Differential AC‐chip calorimeter for glass transition measurements in ultrathin films

Huth, Heiko; Минаков, А. А.; Schick, Christoph

doi:10.1002/polb.20921

Cited by 166 publications

(202 citation statements)

References 34 publications

Supporting

Mentioning

186

Contrasting

Order By: Relevance

“…The amplitude and phase lag of the resulting temperature oscillation provide accurate information on both the heat capacity of the sample and its heat loss to the environment. Using this idea, Huth et al 16 and Guenther et al 17 developed AC chip-calorimeters that can operate at scanning rates below 10 K/min. Xiao et al 15 recently developed a different a)…”

Section: Introductionmentioning

confidence: 99%

Scanning AC nanocalorimetry combined with in-situ x-ray diffraction

Xiao

Gregoire

McCluskey

et al. 2013

Journal of Applied Physics

View full text Add to dashboard Cite

Micromachined nanocalorimetry sensors have shown excellent performance for high-temperature and high-scanning rate calorimetry measurements. Here, we combine scanning AC nanocalorimetry with in-situ x-ray diffraction (XRD) to facilitate interpretation of the calorimetry measurements. Time-resolved XRD during in-situ operation of nanocalorimetry sensors using intense, high-energy synchrotron radiation allows unprecedented characterization of thermal and structural material properties. We demonstrate this experiment with detailed characterization of the melting and solidification of elemental Bi, In, and Sn thin-film samples, using heating and cooling rates up to 300 K/s. Our experiments show that the solidification process is distinctly different for each of the three samples. The experiments are performed using a combinatorial device that contains an array of individually addressable nanocalorimetry sensors. Combined with XRD, this device creates a new platform for high-throughput mapping of the composition dependence of solid-state reactions and phase transformations. V C 2013 AIP Publishing LLC.

show abstract

Section: Introductionmentioning

confidence: 99%

Scanning AC nanocalorimetry combined with in-situ x-ray diffraction

Xiao

Gregoire

McCluskey

et al. 2013

Journal of Applied Physics

View full text Add to dashboard Cite

show abstract

“…where K m and c are the thermal conductivity and the specific heat capacity of the medium in which the wave propagates, respectively [31,49].…”

Section: B the Effect Of Frequency On The Ac Measurementmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

“…In this device, the applied AC frequency is limited to approximately 100Hz because the distance between the sample and the temperature sensor dampens the temperature response of the sensor [32]. Moreover, the scan rate cannot exceed 5 K/min because of considerations of temperature uniformity across the sample and accuracy of the temperature measurements [31].…”

Section: Introductionmentioning

confidence: 99%

“…Integration [31]. In this device, the applied AC frequency is limited to approximately 100Hz because the distance between the sample and the temperature sensor dampens the temperature response of the sensor [32].…”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Scanning AC Nanocalorimetry and Its Applications

Xiao

Vlassak

2016

Fast Scanning Calorimetry

View full text Add to dashboard Cite

This thesis presents an AC nanocalorimetry technique that enables calorimetry measurements on very small quantities of materials over a wide range of scanning rates (from isothermal to 3×10^3 K/s), temperatures (up to 1200 K), and environments. Such working range bridges the gap between traditional scanning calorimetry of bulk materials and nanocalorimetry. The method relies on a micromachined nanocalorimeter with negligible thermal lags between heater, thermometer, and sample. The ability to perform calorimetry measurements over such a broad range of scanning rates makes it an ideal tool to characterize the kinetics of phase transformations, reactions at elevated temperatures or to explore the behavior of materials far from equilibrium. We By combining scanning DC and AC nano-calorimetry techniques, we study the nucleation behavior of undercooled liquid Bi at cooling rates ranging from 10^1 to 10^4 K/s. Upon initial melting, the Bi thin-film sample breaks up into isolated islands. The number of islands in a typical sample is sufficiently large that highly repeatable nucleation behavior is observed, despite the stochastic nature of the nucleation process.We establish a data reduction technique to evaluate the nucleation rate from DC and AC calorimetry results. The results show that the driving force for the nucleation of melted Bi is well described by classical nucleation theory over a wide range of cooling rates. The proposed technique provides a unique and efficient way to examine nucleation kinetics v with cooling rates over several orders of magnitude. The technique is quite general and can be used to evaluate reaction kinetics in other materials.Lastly, we apply the scanning AC nanocalorimetry technique to study solid-gas phase reactions by measuring the change in heat capacity of a sample during reaction. We apply this approach to evaluate the oxidation kinetics of thin-film samples of zirconium in air. The results confirm parabolic oxidation kinetics with an activation energy of 0.59±0.03 eV. The nano-calorimetry measurements were performed using a device that contains an array of micromachined nano-calorimeter sensors in an architecture designed for combinatorial studies. We demonstrate that the oxidation kinetics can be quantified using a single sample, thus enabling high-throughput mapping of the composition-dependence of the reaction rate.vi

show abstract

Physical Aging of Polymers

Cangialosi

2018

Encyclopedia of Polymer Science and Technology

View full text Add to dashboard Cite

This article provides an overview of the most important aspects of physical aging of polymers. First, we briefly introduce basic concepts of the glass transition, that is, the way a nonequilibrium glass is formed. Subsequently, after presenting the way physical aging can be monitored, we describe the main well‐established signatures of physical aging, that is, its nonexponential and nonlinear nature. The next part of the article is dedicated to recent advancements in the physical aging of bulk polymers. In this context, recent experimental activity is discussed, where the existence of multiple mechanisms for equilibrium recovery is presented. In addition, important aspects of physical aging in polymers altered by geometrical confinement are scrutinized in light of the past 20 years efforts aiming to understand glass dynamics in such conditions. It is shown how confined polymers weakly interacting with the confining medium exhibit accelerated physical aging. Importantly, such acceleration was found to be decoupled from the molecular mobility of the glass. Finally, we briefly discuss how recent advancements in physical aging of polymers in bulk and under geometrical confinement should foster experimental efforts to unveil important basic aspects of the glass transition, such as the existence of the so‐called “ideal glass.”

show abstract

Differential AC‐chip calorimeter for glass transition measurements in ultrathin films

Cited by 166 publications

References 34 publications

Scanning AC nanocalorimetry combined with in-situ x-ray diffraction

Scanning AC nanocalorimetry combined with in-situ x-ray diffraction

Scanning AC Nanocalorimetry and Its Applications

Physical Aging of Polymers

Contact Info

Product

Resources

About