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-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 ismore »
- Authors:
-
- Argonne National Lab. (ANL), Argonne, IL (United States)
- Stockholm Univ., Stockholm (Sweden); Halmstad Univ., Halmstad (Sweden)
- Stockholm Univ., Stockholm (Sweden)
- 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 (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division
- OSTI Identifier:
- 1419952
- Alternate Identifier(s):
- OSTI ID: 1413007
- Grant/Contract Number:
- AC02-06CH11357
- Resource 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)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 47 OTHER INSTRUMENTATION
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. https://doi.org/10.1063/1.5016592
Willa, K., Diao, Z., Campanini, D., Welp, U., Divan, R., Hudl, M., Islam, Z., Kwok, W. -K., and Rydh, A. Tue .
"Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature". United States. https://doi.org/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 = {Tue Dec 12 00:00:00 EST 2017},
month = {Tue Dec 12 00:00:00 EST 2017}
}
Web of Science
Works referenced in this record:
Striped superconductors: how spin, charge and superconducting orders intertwine in the cuprates
journal, November 2009
- Berg, Erez; Fradkin, Eduardo; Kivelson, Steven A.
- New Journal of Physics, Vol. 11, Issue 11
Structure of versus temperature by x-ray-absorption spectroscopy
journal, December 1987
- Crozier, E. D.; Alberding, N.; Bauchspiess, K. R.
- Physical Review B, Vol. 36, Issue 16
Melting and reorganization of poly(ethylene terephthalate) on fast heating (1000 K/s)
journal, May 2004
- Minakov, Alexander A.; Mordvintsev, Dmitry A.; Schick, Christoph
- Polymer, Vol. 45, Issue 11
Transition-metal-based magnetic refrigerants for room-temperature applications
journal, January 2002
- Tegus, O.; Brück, E.; Buschow, K. H. J.
- Nature, Vol. 415, Issue 6868
Ideal charge-density-wave order in the high-field state of superconducting YBCO
journal, December 2016
- Jang, H.; Lee, W. -S.; Nojiri, H.
- Proceedings of the National Academy of Sciences, Vol. 113, Issue 51
Structural properties of CuO/TiO2 nanorod in relation to their catalytic activity for simultaneous hydrogen production under solar light
journal, December 2013
- Khemthong, Pongtanawat; Photai, Pairat; Grisdanurak, Nurak
- International Journal of Hydrogen Energy, Vol. 38, Issue 36
In situ observation of transformation pathways of polymorphic forms of 1,3-dipalmitoyl-2-oleoyl glycerol (POP) examined with synchrotron radiation X-ray diffraction and DSC
journal, January 2013
- Bayés-García, Laura; Calvet, Teresa; Àngel Cuevas-Diarte, Miquel
- CrystEngComm, Vol. 15, Issue 2
Collective Dynamics in Water by High Energy Resolution Inelastic X-Ray Scattering
journal, July 1995
- Sette, F.; Ruocco, G.; Krisch, M.
- Physical Review Letters, Vol. 75, Issue 5
Three-dimensional charge density wave order in YBa2Cu3O6.67 at high magnetic fields
journal, November 2015
- Gerber, S.; Jang, H.; Nojiri, H.
- Science, Vol. 350, Issue 6263
High-resolution thermal imaging with a combination of nano-focus X-ray diffraction and ultra-fast chip calorimetry
journal, November 2013
- Rosenthal, Martin; Doblas, David; Hernandez, Jaime J.
- Journal of Synchrotron Radiation, Vol. 21, Issue 1
Hermetic sample enclosure for simultaneous differential scanning calorimetry/synchrotron powder x-ray diffraction
journal, May 1999
- Lexa, Dusan
- Review of Scientific Instruments, Vol. 70, Issue 5
Absorption of circularly polarized x rays in iron
journal, February 1987
- Schütz, G.; Wagner, W.; Wilhelm, W.
- Physical Review Letters, Vol. 58, Issue 7
Elimination of self-absorption in fluorescence hard-x-ray absorption spectra
journal, October 1999
- Pfalzer, P.; Urbach, J. -P.; Klemm, M.
- Physical Review B, Vol. 60, Issue 13
Mixed Magnetism for Refrigeration and Energy Conversion
journal, September 2011
- Dung, Nguyen H.; Ou, Zhi Qiang; Caron, Luana
- Advanced Energy Materials, Vol. 1, Issue 6
Combining X-ray scattering with dielectric and calorimetric experiments for monitoring polymer crystallization
journal, November 2009
- Wurm, Andreas; Minakov, Alexander A.; Schick, Christoph
- European Polymer Journal, Vol. 45, Issue 11
Thin-film alternating current nanocalorimeter for low temperatures and high magnetic fields
journal, April 2005
- Minakov, A. A.; Roy, S. B.; Bugoslavsky, Y. V.
- Review of Scientific Instruments, Vol. 76, Issue 4
High‐speed (10 4 °C/s) scanning microcalorimetry with monolayer sensitivity (J/m 2 )
journal, August 1995
- Lai, S. L.; Ramanath, G.; Allen, L. H.
- Applied Physics Letters, Vol. 67, Issue 9
Single-crystal X-ray diffraction and resonant X-ray magnetic scattering at helium-3 temperatures in high magnetic fields at beamline P09 at PETRA III
journal, August 2015
- Francoual, S.; Strempfer, J.; Warren, J.
- Journal of Synchrotron Radiation, Vol. 22, Issue 5
Differential membrane-based nanocalorimeter for high-resolution measurements of low-temperature specific heat
journal, May 2012
- Tagliati, S.; Krasnov, V. M.; Rydh, A.
- Review of Scientific Instruments, Vol. 83, Issue 5
Thermodynamic signature of a magnetic-field-driven phase transition within the superconducting state of an underdoped cuprate
journal, October 2015
- Kemper, J. B.; Vafek, O.; Betts, J. B.
- Nature Physics, Vol. 12, Issue 1
The beam-heating effect in simultaneous differential scanning calorimetry/synchrotron powder X-ray diffraction
journal, May 2003
- Lexa, Dusan; Jeremy Kropf, A.
- Thermochimica Acta, Vol. 401, Issue 2
Gap symmetry and structure of Fe-based superconductors
journal, October 2011
- Hirschfeld, P. J.; Korshunov, M. M.; Mazin, I. I.
- Reports on Progress in Physics, Vol. 74, Issue 12
Simultaneous differential scanning calorimetry and small-angle x-ray scattering
journal, June 1985
- Russell, T. P.; Koberstein, J. T.
- Journal of Polymer Science: Polymer Physics Edition, Vol. 23, Issue 6
First Order Magnetic Phase Transition in Fe 2 P
journal, January 1978
- Lundgren, Leif; Tarmohamed, Gulzar; Beckman, Olof
- Physica Scripta, Vol. 17, Issue 1
Nanogram calorimetry using microscale suspended SiN x platforms fabricated via focused ion beam patterning
journal, January 2015
- Wickey, K. J.; Chilcote, M.; Johnston-Halperin, E.
- Review of Scientific Instruments, Vol. 86, Issue 1
Re-exploring the double-melting behavior of semirigid-chain polymers with an in-situ combination of synchrotron nano-focus X-ray scattering and nanocalorimetry
journal, August 2016
- Melnikov, A. P.; Rosenthal, M.; Rodygin, A. I.
- European Polymer Journal, Vol. 81
Steady-State, ac-Temperature Calorimetry
journal, September 1968
- Sullivan, Paul F.; Seidel, G.
- Physical Review, Vol. 173, Issue 3
Thermodynamics around the first-order ferromagnetic phase transition of single crystals
journal, October 2014
- Hudl, M.; Campanini, D.; Caron, L.
- Physical Review B, Vol. 90, Issue 14
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
Simultaneous Differential Scanning Calorimetry-Synchrotron X-ray Powder Diffraction: A Powerful Technique for Physical Form Characterization in Pharmaceutical Materials
journal, September 2016
- Clout, Alexander; Buanz, Asma B. M.; Prior, Timothy J.
- Analytical Chemistry, Vol. 88, Issue 20
In-situ X-ray diffraction combined with scanning AC nanocalorimetry applied to a Fe 0.84 Ni 0.16 thin-film sample
journal, May 2013
- Gregoire, John M.; Xiao, Kechao; McCluskey, Patrick J.
- Applied Physics Letters, Vol. 102, Issue 20
Specific heat measurement set-up for quench condensed thin superconducting films
journal, May 2014
- Poran, Shachaf; Molina-Ruiz, Manel; Gérardin, Anne
- Review of Scientific Instruments, Vol. 85, Issue 5
Simulated sample heating from a nanofocused X-ray beam
journal, August 2017
- Wallander, Harald; Wallentin, Jesper
- Journal of Synchrotron Radiation, Vol. 24, Issue 5
Copper K-edge XANES of Cu(I) and Cu(II) oxide mixtures
journal, November 2009
- Gaur, A.; Shrivastava, B. D.; Joshi, S. K.
- Journal of Physics: Conference Series, Vol. 190
Resonant X-Ray Scattering Studies of Charge Order in Cuprates
journal, March 2016
- Comin, Riccardo; Damascelli, Andrea
- Annual Review of Condensed Matter Physics, Vol. 7, Issue 1
Simultaneous X-Ray Diffraction and Differential Scanning Calorimetry (XDDSC) in Studies of Molecular and Liquid Crystals
journal, March 1990
- Ungar, G.; Feijoo, J. L.
- Molecular Crystals and Liquid Crystals Incorporating Nonlinear Optics, Vol. 180, Issue 2
The Combination of Thermal Analysis and Time-Resolved X-ray Techniques: a Powerful Method for Materials Characterization
journal, February 1995
- Bras, W.; Derbyshire, G. E.; Devine, A.
- Journal of Applied Crystallography, Vol. 28, Issue 1
Polarized copper K -edge x-ray-absorption spectra in
journal, July 1990
- Guo, J.; Ellis, D. E.; Alp, E. E.
- Physical Review B, Vol. 42, Issue 1
Magnetocrystalline anisotropy and the magnetocaloric effect in Fe P
journal, September 2013
- Caron, L.; Hudl, M.; Höglin, V.
- Physical Review B, Vol. 88, Issue 9
Simultaneous Synchrotron WAXD and Fast Scanning (Chip) Calorimetry: On the (Isothermal) Crystallization of HDPE and PA11 at High Supercoolings and Cooling Rates up to 200 °C s −1
journal, April 2015
- Baeten, Dorien; Mathot, Vincent B. F.; Pijpers, Thijs F. J.
- Macromolecular Rapid Communications, Vol. 36, Issue 12
Correlated states in β-Li2IrO3 driven by applied magnetic fields
journal, October 2017
- Ruiz, Alejandro; Frano, Alex; Breznay, Nicholas P.
- Nature Communications, Vol. 8, Issue 1
Susceptibility Anisotropy in an Iron Arsenide Superconductor Revealed by X-Ray Diffraction in Pulsed Magnetic Fields
journal, July 2012
- Ruff, J. P. C.; Chu, J. -H.; Kuo, H. -H.
- Physical Review Letters, Vol. 109, Issue 2
The puzzle of high temperature superconductivity in layered iron pnictides and chalcogenides
journal, October 2010
- Johnston, David C.
- Advances in Physics, Vol. 59, Issue 6
Scanning AC nanocalorimetry combined with in-situ x-ray diffraction
journal, June 2013
- Xiao, Kechao; Gregoire, John M.; McCluskey, Patrick J.
- Journal of Applied Physics, Vol. 113, Issue 24
Absorption of circularly polarized x rays in iron
text, January 1987
- Schütz, G.; Wagner, W.; Wilhelm, W.
- Deutsches Elektronen-Synchrotron, DESY, Hamburg
Mixed Magnetism for Refrigeration and Energy Conversion
text, January 2012
- Dung, N. H.; Ou, Z. Q.; Caron, L.
- arXiv
Magnetocrystalline Anisotropy and the Magnetocaloric Effect in Fe2P
text, January 2013
- Caron, L.; Hudl, M.; Höglin, V.
- arXiv
Resonant x-ray scattering studies of charge order in cuprates
text, January 2015
- Comin, Riccardo; Damascelli, Andrea
- arXiv
Ideal charge density wave order in the high-field state of superconducting YBCO
text, January 2016
- Jang, H.; Lee, W. -S.; Nojiri, H.
- arXiv
Works referencing / citing this record:
Phase transition preceding magnetic long-range order in the double perovskite
journal, July 2019
- Willa, Kristin; Willa, Roland; Welp, Ulrich
- Physical Review B, Vol. 100, Issue 4
Superconductivity in
journal, February 2019
- Bao, Jin-Ke; Bugaris, Daniel E.; Zheng, Huihuo
- Physical Review Materials, Vol. 3, Issue 2