A high temperature cell for investigating interfacial structure on the molecular scale in molten salt/alloy systems

James F. Browning; Joohyun Seo; John F. Wenzel; Gabriel M. Veith; Mathieu Doucet; Alexander S. Ivanov; Phillip Halstenberg; Gary Lynn; Sheng Dai

doi:10.1063/5.0065860

A high temperature cell for investigating interfacial structure on the molecular scale in molten salt/alloy systems

James F. Browning, Joohyun Seo, John F. Wenzel, Gabriel M. Veith, Mathieu Doucet, Alexander S. Ivanov, Phillip Halstenberg, Gary Lynn, Sheng Dai

Research output: Contribution to journal › Article › peer-review

1 Scopus citations

Abstract

In this work, we describe the design and development of an in situ neutron reflectometry cell for high temperature investigations of structural changes occurring at the interface between inorganic salts, in their molten state up to 800 °C, and corrosion resistant alloys or other surfaces. In the cell, a molten salt is confined by an annular ring of single crystal sapphire constrained between the sample substrate and a sapphire plate using two gold O-rings, enclosing a liquid salt volume of 20 ml, along with a dynamic cell volume to accommodate expansion of the liquid with heating. As a test case for the cell, we report on an in situ neutron reflectometry measurement of the interface between a eutectic salt mixture of MgCl2-KCl (32:68 molar ratio) and a single crystal sapphire substrate at 450 °C, resulting in the formation of a 60 Å layer having a scattering length density of 1.72 × 10-6 Å-2. While the origin of this layer is uncertain, it is likely to have resulted from the salt reacting with an existing impurity layer on the sapphire substrate.

Original language	English
Article number	123903
Journal	Review of Scientific Instruments
Volume	92
Issue number	12
DOIs	https://doi.org/10.1063/5.0065860
State	Published - Dec 1 2021

Funding

The design and fabrication of the high temperature cell were supported by the U.S. Department of Energy’s Office of Energy Efficiency and Renewable Energy (EERE) under Solar Energy Technologies Office Award No. 33874. The work at ORNL Chemical Sciences Division was supported by the Molten Salts in Extreme Environments (MSEE) Energy Frontier Research Center, funded by the U.S. Department of Energy Office of Science (salt synthesis and assistance with the cell testing and in situ neutron reflectometry experiments). A portion of this research used resources at the Spallation Neutron Source (SNS), a Department of Energy (DOE) Office of Science User Facility operated by ORNL. Neutron reflectometry measurements were carried out on the Liquids Reflectometer at the SNS, which is sponsored by the Scientific User Facilities Division, Office of Basic Energy Sciences, DOE. ORNL is managed by UT-Battelle LLC for DOE under Contract No. DE-AC05-00OR22725.

Funders	Funder number
Scientific User Facilities Division
U.S. Department of Energy
Office of Energy Efficiency and Renewable Energy
Basic Energy Sciences
Oak Ridge National Laboratory
Solar Energy Technologies Office	33874
Solar Energy Technologies Office
UT-Battelle	DE-AC05-00OR22725
UT-Battelle

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title = "A high temperature cell for investigating interfacial structure on the molecular scale in molten salt/alloy systems",

abstract = "In this work, we describe the design and development of an in situ neutron reflectometry cell for high temperature investigations of structural changes occurring at the interface between inorganic salts, in their molten state up to 800 °C, and corrosion resistant alloys or other surfaces. In the cell, a molten salt is confined by an annular ring of single crystal sapphire constrained between the sample substrate and a sapphire plate using two gold O-rings, enclosing a liquid salt volume of 20 ml, along with a dynamic cell volume to accommodate expansion of the liquid with heating. As a test case for the cell, we report on an in situ neutron reflectometry measurement of the interface between a eutectic salt mixture of MgCl2-KCl (32:68 molar ratio) and a single crystal sapphire substrate at 450 °C, resulting in the formation of a 60 {\AA} layer having a scattering length density of 1.72 × 10-6 {\AA}-2. While the origin of this layer is uncertain, it is likely to have resulted from the salt reacting with an existing impurity layer on the sapphire substrate.",

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AU - Doucet, Mathieu

AU - Ivanov, Alexander S.

AU - Halstenberg, Phillip

AU - Lynn, Gary

AU - Dai, Sheng

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N2 - In this work, we describe the design and development of an in situ neutron reflectometry cell for high temperature investigations of structural changes occurring at the interface between inorganic salts, in their molten state up to 800 °C, and corrosion resistant alloys or other surfaces. In the cell, a molten salt is confined by an annular ring of single crystal sapphire constrained between the sample substrate and a sapphire plate using two gold O-rings, enclosing a liquid salt volume of 20 ml, along with a dynamic cell volume to accommodate expansion of the liquid with heating. As a test case for the cell, we report on an in situ neutron reflectometry measurement of the interface between a eutectic salt mixture of MgCl2-KCl (32:68 molar ratio) and a single crystal sapphire substrate at 450 °C, resulting in the formation of a 60 Å layer having a scattering length density of 1.72 × 10-6 Å-2. While the origin of this layer is uncertain, it is likely to have resulted from the salt reacting with an existing impurity layer on the sapphire substrate.

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A high temperature cell for investigating interfacial structure on the molecular scale in molten salt/alloy systems

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