Scanning AC nanocalorimetry study of Zr/B reactive multilayers

Lee, Dongwoo; Sim, Gi-Dong; Xiao, Kechao; Choi, Yong Seok; Vlassak, Joost J.

doi:10.1063/1.4833572

Cited by 27 publications

(25 citation statements)

References 32 publications

(57 reference statements)

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“…The samples were heated to approximately 1550 K at heating rates from 4800 K/s to 56600 K/s. The power input and the temperature data were utilized to determine the reactive heat flow of the nano-laminate sample following the procedures established in our previous work 17 .…”

Section: Methodsmentioning

confidence: 99%

“…The micromachined nanocalorimetry sensors used in this study have been described in detail elsewhere in the literature [17][18][19] ; a brief description of the sensors and experimental details are provided in the methods section. RNLs consisting of alternating Zr and B 4 C layers were sputter deposited directly onto the nanocalorimetry sensors as illustrated schematically in the inset of Figure 1a.…”

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confidence: 99%

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Kinetic Role of Carbon in Solid-State Synthesis of Zirconium Diboride using Nanolaminates: Nanocalorimetry Experiments and First-Principles Calculations

et al. 2015

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Reactive nano-laminates afford a promising route for the low-temperature synthesis of zirconium diboride, an ultrahigh-temperature ceramic with metallic properties. Although the addition of carbon is known to facilitate sintering of ZrB 2 , its effect on the kinetics of the formation reaction has not been elucidated. We have employed a combined approach of nanocalorimetry and first-principles theoretical studies to investigate the kinetic role of carbon in the synthesis of ZrB 2 using B 4 C/Zr reactive nano-laminates. Structural characterization of the laminates by XRD and TEM reveal that the reaction proceeds via inter-diffusion of the B 4 C and Zr layers, which produces an amorphous Zr 3 B 4 C alloy. This amorphous alloy then crystallizes to form a super-saturated ZrB 2 (C) compound. A kinetic analysis shows that carbon lowers the energy barriers for both inter-diffusion and crystallization by more than 20%. Energetic calculations based on first-principles modeling suggest that the reduction of the diffusion barrier may be attributed to the stronger bonding between Zr and C as compared to the bonding between Zr and B.

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Section: Methodsmentioning

confidence: 99%

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confidence: 99%

Kinetic Role of Carbon in Solid-State Synthesis of Zirconium Diboride using Nanolaminates: Nanocalorimetry Experiments and First-Principles Calculations

et al. 2015

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“…Apart from the applications detailed in this thesis, scanning AC nanocalorimetry has also been applied to study the martensitic phase transformation of Fe-Ni system [97], the reaction of Zr/B multilayers [81], and the glass transformation of metallic glasses. In an on-going research project, it is also being applied to study the initial stage of the oxidation reaction for ZrB2 based ceramics.…”

Section: Discussionmentioning

confidence: 99%

“…We perform calorimetry measurements using a nanocalorimeter sensor derived from an original design by Allen and coworkers [3,15], which has negligible thermal lag between sample and temperature sensor thus enabling accurate temperature measurement at very high scanning rates. This nanocalorimeter sensor combined with the appropriate AC-technique [22] is also capable of making accurate measurements at medium to slow scan rates where heat loss to the environment makes DC measurements not practical [81], even allowing in-situ XRD measurements during the scans [26]. By combining AC and DC techniques we have performed measurements on undercooled Bi samples at cooling rates from 10 1 to 10 4 K/s and use classical nucleation theory to interpret the experimental results.…”

Section: Introductionmentioning

confidence: 99%

“…The technique has been applied to study phase transformations in thin-film samples with thickness as small as a few nanometers [5,16,54,55,61,82,[94][95][96]. A recently developed scanning AC nano-calorimetry technique can be used to measure heat capacity over a wide range of temperatures (up to 1300 K) and heating rates (from isothermal to 3000 K/s) [22,24,81]. The technique has been combined with in-situ X-ray diffraction for structural analysis of reaction products [26,97].…”

Section: Introductionmentioning

confidence: 99%

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Scanning AC Nanocalorimetry and Its Applications

Xiao

Vlassak

2016

Fast Scanning Calorimetry

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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

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Fast Scanning Calorimetry

Schick

Androsch

2022

Thermal Analysis of Polymeric Materials

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Scanning AC nanocalorimetry study of Zr/B reactive multilayers

Cited by 27 publications

References 32 publications

Kinetic Role of Carbon in Solid-State Synthesis of Zirconium Diboride using Nanolaminates: Nanocalorimetry Experiments and First-Principles Calculations

Kinetic Role of Carbon in Solid-State Synthesis of Zirconium Diboride using Nanolaminates: Nanocalorimetry Experiments and First-Principles Calculations

Scanning AC Nanocalorimetry and Its Applications

Fast Scanning Calorimetry

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