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

Willa, K.; Diao, Z.; Campanini, D.; Welp, U.; Divan, R.; Hudl, M.; Islam, Z.; Kwok, W. -K.; Rydh, A.

doi:10.1063/1.5016592

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

Journal Article · Tue Dec 12 00:00:00 EST 2017 · Review of Scientific Instruments

DOI:https://doi.org/10.1063/1.5016592· OSTI ID:1419952

^[1]; Diao, Z. ^[2]; Campanini, D. ^[3]; Welp, U. ^[1]; Divan, R. ^[1]; Hudl, M. ^[3]; Islam, Z. ^[1]; Kwok, W. -K. ^[1]; Rydh, A. ^[3]

Argonne National Lab. (ANL), Argonne, IL (United States)
Stockholm Univ., Stockholm (Sweden); Halmstad Univ., Halmstad (Sweden)
Stockholm Univ., Stockholm (Sweden)

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 YBa₂Cu₃O_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 Fe₂P, a material that is of interest for magnetocaloric applications.

View Accepted Manuscript (DOE)

View Accepted Manuscript (Publisher)

Cite

Export

Save

Research Organization:: Argonne National Lab. (ANL), Argonne, IL (United States)

Sponsoring Organization:: 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

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1419952

Alternate ID(s):: OSTI ID: 1413007

Journal Information:: Review of Scientific Instruments, Vol. 88, Issue 12; ISSN 0034-6748

Publisher:: American Institute of Physics (AIP)Copyright Statement

Country of Publication:: United States

Language:: English

Citation Metrics:

Cited by: 16 works

Citation information provided by
Web of Science

References (49)

Striped superconductors: how spin, charge and superconducting orders intertwine in the cuprates Berg, Erez; Fradkin, Eduardo; Kivelson, Steven A. New Journal of Physics, Vol. 11, Issue 11 https://doi.org/10.1088/1367-2630/11/11/115004	journal	November 2009
Structure of $Y {Ba}_{2} {Cu}_{3} O_{7 - δ}$ versus temperature by x-ray-absorption spectroscopy Crozier, E. D.; Alberding, N.; Bauchspiess, K. R. Physical Review B, Vol. 36, Issue 16 https://doi.org/10.1103/physrevb.36.8288	journal	December 1987
Melting and reorganization of poly(ethylene terephthalate) on fast heating (1000 K/s) Minakov, Alexander A.; Mordvintsev, Dmitry A.; Schick, Christoph Polymer, Vol. 45, Issue 11 https://doi.org/10.1016/j.polymer.2004.03.072	journal	May 2004
Transition-metal-based magnetic refrigerants for room-temperature applications Tegus, O.; Brück, E.; Buschow, K. H. J. Nature, Vol. 415, Issue 6868 https://doi.org/10.1038/415150a	journal	January 2002
Ideal charge-density-wave order in the high-field state of superconducting YBCO Jang, H.; Lee, W. -S.; Nojiri, H. Proceedings of the National Academy of Sciences, Vol. 113, Issue 51 https://doi.org/10.1073/pnas.1612849113	journal	December 2016
Structural properties of CuO/TiO2 nanorod in relation to their catalytic activity for simultaneous hydrogen production under solar light Khemthong, Pongtanawat; Photai, Pairat; Grisdanurak, Nurak International Journal of Hydrogen Energy, Vol. 38, Issue 36 https://doi.org/10.1016/j.ijhydene.2013.10.065	journal	December 2013
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 Bayés-García, Laura; Calvet, Teresa; Àngel Cuevas-Diarte, Miquel CrystEngComm, Vol. 15, Issue 2 https://doi.org/10.1039/c2ce26522b	journal	January 2013
Collective Dynamics in Water by High Energy Resolution Inelastic X-Ray Scattering Sette, F.; Ruocco, G.; Krisch, M. Physical Review Letters, Vol. 75, Issue 5 https://doi.org/10.1103/physrevlett.75.850	journal	July 1995
Three-dimensional charge density wave order in YBa2Cu3O6.67 at high magnetic fields Gerber, S.; Jang, H.; Nojiri, H. Science, Vol. 350, Issue 6263 https://doi.org/10.1126/science.aac6257	journal	November 2015
High-resolution thermal imaging with a combination of nano-focus X-ray diffraction and ultra-fast chip calorimetry Rosenthal, Martin; Doblas, David; Hernandez, Jaime J. Journal of Synchrotron Radiation, Vol. 21, Issue 1 https://doi.org/10.1107/s1600577513024892	journal	November 2013
Hermetic sample enclosure for simultaneous differential scanning calorimetry/synchrotron powder x-ray diffraction Lexa, Dusan Review of Scientific Instruments, Vol. 70, Issue 5 https://doi.org/10.1063/1.1149745	journal	May 1999
Absorption of circularly polarized x rays in iron Schütz, G.; Wagner, W.; Wilhelm, W. Physical Review Letters, Vol. 58, Issue 7 https://doi.org/10.1103/physrevlett.58.737	journal	February 1987
Elimination of self-absorption in fluorescence hard-x-ray absorption spectra Pfalzer, P.; Urbach, J. -P.; Klemm, M. Physical Review B, Vol. 60, Issue 13 https://doi.org/10.1103/physrevb.60.9335	journal	October 1999
Mixed Magnetism for Refrigeration and Energy Conversion Dung, Nguyen H.; Ou, Zhi Qiang; Caron, Luana Advanced Energy Materials, Vol. 1, Issue 6 https://doi.org/10.1002/aenm.201100252	journal	September 2011
Combining X-ray scattering with dielectric and calorimetric experiments for monitoring polymer crystallization Wurm, Andreas; Minakov, Alexander A.; Schick, Christoph European Polymer Journal, Vol. 45, Issue 11 https://doi.org/10.1016/j.eurpolymj.2009.07.014	journal	November 2009
Thin-film alternating current nanocalorimeter for low temperatures and high magnetic fields Minakov, A. A.; Roy, S. B.; Bugoslavsky, Y. V. Review of Scientific Instruments, Vol. 76, Issue 4 https://doi.org/10.1063/1.1889432	journal	April 2005
High‐speed (10 ⁴ °C/s) scanning microcalorimetry with monolayer sensitivity (J/m ² ) Lai, S. L.; Ramanath, G.; Allen, L. H. Applied Physics Letters, Vol. 67, Issue 9 https://doi.org/10.1063/1.115016	journal	August 1995
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 Francoual, S.; Strempfer, J.; Warren, J. Journal of Synchrotron Radiation, Vol. 22, Issue 5 https://doi.org/10.1107/s1600577515014149	journal	August 2015
Differential membrane-based nanocalorimeter for high-resolution measurements of low-temperature specific heat Tagliati, S.; Krasnov, V. M.; Rydh, A. Review of Scientific Instruments, Vol. 83, Issue 5 https://doi.org/10.1063/1.4717676	journal	May 2012
Thermodynamic signature of a magnetic-field-driven phase transition within the superconducting state of an underdoped cuprate Kemper, J. B.; Vafek, O.; Betts, J. B. Nature Physics, Vol. 12, Issue 1 https://doi.org/10.1038/nphys3502	journal	October 2015
The beam-heating effect in simultaneous differential scanning calorimetry/synchrotron powder X-ray diffraction Lexa, Dusan; Jeremy Kropf, A. Thermochimica Acta, Vol. 401, Issue 2 https://doi.org/10.1016/s0040-6031(02)00504-x	journal	May 2003
Gap symmetry and structure of Fe-based superconductors Hirschfeld, P. J.; Korshunov, M. M.; Mazin, I. I. Reports on Progress in Physics, Vol. 74, Issue 12 https://doi.org/10.1088/0034-4885/74/12/124508	journal	October 2011
Simultaneous differential scanning calorimetry and small-angle x-ray scattering Russell, T. P.; Koberstein, J. T. Journal of Polymer Science: Polymer Physics Edition, Vol. 23, Issue 6 https://doi.org/10.1002/pol.1985.180230603	journal	June 1985
First Order Magnetic Phase Transition in Fe ₂ P Lundgren, Leif; Tarmohamed, Gulzar; Beckman, Olof Physica Scripta, Vol. 17, Issue 1 https://doi.org/10.1088/0031-8949/17/1/008	journal	January 1978
Nanogram calorimetry using microscale suspended SiN _x platforms fabricated via focused ion beam patterning Wickey, K. J.; Chilcote, M.; Johnston-Halperin, E. Review of Scientific Instruments, Vol. 86, Issue 1 https://doi.org/10.1063/1.4905364	journal	January 2015
Re-exploring the double-melting behavior of semirigid-chain polymers with an in-situ combination of synchrotron nano-focus X-ray scattering and nanocalorimetry Melnikov, A. P.; Rosenthal, M.; Rodygin, A. I. European Polymer Journal, Vol. 81 https://doi.org/10.1016/j.eurpolymj.2015.12.031	journal	August 2016
Steady-State, ac-Temperature Calorimetry Sullivan, Paul F.; Seidel, G. Physical Review, Vol. 173, Issue 3 https://doi.org/10.1103/physrev.173.679	journal	September 1968
Thermodynamics around the first-order ferromagnetic phase transition of ${Fe}_{2} P$ single crystals Hudl, M.; Campanini, D.; Caron, L. Physical Review B, Vol. 90, Issue 14 https://doi.org/10.1103/physrevb.90.144432	journal	October 2014
Thin film microcalorimeter for heat capacity measurements from 1.5 to 800 K Denlinger, D. W.; Abarra, E. N.; Allen, Kimberly Review of Scientific Instruments, Vol. 65, Issue 4, p. 946-959 https://doi.org/10.1063/1.1144925	journal	April 1994
Simultaneous Differential Scanning Calorimetry-Synchrotron X-ray Powder Diffraction: A Powerful Technique for Physical Form Characterization in Pharmaceutical Materials Clout, Alexander; Buanz, Asma B. M.; Prior, Timothy J. Analytical Chemistry, Vol. 88, Issue 20 https://doi.org/10.1021/acs.analchem.6b02549	journal	September 2016
In-situ X-ray diffraction combined with scanning AC nanocalorimetry applied to a Fe _0.84 Ni _0.16 thin-film sample Gregoire, John M.; Xiao, Kechao; McCluskey, Patrick J. Applied Physics Letters, Vol. 102, Issue 20 https://doi.org/10.1063/1.4806972	journal	May 2013
Specific heat measurement set-up for quench condensed thin superconducting films Poran, Shachaf; Molina-Ruiz, Manel; Gérardin, Anne Review of Scientific Instruments, Vol. 85, Issue 5 https://doi.org/10.1063/1.4875590	journal	May 2014
Simulated sample heating from a nanofocused X-ray beam Wallander, Harald; Wallentin, Jesper Journal of Synchrotron Radiation, Vol. 24, Issue 5 https://doi.org/10.1107/s1600577517008712	journal	August 2017
Copper K-edge XANES of Cu(I) and Cu(II) oxide mixtures Gaur, A.; Shrivastava, B. D.; Joshi, S. K. Journal of Physics: Conference Series, Vol. 190 https://doi.org/10.1088/1742-6596/190/1/012084	journal	November 2009
Resonant X-Ray Scattering Studies of Charge Order in Cuprates Comin, Riccardo; Damascelli, Andrea Annual Review of Condensed Matter Physics, Vol. 7, Issue 1 https://doi.org/10.1146/annurev-conmatphys-031115-011401	journal	March 2016
Simultaneous X-Ray Diffraction and Differential Scanning Calorimetry (XDDSC) in Studies of Molecular and Liquid Crystals Ungar, G.; Feijoo, J. L. Molecular Crystals and Liquid Crystals Incorporating Nonlinear Optics, Vol. 180, Issue 2 https://doi.org/10.1080/00268949008042209	journal	March 1990
The Combination of Thermal Analysis and Time-Resolved X-ray Techniques: a Powerful Method for Materials Characterization Bras, W.; Derbyshire, G. E.; Devine, A. Journal of Applied Crystallography, Vol. 28, Issue 1 https://doi.org/10.1107/s0021889894008320	journal	February 1995
Polarized copper K -edge x-ray-absorption spectra in ${YBa}_{2}$ ${Cu}_{3}$ $O_{7 - y}$ Guo, J.; Ellis, D. E.; Alp, E. E. Physical Review B, Vol. 42, Issue 1 https://doi.org/10.1103/physrevb.42.251	journal	July 1990
Magnetocrystalline anisotropy and the magnetocaloric effect in Fe $_{2}$ P Caron, L.; Hudl, M.; Höglin, V. Physical Review B, Vol. 88, Issue 9 https://doi.org/10.1103/physrevb.88.094440	journal	September 2013
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 Baeten, Dorien; Mathot, Vincent B. F.; Pijpers, Thijs F. J. Macromolecular Rapid Communications, Vol. 36, Issue 12 https://doi.org/10.1002/marc.201500081	journal	April 2015
Correlated states in β-Li2IrO3 driven by applied magnetic fields Ruiz, Alejandro; Frano, Alex; Breznay, Nicholas P. Nature Communications, Vol. 8, Issue 1 https://doi.org/10.1038/s41467-017-01071-9	journal	October 2017
Susceptibility Anisotropy in an Iron Arsenide Superconductor Revealed by X-Ray Diffraction in Pulsed Magnetic Fields Ruff, J. P. C.; Chu, J. -H.; Kuo, H. -H. Physical Review Letters, Vol. 109, Issue 2 https://doi.org/10.1103/physrevlett.109.027004	journal	July 2012
The puzzle of high temperature superconductivity in layered iron pnictides and chalcogenides Johnston, David C. Advances in Physics, Vol. 59, Issue 6 https://doi.org/10.1080/00018732.2010.513480	journal	October 2010
Scanning AC nanocalorimetry combined with in-situ x-ray diffraction Xiao, Kechao; Gregoire, John M.; McCluskey, Patrick J. Journal of Applied Physics, Vol. 113, Issue 24 https://doi.org/10.1063/1.4811686	journal	June 2013
Absorption of circularly polarized x rays in iron Schütz, G.; Wagner, W.; Wilhelm, W. Deutsches Elektronen-Synchrotron, DESY, Hamburg https://doi.org/10.3204/pubdb-2017-03531	text	January 1987
Mixed Magnetism for Refrigeration and Energy Conversion Dung, N. H.; Ou, Z. Q.; Caron, L. arXiv https://doi.org/10.48550/arxiv.1203.0556	text	January 2012
Magnetocrystalline Anisotropy and the Magnetocaloric Effect in Fe2P Caron, L.; Hudl, M.; Höglin, V. arXiv https://doi.org/10.48550/arxiv.1307.2784	text	January 2013
Resonant x-ray scattering studies of charge order in cuprates Comin, Riccardo; Damascelli, Andrea arXiv https://doi.org/10.48550/arxiv.1509.03313	text	January 2015
Ideal charge density wave order in the high-field state of superconducting YBCO Jang, H.; Lee, W. -S.; Nojiri, H. arXiv https://doi.org/10.48550/arxiv.1607.05359	text	January 2016

Cited By (2)

Phase transition preceding magnetic long-range order in the double perovskite ${Ba}_{2} {NaOsO}_{6}$ Willa, Kristin; Willa, Roland; Welp, Ulrich Physical Review B, Vol. 100, Issue 4 https://doi.org/10.1103/physrevb.100.041108	journal	July 2019
Superconductivity in $Y_{7} R u_{4} InG e_{12}$ Bao, Jin-Ke; Bugaris, Daniel E.; Zheng, Huihuo Physical Review Materials, Vol. 3, Issue 2 https://doi.org/10.1103/physrevmaterials.3.024802	journal	February 2019

Similar Records

Combining nanocalorimetry and dynamic transmission electron microscopy for in situ characterization of materials processes under rapid heating and cooling

Journal Article · Fri Aug 15 00:00:00 EDT 2014 · Review of Scientific Instruments · OSTI ID:1419952

LaGrange, Thomas; Reed, Bryan W.; Campbell, Geoffrey H.; +1 more

Design and fabrication of a differential scanning nanocalorimeter

Journal Article · Mon Dec 19 00:00:00 EST 2016 · Journal of Micromechanics and Microengineering · OSTI ID:1419952

Zuo, Lei; Chen, Xiaoming; Yu, Shifeng; +1 more

Thin-film alternating current nanocalorimeter for low temperatures and high magnetic fields

Journal Article · Fri Apr 01 00:00:00 EST 2005 · Review of Scientific Instruments · OSTI ID:1419952

Minakov, A A; Roy, S B; Bugoslavsky, Y V; +1 more

Related Subjects

47 OTHER INSTRUMENTATION

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

Citation Formats

References (49)

Cited By (2)

Similar Records

Related Subjects