Exploring crucible designs for differential scanning calorimetry measurements of fluoride salts

Piro, M.H.A.; Lipkina, K.; Hallatt, Daniel

doi:10.1016/j.tca.2021.178860

Cited by 10 publications

(5 citation statements)

References 29 publications

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“…Both heating and cooling effects were analyzed to establish melting and crystallization temperatures/behavior. Samples were prepared in the glovebox and consisted of 10–50 mg of material within individual custom nickel liners that were hermetically sealed in high-pressure, 100 μL chrome-nickel stainless steel crucibles as previously described. , Two DSC calibration methods were used: The suggested method of Netzsch-Gerätebau GmbH, which consists of heating the sample three times at the same heating rate (β), where β = 5 K min –1 , and then using the average values of the second and third measurements. Sensitivity and temperature corrections were obtained from measurements with indium, lead, silver, CsCl, and NaCl standards.…”

Section: Methodsmentioning

confidence: 99%

“…Samples were prepared in the glovebox and consisted of 10−50 mg of material within individual custom nickel liners that were hermetically sealed in high-pressure, 100 μL chrome-nickel stainless steel crucibles as previously described. 62,63 Two DSC calibration methods were used: i. The suggested method of Netzsch-Geraẗebau GmbH, which consists of heating the sample three times at the same heating rate (β), where β = 5 K min −1 , and then using the average values of the second and third measurements.…”

Section: Thermal Analysismentioning

confidence: 99%

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Thermal Property Modeling and Assessment of the Physical Properties of FLiNaK

Schorne-Pinto,

Aziziha,

Tisdale

et al. 2024

ACS Appl. Energy Mater.

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The thermodynamic properties of the LiF−NaF−KF system and its subsystems were re-evaluated using the CALPHAD method, focusing on the deviations from ideality in the heat capacity [C p (T)] of mixtures, temperature-dependence of mixing enthalpies (Δ mix H), vapor pressures of mixtures, and enthalpies of fusion (ΔH fus ) using reported values and measurements. The results of this work confirmed a pseudoternary eutectic at 732.9 K and 46.5LiF− 11.5NaF−42KF mol % (FLiNaK) with determined C p (T) = 69.822 + 0.000679T + 2,137,152T −2 J mol −1 K −1 (732.9 < T < 1200 K) and ΔH fus = 18,051 J mol −1 in good agreement to the experimental values. The resulting accurate thermodynamic representation can be used to find relevant excess thermochemical properties in the whole pseudoternary space and provide insights into their composition and temperature dependence. A detailed evaluation of select thermophysical properties was also conducted to determine recommended density, thermal diffusivity, thermal conductivity, vapor pressures, and boiling point with calculated uncertainties over the temperature range of interest for FLiNaK−salt energy applications.

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Section: Methodsmentioning

confidence: 99%

Section: Thermal Analysismentioning

confidence: 99%

Thermal Property Modeling and Assessment of the Physical Properties of FLiNaK

Schorne-Pinto,

Aziziha,

Tisdale

et al. 2024

ACS Appl. Energy Mater.

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“…Use of DSC crucibles that are stable at high temperatures is necessary to measure the thermal and thermochemical behavior of molten fluoride salts over the range of temperatures that are of interest to MSR developers. Measurements at elevated temperature require a hermetic seal to maintain salt purity in the presence of atmospheric impurities and prevent loss of salt components (Piro, Lipkina, and Hallat, 2021). Analyses with salts sealed in the gold cells currently used at Argonne and elsewhere are limited to temperatures below approximately 800 °C because softening of gold and distortion of the cells occurs at higher temperatures.…”

Section: High Temperature Dsc Cruciblesmentioning

confidence: 99%

“…Nickel is resistant to corrosive attack by the fluoride salts of interest to MSR developers (Piro, Lipkina, andHallat, 2021 andMcMurray et al, 2018). Nickel crucibles were fabricated at Argonne from sheet stock of Ni-201 metal to match the design of the commercially available gold cells.…”

Section: Nickel Cruciblesmentioning

confidence: 99%

Property Measurements of the NaCl-PuCl<sub>3</sub> Molten Salt System

Gardner

Rose

2022

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“…Stock materials must be rigorously dried and purified, and subsequent storage and handling must be performed under controlled atmospheric conditions. The melting point of pure unmixed salts is generally high, in excess of 1075 K. Given the elevated vapor pressure at high temperatures (> 1300 K), single-use sealed containers are often required [8]. Conventional methods for measurement of thermal properties generally require non-trivial adaptations.…”

Section: Introductionmentioning

confidence: 99%

Feasibility of volumetric expansion of molten chlorides by conventional pushrod dilatometry

Parker

Abdul-Jabbar

Jackson

et al. 2022

J Radioanal Nucl Chem

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This study is a short communication on progress made in the adaptation of conventional push-rod dilatometry for the measurement of volumetric expansion of liquid salts up to 1300 K. A new crucible design is offered as a practical solution for measurement of liquid salts by this method. Proof-of-concept measurements of the volumetric expansion of sodium chloride (NaCl) are compared to the available data in literature. Measurement of the coefficient of thermal expansion (CTE) of solid NaCl compared favorably to the available data in literature, confirming both magnitude and trend. The average CTE of NaCl (solid) was $$\overline{\alpha }_{{{\text{NaCl}}\;{\text{Solid}}}} = 5.63 \cdot 10^{ - 5} {\raise0.7ex\hbox{$1$} \!\mathord{\left/ {\vphantom {1 K}}\right.\kern-\nulldelimiterspace} \!\lower0.7ex\hbox{$K$}}$$ α ¯ NaCl Solid = 5.63 · 10 - 5 1 K . The volumetric expansion of liquid NaCl was measured as $$\beta_{{{\text{NaCl}}\;{\text{Liquid}}}} \approx 3.96 \cdot 10^{ - 5} 1/K$$ β NaCl Liquid ≈ 3.96 · 10 - 5 1 / K and is essentially constant from the melt point to 1300 K. The volumetric expansion produced by this method is in reasonable agreement with the available published data and previous measurements made by the authors by neutron radiographic technique.

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Exploring crucible designs for differential scanning calorimetry measurements of fluoride salts

Cited by 10 publications

References 29 publications

Thermal Property Modeling and Assessment of the Physical Properties of FLiNaK

Thermal Property Modeling and Assessment of the Physical Properties of FLiNaK

Property Measurements of the NaCl-PuCl<sub>3</sub> Molten Salt System

Feasibility of volumetric expansion of molten chlorides by conventional pushrod dilatometry

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