Design of a Combined Setup for Simultaneous Measurements of the Microstructural and Thermo-Analytical Parameters of Nanogram-Size Samples

Abstract:

In the present paper, we describe an experimental setup combining micro- and nano-focus X-ray scattering and chip calorimetry (nanocalorimetry), which is designed for in-situ measurements on nanogram-size samples. Such combination of techniques capable to simultaneously probe the micro-structural and thermodynamic properties of materials can be useful for studies of materials having a complex phase behavior or prone to form metastable states. The setup is made compatible with micro- and nano-focus synchrotron beamlines.

• Periodical: Applied Mechanics and Materials (Volume 788)
• Pages: 136-142
• DOI: https://doi.org/10.4028/www.scientific.net/AMM.788.136
• Online since: August 2015
• Authors: Martin Rosenthal, Alexey P. Melnikov, Andrei A. Rychkov, David Doblas, Dmitriy V. Anokhin, Manfred Burghammer, Dmitriy A. Ivanov*
• Keywords: Melting, Nanocalorimetry, Nanodiffraction, Poly (Trimethylene Terepthalate), Semicrystalline Polymer

References

[1] L. H. Allen, G. Ramanath, S. L. Lai, Z. Ma, S. Lee, D. D. J. Allman, K. P. Fuchs, 1 000 000 °C/s thin film electrical heater: In situ resistivity measurements of Al and Ti/Si thin films during ultra rapid thermal annealing, Appl. Phys. Lett. 64 (1994).

DOI: 10.1063/1.111116

[2] S. L. Lai, G. Ramanath, L. H. Allen, P. Infante, Z. Ma, High-speed (104 oC/s) scanning microcalorimetry with monolayer sensitivity (J/m2), Appl. Phys. Lett. 67 (1995) 1229-1231.

DOI: 10.1063/1.115016

[3] S. Lai, L. H. Allen, MEMS-based scanning calorimeter for thermodynamic properties of nanostructures, Microscale Thermophysical Engineering. 2 (1998) 11-19.

DOI: 10.1080/108939598200060

[4] A.T. Kwan, M. Yu. Efremov, E. A. Olson, F. Schiettekatte, M. Zhang, P. H. Geil, L. H. Allen., Nanoscale Calorimetry of Isolated Polyethylene Single Crystals, J. Polym. Sci., Part B: Polym. Phys. 39 (2001) 1237-1245.

DOI: 10.1002/polb.1097

[5] E. A. Olson, M. Yu. Efremov, M. Zhang, Z. S. Zhang, L. H. Allen., The Design and Operation of a MEMS Differential Scanning Nanocalorimeter for High-speed Heat Capacity Measurements of Ultrathin Films, Journal of Microelectromechanical Systems. 12 (2003).

DOI: 10.1109/jmems.2003.811755

[6] M. Yu. Efremov, E. A. Olson, M. Zhang, L. H. Allen, Glass Transition of Thin Films of Poly(2-vinyl pyridine) and Poly(methyl methacrylate): Nanocalorimetry Measurements, Thermochim. Acta. 403 (2003) 37-41.

DOI: 10.1016/s0040-6031(03)00122-9

[7] W. A. Donald, R. D. Leib, J. T. O'Brien, A. I. S. Holm, E. R. Williams, Nanocalorimetry in mass spectrometry: A route to understanding ion and electron solvation, Proceedings of the National Academy of Sciences. 105 (2008) 18102–18107.

DOI: 10.1073/pnas.0801549105

[8] M. D. Grapes, T. LaGrange, K. Woll, B. W. Reed, G. H. Campbell, D. A. LaVan, T. P. Weihs, In situ transmission electron microscopy investigation of the interfacial reaction between Ni and Al during rapid heating in a nanocalorimeter, APL Mater. 2 (2014).

DOI: 10.1063/1.4900818

[9] K. C. Xiao, J. M. Gregoire, P. J. McCluskey, D. Dale, J. J. Vlassak, Scanning AC nanocalorimetry combined with in-situ x-raydiffraction, J. Appl. Phys. 113 (2013) 243501-10.

DOI: 10.1063/1.4811686

[10] J. M. Gregoire, K. C. Xiao, P. J. McCluskey, D. Dale, G. Cuddalorepatta, J. J. Vlassak, In-situ X-ray diffraction combined with scanning AC nanocalorimetry applied to a Fe0. 84Ni0. 16 thin-film sample, Appl. Phys. Lett. 102 (2013) 201902-4.

DOI: 10.1063/1.4806972

[11] J. M. Gregoirea, P. J. McCluskeya, D. Daleb, S. Dingc, J. Schroersc, J. J. Vlassak, Combining combinatorial nanocalorimetry and X-ray diffraction techniques to study the effects of composition and quench rate on Au–Cu–Si metallic glasses, Scr. Mater. 66 (2012).

DOI: 10.1016/j.scriptamat.2011.10.034

[12] M. van Drongelen, T. Meijer-Vissers, D. Cavallo, G. Portale, R. Androsch, Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter, Thermochim. Acta. 563 (2013) 33-37.

DOI: 10.1016/j.tca.2013.04.007

[13] N. Piazzon, M. Rosenthal, A. Bondar, D. Spitzer, D.A. Ivanov, Characterization of Explosives Traces by the Nanocalorimetry, J. Phys. Chem. Solids. 71 (2010) 114-118.

DOI: 10.1016/j.jpcs.2009.07.032

[14] D. Spitzer, K. Bonnot, L. Schlur, N. Piazzon, D. Doblas, D. Ivanov, T. Cottineau, V. Keller, Bio-inspired explosive sensors and specific signatures, Procedia Engineering. 87 (2014) 740 – 746.

DOI: 10.1016/j.proeng.2014.11.643

[15] M. Rosenthal, D. Doblas, J.J. Hernandez, Ya.I. Odarchenko, M. Burghammer, E. Di Cola, D. Spitzer, A.E. Antipov, L.S. Aldoshin, D.A. Ivanov, High-Resolution Thermal Imaging with a Combination of Nano-Focus X-ray Diffraction and Ultra-Fast Chip Calorimetry, Journal of Synchrotron Radiation. 21 (2014).

DOI: 10.1107/s1600577513024892

[16] C. Riekel, E. Di Cola, M. Burghammer, M. Reynolds, M. Rosenthal, D. Doblas, D. A. Ivanov, Thermal Transformations of Self-Assembled Gold Glyconanoparticles Probed by Combined Nanocalorimetry and X-ray Nanobeam Scattering, Langmuir. 31 (2015).

DOI: 10.1021/la504015e

[17] M. Rosenthal, M. Burghammer, G. Bar, E. T. Samulski, D. A. Ivanov, Switching Chirality of Hybrid Left−Right Crystalline Helicoids Built of Achiral Polymer Chains: When Right to Left Becomes Left to Right, Macromolecules. 47 (2014) 8295–8304.

DOI: 10.1021/ma501733n

[18] M. Rosenthal, G. Portale, M. Burghammer, G. Bar, E. T. Samulski, D. A. Ivanov, Exploring the Origin of Crystalline Lamella Twist in Semi-Rigid Chain Polymers: the Model of Keith and Padden revisited, Macromolecules. 45 (2012) 7454-7460.

DOI: 10.1021/ma301446t

[19] D. A. Ivanov, G. Bar, M. Dosière, M. H.J. Koch, A Novel View on Crystallization and Melting of Semirigid Chain Polymers: The Case of Poly(trimethylene terephthalate), Macromolecules. 41 (2008) 9224-9233.

DOI: 10.1021/ma801604a