Combining nanocalorimetry and atomic force microscopy to study structure formation processes on the nanoscale

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Abstract

Wide range of rapid analytical methods intended for the physicochemical analysis of organic compounds are being actively developed. The present paper highlights the possibility of studying microquantities of polymer materials using a chip calorimetry (nanocalorimetry) method combined with atomic force microscopy (AFM). An experimental setup is presented for conducting combined studies using ultrafast chip calorimetry and AFM. The main technological aspects of combining the two methods are considered, and behavior of a nanocalorimetric sensor when interacting with a cold AFM cantilever for measurements of microquantities of polymer materials at different temperatures is addressed in situ.

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About the authors

A. F. Akhkiamova

Lomonosov Moscow State University; Federal Research Center of Problems of Chemical Physics and Medicinal Chemistry, RAS; NUST MISIS

Email: azigy@mail.ru
ORCID iD: 0000-0003-0177-7818

Junior Researcher

Russian Federation, Moscow; Chernogolovka; Moscow

A. F. Abukaev

Lomonosov Moscow State University

Email: azigy@mail.ru
ORCID iD: 0000-0002-7164-5688

Junior Researcher

Russian Federation, Moscow

I. I. Rulev

Lomonosov Moscow State University; NUST MISIS

Email: azigy@mail.ru
ORCID iD: 0009-0000-9652-7680

Junior Researcher

Russian Federation, Moscow; Moscow

A. Y. Konyakhina

Sirius University of Science and Technology

Email: azigy@mail.ru
ORCID iD: 0000-0002-0287-3396

Junior Researcher

Russian Federation, Township Sirius

A. P. Melnikov

Lomonosov Moscow State University

Email: azigy@mail.ru
ORCID iD: 0000-0003-2277-9644

Doct. of Sci. (Physics and Mathematics), Researcher

Russian Federation, Moscow

D. A. Ivanov

Lomonosov Moscow State University; Federal Research Center of Problems of Chemical Physics and Medicinal Chemistry, RAS; Sirius University of Science and Technology; NUST MISIS

Author for correspondence.
Email: azigy@mail.ru
ORCID iD: 0000-0002-5905-2652

Doct. of Sci. (Physics and Mathematics), Senior Researcher

Russian Federation, Moscow; Chernogolovka; Township Sirius; Moscow

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Supplementary files

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2. Fig.1. General view of the universal holder with nanocalorimetric sensor

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3. Fig.2. Procedure of particle entrapment by keratin fibre keratin fibre procedure

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4. Fig.3. View of the AFM control head directly above nanocalorimetric sensor active zone (a). Optical image of the nanocalorimetric sensor combined active zone and AFM cantilever (b)

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5. Fig.4. Plots of the temperature spike of the sensor, in real time, when the cantilever is introduced into the system at temperatures of 50 °C, 100 °C, 150 °C and 200 °C

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6. Fig.5. Graph of temperature spike dependence on the sensor when introducing a cantilever as a function of active area temperature of the sensor

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7. Fig.6. AFM images of surface topography of nanocalorimetric sensor active area at 50 °C (left) and 200 °C (right)

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8. Fig.7. AFM image of an isothermally crystallised poly(trimethylene terephthalate) sample crystallised at 210 °C at the nanocalorimetric sensor temperature of 200 °C

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Copyright (c) 2024 Akhkiamova A.F., Abukaev A.F., Rulev I.I., Konyakhina A.Y., Melnikov A.P., Ivanov D.A.