Islam, Z. and Kwok, W. -K. and Rydh, A.},
abstractNote = {Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-delta crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.},
doi = {10.1063/1.5016592},
journal = {Review of Scientific Instruments},
number = 12,
volume = 88,
place = {United States},
year = 2017,
month =
}
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  • Gadolinium aluminates, GdAlO{sub 3}, Gd{sub 3}Al{sub 5}O{sub 12} and Gd{sub 4}Al{sub 2}O{sub 9} were synthesized by the solution combustion method. Very fine particles in the nanoparticle range of {approx}10-20 nm could be prepared by this method as evidenced by surface area measurement by multipoint BET method. Thermal studies on these compounds were carried out using high-temperature X-ray diffraction (HT-XRD) and differential scanning calorimetry (DSC) methods. The thermal expansion coefficients of GdAlO{sub 3}, Gd{sub 3}Al{sub 5}O{sub 12} and Gd{sub 4}Al{sub 2}O{sub 9} were calculated from the lattice parameter data and specific heats were calculated from DSC data. The lattice parameters ofmore » GdAlO{sub 3} and Gd{sub 3}Al{sub 5}O{sub 12} were found to increase linearly with temperature whereas Gd{sub 4}Al{sub 2}O{sub 9} did not show a linear trend. The specific heats of these compounds show an increasing trend with increase in aluminum atom fraction. Based on the thermodynamic data available in the literature and the specific heat data obtained in this study, oxygen potential diagram was constructed at 1000 K. - Graphical abstract: Isothermal oxygen potential diagram for the system Gd-Al-O at 1000 K.« less
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