Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Bridging length scales in hard materials with ultra-small angle X-ray scattering – a critical review

Journal Article · · IUCrJ
 [1];  [2]
  1. National Institute of Standards and Technology, Gaithersburg, MD (United States)
  2. Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Owing to their exceptional properties, hard materials such as advanced ceramics, metals and composites have enormous economic and societal value, with applications across numerous industries. Understanding their microstructural characteristics is crucial for enhancing their performance, materials development and unleashing their potential for future innovative applications. However, their microstructures are unambiguously hierarchical and typically span several length scales, from sub-ångstrom to micrometres, posing demanding challenges for their characterization, especially for in situ characterization which is critical to understanding the kinetic processes controlling microstructure formation. This review provides a comprehensive description of the rapidly developing technique of ultra-small angle X-ray scattering (USAXS), a nondestructive method for probing the nano-to-micrometre scale features of hard materials. USAXS and its complementary techniques, when developed for and applied to hard materials, offer valuable insights into their porosity, grain size, phase composition and inhomogeneities. We discuss the fundamental principles, instrumentation, advantages, challenges and global status of USAXS for hard materials. Using selected examples, we demonstrate the potential of this technique for unveiling the microstructural characteristics of hard materials and its relevance to advanced materials development and manufacturing process optimization. We also provide our perspective on the opportunities and challenges for the continued development of USAXS, including multimodal characterization, coherent scattering, time-resolved studies, machine learning and autonomous experiments. Our goal is to stimulate further implementation and exploration of USAXS techniques and inspire their broader adoption across various domains of hard materials science, thereby driving the field toward discoveries and further developments.
Research Organization:
Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Organization:
USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)
Grant/Contract Number:
AC02-06CH11357
OSTI ID:
2425975
Alternate ID(s):
OSTI ID: 2564699
Journal Information:
IUCrJ, Journal Name: IUCrJ Journal Issue: 5 Vol. 11; ISSN 2052-2525
Publisher:
International Union of CrystallographyCopyright Statement
Country of Publication:
United States
Language:
English

References (113)

Nanoporous Metals with Structural Hierarchy: A Review journal August 2017
Ultra-small-angle X-ray scattering-X-ray photon correlation spectroscopy studies of incipient structural changes in amorphous calcium phosphate-based dental composites journal February 2012
Structural Characterization of RDX-Based Explosive Nanocomposites journal November 2012
Concurrent design of hierarchical materials and structures book January 2008
Transmission Electron Microscopy book January 1996
Hybrid and Hierarchical Composite Materials book January 2015
Mechanics of hierarchical materials journal March 2008
Review of the synergies between computational modeling and experimental characterization of materials across length scales journal November 2015
Hydration kinetics and morphology of cement pastes with pozzolanic volcanic ash studied via synchrotron-based techniques journal October 2017
Glassy Carbon as an Absolute Intensity Calibration Standard for Small-Angle Scattering journal August 2009
Ultra-Small-Angle X-ray Scattering Instrument at the Advanced Photon Source: History, Recent Development, and Current Status journal October 2012
Simulation of TTT Curves for Additively Manufactured Inconel 625 journal October 2018
Characterization of Complex Thermal Barrier Deposits Pore Microstructures by a Combination of Imaging, Scattering, and Intrusion Techniques journal July 2009
Phase Fraction and Evolution of Additively Manufactured (AM) 15-5 Stainless Steel and Inconel 625 AM-Bench Artifacts journal August 2019
Phase Composition and Phase Transformation of Additively Manufactured Nickel Alloy 718 AM Bench Artifacts journal February 2024
Analysis of small-angle scattering data from colloids and polymer solutions: modeling and least-squares fitting journal July 1997
Scattering studies of large scale structures at the ultra small angle neutron scattering instrument S18 journal February 2002
Relationship between differences in silica fume additives and fine-scale microstructural evolution in cement based materials journal October 1998
SAXS and SANS studies of polymer colloids journal May 2001
A new method for the quantitative analysis of the scale and composition of nanosized oxide in 9Cr-ODS steel journal October 2009
In situ structural characterization of ageing kinetics in aluminum alloy 2024 across angstrom-to-micrometer length scales journal June 2016
Effect of heat treatment on the microstructural evolution of a nickel-based superalloy additive-manufactured by laser powder bed fusion journal June 2018
Precipitation kinetics, microstructure evolution and mechanical behavior of a developed Al–Mn–Sc alloy fabricated by selective laser melting journal July 2020
Precipitation kinetics in metallic alloys: Experiments and modeling journal November 2021
Solidification modes during additive manufacturing of steel revealed by high-speed X-ray diffraction journal March 2023
A novel SAXS model for multi-texture systems: application to CaCO3 calcination using in-situ USAXS-SAXS-WAXS journal December 2022
Microstructural changes in white Portland cement paste under the first drying process evaluated by WAXS, SAXS, and USAXS journal January 2017
Ultra-small-angle scattering studies of complex fluids journal June 2005
Precipitate characterisation in metallic systems by small-angle X-ray or neutron scattering journal April 2012
Structural and dynamical studies of acid-mediated conversion in amorphous-calcium-phosphate based dental composites journal October 2014
Coupling in situ atomic force microscopy (AFM) and ultra-small-angle X-ray scattering (USAXS) to study the evolution of zinc morphology during electrodeposition within an imidazolium based ionic liquid electrolyte journal May 2020
Towards understanding the microstructural and structural changes in natural hierarchical materials for energy recovery: In-operando multi-scale X-ray scattering characterization of Na- and Ca-montmorillonite on heating to 1150 °C journal May 2017
Manufacturing and characterization of Ni-free N-containing ODS austenitic alloy journal April 2018
A brief guide to synchrotron radiation-based microtomography in (structural) geology and rock mechanics journal August 2014
Emerging X-ray imaging technologies for energy materials journal April 2020
Advanced neutron and X-ray techniques for insights into the microstructure of EB-PVD thermal barrier coatings journal June 2006
Processes controlling helium bubble dynamics at varying temperatures in simulated radioactive materials journal September 2022
DND-CAT's new triple area detector system for simultaneous data collection at multiple length scales
  • Weigand, Steven J.; Keane, Denis T.
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 649, Issue 1 https://doi.org/10.1016/j.nima.2010.12.045
journal September 2011
Ultra-small-angle scattering with polarized neutrons journal July 2007
Nature’s hierarchical materials journal November 2007
Application of USAXS analysis and non-interacting approximation to determine the influence of process parameters and ageing on the thermal conductivity of electron-beam physical vapor deposited thermal barrier coatings journal January 2007
In Situ Angstrom-to-Micrometer Characterization of the Structural and Microstructural Changes in Kaolinite on Heating Using Ultrasmall-Angle, Small-Angle, and Wide-Angle X-ray Scattering (USAXS/SAXS/WAXS) journal October 2017
Pressure-Thresholded Response in Cylindrically Shocked Cyclotrimethylene Trinitramine (RDX) journal February 2020
Machine Learning Automated Analysis of Enormous Synchrotron X-ray Diffraction Datasets journal July 2023
In Situ Structural and Electrical Conductivity Characterization of Sr2MMoO6−δ Double Perovskite Solid Oxide Fuel Cell Anode Materials journal May 2020
Synchrotron Imaging of Pore Formation in Li Metal Solid-State Batteries Aided by Machine Learning journal September 2020
Impact of Catalyst Ink Dispersing Methodology on Fuel Cell Performance Using in-Situ X-ray Scattering journal July 2019
Dehydration Effect on the Pore Size, Porosity, and Fractal Parameters of Shale Rocks: Ultrasmall-Angle X-ray Scattering Study journal October 2014
Structure of Age-Hardened Aluminium-Copper Alloys journal September 1938
X-ray focusing with efficient high-NA multilayer Laue lenses journal November 2017
Structural analysis of hierarchically organized zeolites journal October 2015
Coherent lensless X-ray imaging journal November 2010
Multipurpose soft-material SAXS/WAXS/GISAXS beamline at SPring-8 journal March 2011
Quantification of Thermal Oxidation in Metallic Glass Powder using Ultra-small Angle X-ray Scattering journal May 2019
Grain boundary widening controls siderite (FeCO3) replacement of limestone (CaCO3) journal March 2023
Hybrid microstructure of smectite clay gels revealed using neutron and synchrotron X-ray scattering journal November 2023
X-ray computed tomography journal February 2021
Hierarchical porous materials: catalytic applications journal January 2013
Hierarchical photocatalysts journal January 2016
Hierarchically porous materials: synthesis strategies and structure design journal January 2017
Novel aqueous amine looping approach for the direct capture, conversion and storage of CO 2 to produce magnesium carbonate journal January 2020
Effective pinhole-collimated ultrasmall-angle x-ray scattering instrument for measuring anisotropic microstructures journal March 2002
An X‐Ray Interferometer journal April 1965
Tailless X‐Ray Single‐Crystal Reflection Curves Obtained by Multiple Reflection journal November 1965
Kinetic transition in the growth of Al nanocrystals in Al-Sm alloys journal March 2012
Correlating chemistry and mass transport in sustainable iron production journal October 2023
Multi-bend Achromat Lattices for Storage Ring Light Sources journal November 2014
Coherent Diffractive Imaging at the High-Energy PETRA III Synchrotron Storage Ring journal June 2020
Recent developments in ultra–small angle neutron scattering techniques journal January 1998
Ultra-Small-Angle X-ray Scattering of Polymers journal February 2010
Diffraction enhanced x-ray imaging journal November 1997
Computed tomography of x-ray index of refraction using the diffraction enhanced imaging method journal March 2000
Ultra-small-angle X-ray diffraction and scattering experiments using medium-length beamlines at SPring-8 journal April 2003
X-ray imaging with ultra-small-angle X-ray scattering as a contrast mechanism journal September 2004
Quantitative characterization of the contrast mechanisms of ultra-small-angle X-ray scattering imaging journal March 2008
Ultra-small-angle X-ray scattering at the Advanced Photon Source journal April 2009
Development of ultra-small-angle X-ray scattering–X-ray photon correlation spectroscopy journal January 2011
High-energy ultra-small-angle X-ray scattering instrument at the Advanced Photon Source journal November 2012
Kookaburra: the ultra-small-angle neutron scattering instrument at OPAL journal October 2013
High-resolution small-angle X-ray scattering camera for anomalous scattering journal February 1991
Small-Angle X-ray Scattering of Inorganic Glasses. Data Treatment and Analysis journal December 1997
Construction of a Two-Dimensional Ultra-Small-Angle X-ray Scattering Apparatus journal October 1997
In-situ observation of small-angle X-ray scattering by dislocations journal June 2000
Ultra-small-angle X-ray scattering from dislocation structures journal October 2005
Cateretê: the coherent X-ray scattering beamline at the fourth-generation synchrotron facility SIRIUS journal August 2021
An iterative method of slit-correcting small angle X-ray data journal August 1967
A new method of evaluating slit-smeared small-angle X-ray scattering data journal May 1970
A twelve-analyzer detector system for high-resolution powder diffraction journal July 2008
P03, the microfocus and nanofocus X-ray scattering (MiNaXS) beamline of the PETRA III storage ring: the microfocus endstation journal May 2012
NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering journal March 2017
An in situ USAXS–SAXS–WAXS study of precipitate size distribution evolution in a model Ni-based alloy journal May 2017
Inverse transformation: unleashing spatially heterogeneous dynamics with an alternative approach to XPCS data analysis journal February 2018
CONTIN XPCS : software for inverse transform analysis of X-ray photon correlation spectroscopy dynamics journal February 2018
Development of combined microstructure and structure characterization facility for in situ and operando studies at the Advanced Photon Source journal June 2018
A multipurpose instrument for time-resolved ultra-small-angle and coherent X-ray scattering journal October 2018
Classifying and analyzing small-angle scattering data using weighted k nearest neighbors machine learning techniques journal February 2020
Performance of the time-resolved ultra-small-angle X-ray scattering beamline with the Extremely Brilliant Source journal February 2022
Performance of the new biological small- and wide-angle X-ray scattering beamline 13A at the Taiwan Photon Source journal March 2022
High-efficiency coherence-preserving harmonic rejection with crystal optics journal August 2018
Extending synchrotron SAXS instrument ranges through addition of a portable, inexpensive USAXS module with vertical rotation axes journal April 2021
Improvement of ultra-small-angle XPCS with the Extremely Brilliant Source journal January 2024
Microstructure-Property Correlations in Industrial Thermal Barrier Coatings journal July 2004
Characterization of Ceramics by X-Ray and Neutron Small-Angle Scattering journal June 2005
In situ characterization of ceramic cold sintering by small‐angle scattering journal February 2021
Three-dimensional visualization of nanoparticle lattices and multimaterial frameworks journal April 2022
Cold Sintering: Progress, Challenges, and Future Opportunities journal July 2019
Hard X-Ray Photon Correlation Spectroscopy Methods for Materials Studies journal July 2018
X-ray Energy Dependence of the Properties of the Focused Beams Produced by Polycapillary X-ray Lens journal July 2008
Solid-State Transformation of an Additive Manufactured Inconel 625 Alloy at 700 °C journal September 2021
In Situ Microstructure Characterization of Potassium Di-Phosphate (KDP) Densification during Cold Sintering journal October 2022
How Austenitic Is a Martensitic Steel Produced by Laser Powder Bed Fusion? A Cautionary Tale journal November 2021
Connecting the Morphological and Crystal Structural Changes during the Conversion of Lithium Hydroxide Monohydrate to Lithium Carbonate Using Multi-Scale X-ray Scattering Measurements journal September 2017
The high resolution powder diffraction beam line at ESRF journal January 2004

Similar Records

Bridging Structural and Chemical Insights: Integrating In Situ Electron Microscopy and X-ray Spectroscopy for Catalysis Research
Journal Article · Tue Jun 17 20:00:00 EDT 2025 · Journal of Physical Chemistry Letters · OSTI ID:2572412

Bridging the length scales on mechanical property evaluation (Final Report)
Technical Report · Wed Nov 30 23:00:00 EST 2022 · OSTI ID:1907269