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Title: Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements

Abstract

In situ measurements of geological materials under compression and with hydrostatic fluid pressure are important in understanding their behavior under field conditions, which in turn provides critical information for application-driven research. In particular, understanding the role of nano- to micro-scale porosity in the subsurface liquid and gas flow is critical for the high-fidelity characterization of the transport and more efficient extraction of the associated energy resources. In other applications, where parts are produced by the consolidation of powders by compression, the resulting porosity and crystallite orientation (texture) may affect its in-use characteristics. Small-angle neutron scattering (SANS) and ultra SANS are ideal probes for characterization of these porous structures over the nano to micro length scales. Here we show the design, realization, and performance of a novel neutron scattering sample environment, a specially designed compression cell, which provides compressive stress and hydrostatic pressures with effective stress up to 60 MPa, using the neutron beam to probe the effects of stress vectors parallel to the neutron beam. In conclusion, we demonstrate that the neutron optics is suitable for the experimental objectives and that the system is highly stable to the stress and pressure conditions of the measurements.

Authors:
 [1];  [1]; ORCiD logo [1];  [1]; ORCiD logo [1]; ORCiD logo [1];  [2]; ORCiD logo [3];  [4];  [4]
  1. Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
  2. National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States)
  3. Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  4. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Publication Date:
Research Org.:
Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Fossil Energy (FE); National Science Foundation (NSF)
OSTI Identifier:
1481976
Alternate Identifier(s):
OSTI ID: 1639078
Report Number(s):
LA-UR-18-20274; SAND-2020-6571J
Journal ID: ISSN 0034-6748
Grant/Contract Number:  
AC52-06NA25396; AC04-94AL85000; SC0006883; NA0003525; FWP FE-406/408/409; DMR-1508249
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 89; Journal Issue: 5; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION; Particle beams; physics of gases; hydrostatics; neutron optics; geological materials; compressive stress; neutron scattering; transition metals; measurement theory

Citation Formats

Hjelm, Rex P., Taylor, Mark A., Frash, Luke P., Hawley, Marilyn E., Ding, Mei, Xu, Hongwu, Barker, John, Olds, Daniel, Heath, Jason, and Dewers, Thomas. Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements. United States: N. p., 2018. Web. https://doi.org/10.1063/1.5022678.
Hjelm, Rex P., Taylor, Mark A., Frash, Luke P., Hawley, Marilyn E., Ding, Mei, Xu, Hongwu, Barker, John, Olds, Daniel, Heath, Jason, & Dewers, Thomas. Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements. United States. https://doi.org/10.1063/1.5022678
Hjelm, Rex P., Taylor, Mark A., Frash, Luke P., Hawley, Marilyn E., Ding, Mei, Xu, Hongwu, Barker, John, Olds, Daniel, Heath, Jason, and Dewers, Thomas. Tue . "Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements". United States. https://doi.org/10.1063/1.5022678. https://www.osti.gov/servlets/purl/1481976.
@article{osti_1481976,
title = {Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements},
author = {Hjelm, Rex P. and Taylor, Mark A. and Frash, Luke P. and Hawley, Marilyn E. and Ding, Mei and Xu, Hongwu and Barker, John and Olds, Daniel and Heath, Jason and Dewers, Thomas},
abstractNote = {In situ measurements of geological materials under compression and with hydrostatic fluid pressure are important in understanding their behavior under field conditions, which in turn provides critical information for application-driven research. In particular, understanding the role of nano- to micro-scale porosity in the subsurface liquid and gas flow is critical for the high-fidelity characterization of the transport and more efficient extraction of the associated energy resources. In other applications, where parts are produced by the consolidation of powders by compression, the resulting porosity and crystallite orientation (texture) may affect its in-use characteristics. Small-angle neutron scattering (SANS) and ultra SANS are ideal probes for characterization of these porous structures over the nano to micro length scales. Here we show the design, realization, and performance of a novel neutron scattering sample environment, a specially designed compression cell, which provides compressive stress and hydrostatic pressures with effective stress up to 60 MPa, using the neutron beam to probe the effects of stress vectors parallel to the neutron beam. In conclusion, we demonstrate that the neutron optics is suitable for the experimental objectives and that the system is highly stable to the stress and pressure conditions of the measurements.},
doi = {10.1063/1.5022678},
journal = {Review of Scientific Instruments},
number = 5,
volume = 89,
place = {United States},
year = {2018},
month = {5}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Figures / Tables:

Figure 1 Figure 1: Compression cell assembly in cross section. The ram assembly, containing a sapphire neutron window, applies stress on the sample that is placed between the ram and a fixed plate, which holds a second neutron window. Hydrostatic fluid pressure is applied through the fluid ports. The incident neutron beammore » passes through a channel in the ram assembly, sapphire window and sample. The scattered beam exits the sample chamber through the second neutron window. A gadolinium foil lining controls reflections from the channel walls and the beam size is matched to the compression cell beam acceptance angles using a ¼ inch (6.3 mm) cadmium incident beam aperture.« less

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