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Title: Understanding Synthesis and Structural Variation of Nanomaterials Through In Situ/Operando XAS and SAXS

Journal Article · · Small
 [1];  [2];  [2]; ORCiD logo [3]
  1. Northern Illinois Univ., DeKalb, IL (United States)
  2. Argonne National Lab. (ANL), Argonne, IL (United States)
  3. Northern Illinois Univ., DeKalb, IL (United States); Argonne National Lab. (ANL), Argonne, IL (United States)

Nanostructured materials with high surface area and low coordinated atoms present distinct intrinsic properties from their bulk counterparts. However, nanomaterials' nucleation/growth mechanism during the synthesis process and the changes of the nanomaterials in the working state are still not thoroughly studied. As two indispensable methods, X-ray absorption spectroscopy (XAS) provides nanomaterials' electronic structure and coordination environment, while small-angle X-ray scattering (SAXS) offers structural properties and morphology information. Here, a combination of in situ/operando XAS and SAXS provides high temporal and spatial resolution to monitor the evolution of nanomaterials. This review gives a brief introduction to in situ/operando SAXS/XAS cells. In addition, the application of in situ/operando XAS and SAXS in preparing nanomaterials and studying changes of working nanomaterials are summarized.

Research Organization:
Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities Division; National Science Foundation (NSF)
Grant/Contract Number:
AC02-06CH11357
OSTI ID:
1903019
Journal Information:
Small, Journal Name: Small Journal Issue: 19 Vol. 18; ISSN 1613-6810
Publisher:
WileyCopyright Statement
Country of Publication:
United States
Language:
English

References (70)

Manganese Oxide Nanomaterials: Synthesis, Properties, and Theranostic Applications journal January 2020
Insights into the Nanostructure, Solvation, and Dynamics of Liquid Electrolytes through Small‐Angle X‐Ray Scattering journal December 2020
Surface Reconstruction of Ultrathin Palladium Nanosheets during Electrocatalytic CO 2 Reduction journal September 2020
Electroreduction of CO 2 on Single-Site Copper-Nitrogen-Doped Carbon Material: Selective Formation of Ethanol and Reversible Restructuration of the Metal Sites journal September 2019
Size‐Dependent Activity and Selectivity of Atomic‐Level Copper Nanoclusters during CO/CO 2 Electroreduction journal October 2020
The Pyridyl Functional Groups Guide the Formation of Pd Nanoparticles Inside A Porous Poly(4-Vinyl-Pyridine) journal July 2015
Effect of Particle Size upon Pt/SiO 2 Catalytic Cracking of n -Dodecane under Supercritical Conditions: In situ SAXS and XANES Studies journal November 2016
On the Formation of Palladium (II) Iodide Nanoparticles: An In Situ SAXS/XAS Study and Catalytic Evaluation on an Aryl Alkenylation Reaction in Water Medium journal December 2018
Activation of Co−Mo−S Hydrodesulfurization Catalysts Under Refinery Conditions‐A Combined SAXS/XAS Study journal September 2019
Few‐Layered Tin Sulfide Nanosheets Supported on Reduced Graphene Oxide as a High‐Performance Anode for Potassium‐Ion Batteries journal February 2019
Operando XAS/SAXS: Guiding Design of Single‐Atom and Subnanocluster Catalysts journal February 2021
A Review of Grazing Incidence Small‐ and Wide‐Angle X‐Ray Scattering Techniques for Exploring the Film Morphology of Organic Solar Cells journal August 2020
Switchable CO2 electroreduction via engineering active phases of Pd nanoparticles journal April 2017
In Situ X-ray Absorption Spectroscopy Studies of Nanoscale Electrocatalysts journal June 2019
A review of the electrochemical performance of alloy anodes for lithium-ion batteries journal January 2011
Monitoring and quantifying morphological and structural changes in electrode materials under operando conditions journal December 2020
Prospective of combustion method for preparation of nanomaterials: A challenge journal May 2021
Preparation of silicon nanomaterials by arc discharge journal December 2015
Simultaneous measurement of X-ray small angle scattering, absorption and reactivity: A continuous flow catalysis reactor
  • Lee, Sungsik; Lee, Byeongdu; Seifert, Soenke
  • 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.2010.12.172
journal September 2011
Restructuring in block copolymer thin films: In situ GISAXS investigations during solvent vapor annealing journal March 2017
Exploring Pore Formation of Atomic Layer-Deposited Overlayers by in Situ Small- and Wide-Angle X-ray Scattering journal September 2016
In Situ / Operando Electrocatalyst Characterization by X-ray Absorption Spectroscopy journal September 2020
Small Angle X-ray Scattering for Nanoparticle Research journal April 2016
Emerging Two-Dimensional Nanomaterials for Electrocatalysis journal March 2018
Two-Dimensional Metal Nanomaterials: Synthesis, Properties, and Applications journal June 2018
Temperature-Dependent Evolution of the Oxidation States of Cobalt and Platinum in Co 1– x Pt x Clusters under H 2 and CO + H 2 Atmospheres journal September 2016
Revisiting the ZnO Q-dot Formation Toward an Integrated Growth Model: From Coupled Time Resolved UV–Vis/SAXS/XAS Data to Multivariate Analysis journal December 2016
Inherent Size Effects on XANES of Nanometer Metal Clusters: Size-Selected Platinum Clusters on Silica journal December 2016
In Situ Time-Resolved X-ray Absorption Fine Structure and Small Angle X-ray Scattering Revealed an Unexpected Phase Structure Transformation during the Growth of Nickel Phosphide Nanoparticles journal June 2018
Subnanometer Substructures in Nanoassemblies Formed from Clusters under a Reactive Atmosphere Revealed Using Machine Learning journal August 2018
Insights from In Situ Studies on the Early Stages of Platinum Nanoparticle Formation journal March 2021
A New Insight into Growth Mechanism and Kinetics of Mesoporous Silica Nanoparticles by in Situ Small Angle X-ray Scattering journal July 2015
Structure-Sensitive CO 2 Electroreduction to Hydrocarbons on Ultrathin 5-fold Twinned Copper Nanowires journal January 2017
Ultrathin Bismuth Nanosheets for Stable Na-Ion Batteries: Clarification of Structure and Phase Transition by in Situ Observation journal January 2019
Encapsulation Methods for Control of Catalyst Deactivation: A Review journal June 2020
CO 2 Methanation on Cu-Cluster Decorated Zirconia Supports with Different Morphology: A Combined Experimental In Situ GIXANES/GISAXS, Ex Situ XPS and Theoretical DFT Study journal May 2021
In Situ XAS/SAXS Study of Al 2 O 3 -Coated PtGa Catalysts for Propane Dehydrogenation journal August 2021
Combining SAXS and XAS To Study the Operando Degradation of Carbon-Supported Pt-Nanoparticle Fuel Cell Catalysts journal June 2018
Dynamic Behavior of Pd/P4VP Catalyst during the Aerobic Oxidation of 2-Propanol: A Simultaneous SAXS/XAS/MS Operando Study journal June 2018
Insights into the Degradation Mechanism of Nanoporous Alloy-Type Li-Ion Battery Anodes journal April 2021
Mechanisms of SnO 2 Nanoparticles Formation and Growth in Acid Ethanol Solution Derived from SAXS and Combined Raman–XAS Time-Resolved Studies journal November 2014
Direct Synthesis of Controllable Microstructures of Thermally Stable and Ordered Mesoporous Crystalline Titanium Oxides and Carbide/Carbon Composites journal March 2010
X-ray Absorption Spectroscopy of Low Temperature Fuel Cell Catalysts journal October 2004
Concerted Growth and Ordering of Cobalt Nanorod Arrays as Revealed by Tandem in Situ SAXS-XAS Studies journal June 2016
Reduction-Triggered Self-Assembly of Nanoscale Molybdenum Oxide Molecular Clusters journal August 2016
In Situ X-ray Absorption Spectroscopy of a Synergistic Co–Mn Oxide Catalyst for the Oxygen Reduction Reaction journal December 2018
Evolution Pathway from Iron Compounds to Fe 1 (II)–N 4 Sites through Gas-Phase Iron during Pyrolysis journal December 2019
Formation and Growth of Pd Nanoparticles Inside a Highly Cross-Linked Polystyrene Support: Role of the Reducing Agent journal April 2014
Promises and challenges of nanomaterials for lithium-based rechargeable batteries journal June 2016
The role of nanotechnology in the development of battery materials for electric vehicles journal December 2016
Highly selective electrocatalytic CO2 reduction to ethanol by metallic clusters dynamically formed from atomically dispersed copper journal July 2020
Following the structure of copper-zinc-alumina across the pressure gap in carbon dioxide hydrogenation journal June 2021
Size- and shape-dependent catalytic performances of oxidation and reduction reactions on nanocatalysts journal January 2016
In situ , operando studies on the size and structure of supported Pt catalysts under supercritical conditions by simultaneous synchrotron-based X-ray techniques journal January 2019
Operando X-ray characterization of high surface area iridium oxides to decouple their activity losses for the oxygen evolution reaction journal January 2019
An in situ SAXS investigation of the formation of silver nanoparticles and bimetallic silver–gold nanoparticles in controlled wet-chemical reduction synthesis journal January 2020
Nanomaterials: a review of synthesis methods, properties, recent progress, and challenges journal January 2021
The role of pre-nucleation clusters in the crystallization of gold nanoparticles journal January 2020
Following the formation of nanometer-sized clusters by time-resolved SAXS and EXAFS techniques journal October 2002
Combined TPRx, in situ GISAXS and GIXAS studies of model semiconductor-supported platinum catalysts in the hydrogenation of ethene journal January 2010
Nanostructured metal chalcogenides: synthesis, modification, and applications in energy conversion and storage devices journal January 2013
Nanomaterials for energy conversion and storage journal January 2013
Copper nanoparticle ensembles for selective electroreduction of CO 2 to C 2 –C 3 products journal September 2017
A versatile sample-environment cell for non-ambient X-ray scattering experiments journal July 2008
The AMPIX electrochemical cell: a versatile apparatus for in situ X-ray scattering and spectroscopic measurements journal November 2012
A radially accessible tubular in situ X-ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices journal September 2016
Electrochemical Flow-Cell Setup for In Situ X-ray Investigations: I. Cell for SAXS and XAS at Synchrotron Facilities journal January 2016
Small Angle X-Ray Scattering Technique for the Particle Size Distribution of Nonporous Nanoparticles journal December 2013
Review of Research on Template Methods in Preparation of Nanomaterials journal January 2016
Heterogeneous Catalyst Deactivation and Regeneration: A Review journal February 2015