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Related Concept Videos

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Ionic Crystal Structures

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Related Experiment Video

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Resolving the Atomic Structure of Sequential Infiltration Synthesis Derived Inorganic Clusters.

Xiang He, Ruben Z Waldman1, David J Mandia

  • 1Pritzker School of Molecular Engineering, University of Chicago, Chicago, Illinois 60637, United States.

ACS Nano
|November 10, 2020
PubMed
Summary

Sequential infiltration synthesis (SIS) precisely deposits inorganic solids within polymer templates. This study reveals the atomic structure of indium oxide hydroxide clusters and their evolution into porous indium oxide solids after template removal.

Keywords:
X-ray characterizationindium oxidepair distribution functionsequential infiltration synthesistransmission electron microscopy

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Area of Science:

  • Materials Science
  • Nanotechnology
  • Inorganic Chemistry

Background:

  • Sequential infiltration synthesis (SIS) allows precise inorganic material deposition within soft templates, enabling complex nanoscale structures.
  • Previous SIS studies focused on morphology, but the initial growth stages and atomic structure of nuclei remained unclear.
  • Understanding early SIS growth is crucial for controlling the formation of advanced inorganic nanostructures.

Purpose of the Study:

  • To investigate the structural evolution of indium oxide hydroxide (InO(OH)) clusters during Sequential Infiltration Synthesis (SIS) within a poly(methyl methacrylate) (PMMA) template.
  • To characterize the formation of porous indium oxide (In2O3) solids after PMMA template removal and annealing.
  • To determine how the number of SIS cycles influences the atomic structure and morphology of the resulting inorganic materials.

Main Methods:

  • Utilized In K-edge extended X-ray absorption fine structure (EXAFS) spectroscopy.
  • Employed atomic pair distribution function (PDF) analysis from high-energy X-ray scattering.
  • Analyzed samples as a function of Sequential Infiltration Synthesis (SIS) cycle number.

Main Results:

  • Early SIS cycles produced high-aspect-ratio InO(OH) clusters, evolving into a 3D network with increased cycling.
  • Atomic structures of InO(OH) clusters resemble multinuclear clusters with bonding patterns related to In2O3 and In(OH)3.
  • Annealing removed the PMMA template and formed cubic In2O3 nanocrystals, with structural details dependent on SIS cycle number.

Conclusions:

  • SIS enables the formation of InO(OH) clusters with structures predictive of 3D arrays of discrete-atom-number clusters.
  • The study elucidates the atomic-level transformation from clusters within a template to porous In2O3 solids.
  • SIS offers a versatile route for creating complex inorganic nanostructures with tunable properties based on synthesis parameters.