Development of a variable temperature mechanical loading device for in situ neutron scattering measurements

Zhao, Yunlai; Zhang, Shizhong; Zhao, Hua; Sun, G. B.; Xu, Yong

doi:10.1007/s12206-022-0716-3

Cited by 3 publications

(1 citation statement)

References 22 publications

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“…However, the reported devices lack complete descriptions of temperature control, temperature calibration, or diffraction angle are missing [3]. Some tensile devices were designed in neutron scattering measurements in a range from 218 K to 473 K at 6 kN with a maximum 30 mm travel of grips [4]. Correspondingly, some researchers studied the dynamic response and bulk deformation of sample rods by utilizing quasi-static and dynamic in situ neutron diffraction techniques with a load of 30 kN at the temperature of 500 K [5].…”

Section: Introductionmentioning

confidence: 99%

Temperature calibration of sample rods for neutron diffraction apparatus in the range of 6–473 K

Zhang,

Su,

Zhou

et al. 2024

Meas. Sci. Technol.

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Internal stresses play a crucial part in determining a material's properties, which emphasizes the significance of accurate stress measurement and analysis. Neutron diffraction technology is a very promising approach to studying the complex microstructural properties of many materials, especially with the growing demand for cryogenic studies. This new device has a robust load capacity of 50 kN and works smoothly in a wide temperature range of 6 K to 473 K. Furthermore, the diffraction angle is 47 degrees broader. Regardless of the samples, we observed that a thermal balance point existed close to 180 K. Importantly, thermal resistance (TR) was eliminated by the use of an analytical method, which has an extraordinarily small error of 2%. Using this exact calibration methodology ensures that the sample temperature is accurate during the experiments. This work presents a crucial apparatus for investigating the complexity of internal stresses in materials and offers an effective method for estimating and managing sample temperatures while doing research.

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Section: Introductionmentioning

confidence: 99%

Temperature calibration of sample rods for neutron diffraction apparatus in the range of 6–473 K

Zhang,

Su,

Zhou

et al. 2024

Meas. Sci. Technol.

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A Portable Miniature Cryogenic Environment for In Situ Neutron Diffraction

Chen,

Yu,

2024

Crystals

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Neutron diffraction instruments offer a platform for materials science and engineering studies at extended temperature ranges far from ambient. As one of the widely used neutron sample environment types, cryogenic furnaces are usually bulky and complex, and they may need hours of beamtime overhead for installation, configuration, cooling, and sample change, etc. To reduce the overhead time and expedite experiments at the state-of-the-art high-flux neutron source, we developed a low-cost, miniature, and easy-to-use cryogenic environment (77–473 K) for in situ neutron diffraction. A travel-size mug serves for the environment where the samples sit inside. Immediate cooling and an isothermal dwell at 77 K are realized on the sample by direct contact with liquid N2 in the mug. The designed Al inserts serve as the holder of samples and heating elements, alleviate the thermal gradient, and clear neutron pathways. Both a single-sample continuous measurement and multi-sample high-throughput measurements are demonstrated in this environment. High-quality and refinable in situ neutron diffraction patterns are acquired on model materials. The results quantify the orthorhombic-to-cubic phase transformation process in LiMn2O4 and differentiate the anisotropic lattice thermal expansions and bond length evolutions between rhombohedral perovskite oxides with composition variation.

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