High-pressure and high-temperature differential scanning calorimeter for combined pressure-concentration-temperature measurements of hydrides

Mauron, Philippe; Bielmann, M.; Bissig, V.; Remhof, Arndt; Züttel, Andreas

doi:10.1063/1.3233939

Cited by 6 publications

(8 citation statements)

References 11 publications

(12 reference statements)

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“…The only calorimeter apparently available for studying metal hydride materials at high pressures and temperatures is a bespoke instrument that operates at hydrogen pressures up to 200 bars and temperatures up to 600°C. 6 Here, we present an alternative calorimeter design that enables the study of gram-scale heterogeneous chemical reactions at temperatures up to at least 1232°C while under pure hydrogen pressures up to 33 bars. The architecture of this calorimeter enables simultaneous calorimetric and pressure measurements.…”

Section: Introductionmentioning

confidence: 99%

High-temperature high-pressure calorimeter for studying gram-scale heterogeneous chemical reactions

MacLeod

Schauer

et al. 2017

Review of Scientific Instruments

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We present an instrument for measuring pressure changes and heat flows of physical and chemical processes occurring in gram-scale solid samples under high pressures of reactive gases. Operation is demonstrated at 1232 °C under 33 bars of pure hydrogen. Calorimetric heat flow is inferred using a grey-box non-linear lumped-element heat transfer model of the instrument. Using an electrical calibration heater to deliver 900 J/1 W pulses at the sample position, we demonstrate a dynamic calorimetric power resolution of 50 mW when an 80-s moving average is applied to the signal. Integration of the power signal showed that the 900 J pulse energy could be measured with an average accuracy of 6.35% or better over the temperature range 150-1100 °C. This instrument is appropriate for the study of high-temperature metal hydride materials for thermochemical energy storage.

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Section: Introductionmentioning

confidence: 99%

High-temperature high-pressure calorimeter for studying gram-scale heterogeneous chemical reactions

MacLeod

Schauer

et al. 2017

Review of Scientific Instruments

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“…Calorimetric reactors enable direct measurement of reaction thermodynamics and kinetics, and past work − has developed sensitive calorimeters to study surface reactions and catalysis. In Table we summarize data from five representative studies, listing their operating range and main figures of merit.…”

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confidence: 99%

“…In Table we summarize data from five representative studies, listing their operating range and main figures of merit. The instruments employ various temperature sensors, such as RTDs, thermocouples, , and pyroelectric heat detectors . In addition, they use several techniques for quantifying the mass of gas-phase reactants, such as pressure–concentration measurements, , molecular beams with known fluxes of reactants, and gravimetric measurements using a microbalance .…”

mentioning

confidence: 99%

“…The instruments employ various temperature sensors, such as RTDs, thermocouples, , and pyroelectric heat detectors . In addition, they use several techniques for quantifying the mass of gas-phase reactants, such as pressure–concentration measurements, , molecular beams with known fluxes of reactants, and gravimetric measurements using a microbalance . Additionally, the specifications of two relevant, commercially available instruments are listed in Table .…”

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confidence: 99%

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Microwatt-Resolution Calorimeter for Studying the Reaction Thermodynamics of Nanomaterials at High Temperature and Pressure

et al. 2020

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Calorimetry of reactions involving nanomaterials is of great current interest, but requires high-resolution heat flow measurements and long-term thermal stability. Such studies are especially challenging at elevated reaction pressures and temperatures. Here, we present an instrument for measuring the enthalpy of reactions between gas-phase reactants and milligram scale nanomaterial samples. This instrument can resolve the net change in the amount of gas-phase reactants due to surface reactions in an operating range from room temperature to 300 °C and reaction pressures of 10 mbar to 30 bar. The calorimetric resolution is shown to be <3 μW/√Hz, with a long-term stability <4 μW/hour. The performance of the instrument is demonstrated via a set of experiments involving H2 absorption on Pd nanoparticles at various pressures and temperatures. For this specific reaction, we obtained a mass balance resolution of 0.1 μmol/√Hz. Results from these experiments are in good agreement with past studies establishing the feasibility of performing high resolution calorimetry on milligram scale nanomaterials, which can be employed in future studies probing catalysis, phase transformations, and thermochemical energy storage.

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“…Various types of temperature sensors are designed to serve this purpose. [1][2][3] The commonly used thermocouples and diode sensors are not suitable in RF environment due to electromagnetic perturbation. Photonic sensors offer alternative solution as these are immune to electromagnetic interference, small in size and robust.…”

mentioning

confidence: 99%

Note: Epitaxial ruby thin film based photonic sensor for temperature measurement

Kumari

Khare

2011

Review of Scientific Instruments

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Deposition of optical quality C-axis oriented epitaxial thin film of ruby via pulsed laser deposition technique on sapphire substrate is reported. The film is characterized by Raman spectra and photoluminescence spectra. The peak positions of R-line and the corresponding linewidth are observed to be temperature dependent. The sensitivity of R(1)-line position, υ, with the temperature, (dυ/dT), in the range of 138-368 K shows linear behavior confirming its applicability as temperature sensor.

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High-pressure and high-temperature differential scanning calorimeter for combined pressure-concentration-temperature measurements of hydrides

Cited by 6 publications

References 11 publications

High-temperature high-pressure calorimeter for studying gram-scale heterogeneous chemical reactions

High-temperature high-pressure calorimeter for studying gram-scale heterogeneous chemical reactions

Microwatt-Resolution Calorimeter for Studying the Reaction Thermodynamics of Nanomaterials at High Temperature and Pressure

Note: Epitaxial ruby thin film based photonic sensor for temperature measurement

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