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Title: Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source

Abstract

Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. But, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elastic and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. Furthermore,more » to demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr 64Ni 36 measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample ( 100 mg).« less

Authors:
 [1]; ORCiD logo [2];  [3]; ORCiD logo [3];  [4];  [4];  [5];  [6];  [2]; ORCiD logo [2]; ORCiD logo [7];  [4];  [8];  [3]
  1. North Central College, Naperville, IL (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  3. Washington Univ., St. Louis, MO (United States)
  4. Iowa State Univ., Ames, IA (United States)
  5. Iowa State Univ., Ames, IA (United States); Ames Lab., Ames, IA (United States)
  6. Univ. of Tennessee, Knoxville, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  7. City Univ., of Hong Kong (China)
  8. Univ. of Tennessee, Knoxville, TN (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1265812
Alternate Identifier(s):
OSTI ID: 1235380
Grant/Contract Number:
AC05-00OR22725; AC02-07CH11358
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 87; Journal Issue: 1; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY

Citation Formats

Mauro, N. A., Vogt, A. J., Derendorf, K. S., Johnson, M. L., Rustan, G. E., Quirinale, D. G., Kreyssig, A., Lokshin, K. A., Neuefeind, J. C., An, Ke, Wang, Xun-Li, Goldman, A. I., Egami, T., and Kelton, K. F. Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source. United States: N. p., 2016. Web. doi:10.1063/1.4939194.
Mauro, N. A., Vogt, A. J., Derendorf, K. S., Johnson, M. L., Rustan, G. E., Quirinale, D. G., Kreyssig, A., Lokshin, K. A., Neuefeind, J. C., An, Ke, Wang, Xun-Li, Goldman, A. I., Egami, T., & Kelton, K. F. Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source. United States. doi:10.1063/1.4939194.
Mauro, N. A., Vogt, A. J., Derendorf, K. S., Johnson, M. L., Rustan, G. E., Quirinale, D. G., Kreyssig, A., Lokshin, K. A., Neuefeind, J. C., An, Ke, Wang, Xun-Li, Goldman, A. I., Egami, T., and Kelton, K. F. Fri . "Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source". United States. doi:10.1063/1.4939194. https://www.osti.gov/servlets/purl/1265812.
@article{osti_1265812,
title = {Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source},
author = {Mauro, N. A. and Vogt, A. J. and Derendorf, K. S. and Johnson, M. L. and Rustan, G. E. and Quirinale, D. G. and Kreyssig, A. and Lokshin, K. A. and Neuefeind, J. C. and An, Ke and Wang, Xun-Li and Goldman, A. I. and Egami, T. and Kelton, K. F.},
abstractNote = {Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. But, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elastic and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. Furthermore, to demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr64Ni36 measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample ( 100 mg).},
doi = {10.1063/1.4939194},
journal = {Review of Scientific Instruments},
number = 1,
volume = 87,
place = {United States},
year = {Fri Jan 01 00:00:00 EST 2016},
month = {Fri Jan 01 00:00:00 EST 2016}
}

Journal Article:
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Cited by: 6works
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  • Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. However, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elasticmore » and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. To demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr{sub 64}Ni{sub 36} measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample (∼100 mg)« less
  • Cited by 6
  • High-energy x-ray diffraction studies of metallic liquids provide valuable information about structural evolution on the atomic length scale, leading to insights into the origin of the nucleation barrier and the processes of supercooling and glass formation. The containerless processing of the beamline electrostatic levitation (BESL) facility allows coordinated thermophysical and structural studies of equilibrium and supercooled liquids to be made in a contamination-free, high-vacuum ({approx}10{sup -8} Torr) environment. To date, the incorporation of electrostatic levitation facilities into synchrotron beamlines has been difficult due to the large footprint of the apparatus and the difficulties associated with its transportation and implementation. Here,more » we describe a modular levitation facility that is optimized for diffraction studies of high-temperature liquids at high-energy synchrotron beamlines. The modular approach used in the apparatus design allows it to be easily transported and quickly setup. Unlike most previous electrostatic levitation facilities, BESL can be operated by a single user instead of a user team.« less
  • We describe a new high temperature environment based on aerodynamic levitation and laser heating designed for neutron scattering experiments up to 3000 deg. C. The sample is heated to the desired temperature with three CO{sub 2} lasers from different directions in order to obtain a homogeneous temperature distribution. The apparent temperature of the sample is measured with an optical pyrometer, and two video cameras are employed to monitor the sample behavior during heating. The levitation setup is enclosed in a vacuum-tight chamber, enabling a high degree of gas purity and a reproducible sample environment for structural investigations on both oxidemore » and metallic melts. High-quality neutron diffraction data have been obtained on liquid Y{sub 3}Al{sub 5}O{sub 12} and ZrNi alloy for relatively short counting times (1.5 h)« less
  • A new levitation apparatus coupled to a synchrotron-derived x-ray source has been developed to study the structure of liquids at temperatures up to 3000 K. The levitation apparatus employs conical nozzle levitation using aerodynamic forces to stably position solid and liquid specimens at high temperatures. A 270 W CO{sub 2} laser was used to heat the specimens to desired temperatures. Two optical pyrometers were used to record the specimen temperature, heating curves, and cooling curves. Three video cameras and a video recorder were employed to obtain and record specimen views in all three dimensions. The levitation assembly was supported onmore » a three-axis translation stage to facilitate precise positioning of the specimen in the synchrotron radiation beam. The levitation system was enclosed in a vacuum chamber with Be windows, connections for vacuum and gas flow, ports for pyrometry, video, and pressure measurements. The vacuum system included automatic pressure control and multi-channel gas flow control. A phosphor screen coupled to a high-resolution video microscope provided images of the x-ray beam and specimen shadow which were used to establish the specimen position. The levitation apparatus was integrated with x-ray diffractometers located at X-6B and X-25 beamlines at the National Synchrotron Light Source. X-ray structural measurements have been obtained on a number of materials including Al{sub 2}O{sub 3}, Ni, Si, Ge, and other metallic and ceramic materials in the liquid state. {copyright} {ital 1997 American Institute of Physics. }« less