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

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 YBa 2Cu 3O 7-δ 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. Lastly, 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 Fe 2P,more » a material that is of interest for magnetocaloric applications.« less
Authors:
ORCiD logo [1] ;  [2] ;  [3] ;  [1] ;  [1] ;  [3] ;  [1] ;  [1] ;  [3]
  1. Argonne National Lab. (ANL), Argonne, IL (United States)
  2. Stockholm Univ., Stockholm (Sweden); Halmstad Univ., Halmstad (Sweden)
  3. Stockholm Univ., Stockholm (Sweden)
Publication Date:
Grant/Contract Number:
AC02-06CH11357
Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 88; Journal Issue: 12; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
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 (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION
OSTI Identifier:
1419952
Alternate Identifier(s):
OSTI ID: 1413007

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., 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. https://www.osti.gov/servlets/purl/1419952.
@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-δ 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. Lastly, 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 = {12}
}

Works referenced in this record:

Thin film microcalorimeter for heat capacity measurements from 1.5 to 800 K
journal, April 1994
  • Denlinger, D. W.; Abarra, E. N.; Allen, Kimberly
  • Review of Scientific Instruments, Vol. 65, Issue 4, p. 946-959
  • DOI: 10.1063/1.1144925