Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al2O3 Nanocrystals

Zichang Xiong; Himashi P. Andaraarachchi; Jacob T. Held; Rick W. Dorn; Yong Jin Jeong; Aaron Rossini; Uwe R. Kortshagen

doi:10.3390/nano13101627

Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al₂O₃ Nanocrystals

Zichang Xiong, Himashi P. Andaraarachchi, Jacob T. Held, Rick W. Dorn, Yong Jin Jeong, Aaron Rossini, Uwe R. Kortshagen

Research output: Contribution to journal › Article › peer-review

2 Scopus citations

Abstract

Gamma alumina (γ-Al₂O₃) is widely used as a catalyst and catalytic support due to its high specific surface area and porosity. However, synthesis of γ-Al₂O₃ nanocrystals is often a complicated process requiring high temperatures or additional post-synthetic steps. Here, we report a single-step synthesis of size-controlled and monodisperse, facetted γ-Al₂O₃ nanocrystals in an inductively coupled nonthermal plasma reactor using trimethylaluminum and oxygen as precursors. Under optimized conditions, we observed phase-pure, cuboctahedral γ-Al₂O₃ nanocrystals with defined surface facets. Nuclear magnetic resonance studies revealed that nanocrystal surfaces are populated with AlO₆, AlO₅ and AlO₄ units with clusters of hydroxyl groups. Nanocrystal size tuning was achieved by varying the total reactor pressure yielding particles as small as 3.5 nm, below the predicted thermodynamic stability limit for γ-Al₂O₃.

Original language	English (US)
Article number	1627
Journal	Nanomaterials
Volume	13
Issue number	10
DOIs	https://doi.org/10.3390/nano13101627
State	Published - May 2023

Bibliographical note

Funding Information:
This research was supported by the Army Research Office under MURI Grant W911NF-18-1-0240. Parts of this work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from the US National Science Foundation through the MRSEC (Award Number DMR-2011401) and the NNCI (Award Number ECCS-2025124) programs. Solid-State NMR Spectroscopy (R.D. and A.R.) was supported work was supported by the National Science Foundation under Grant No. CBET-1916809. 19.6 T NMR experiments were performed at the National High Magnetic Field Laboratory. The National High Magnetic Field Laboratory is supported by the National Science Foundation through NSF/DMR-1644779 and the State of Florida.

Publisher Copyright:
© 2023 by the authors.

Keywords

gamma alumina
nonthermal plasma
size-control

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title = "Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al2O3 Nanocrystals",

abstract = "Gamma alumina (γ-Al2O3) is widely used as a catalyst and catalytic support due to its high specific surface area and porosity. However, synthesis of γ-Al2O3 nanocrystals is often a complicated process requiring high temperatures or additional post-synthetic steps. Here, we report a single-step synthesis of size-controlled and monodisperse, facetted γ-Al2O3 nanocrystals in an inductively coupled nonthermal plasma reactor using trimethylaluminum and oxygen as precursors. Under optimized conditions, we observed phase-pure, cuboctahedral γ-Al2O3 nanocrystals with defined surface facets. Nuclear magnetic resonance studies revealed that nanocrystal surfaces are populated with AlO6, AlO5 and AlO4 units with clusters of hydroxyl groups. Nanocrystal size tuning was achieved by varying the total reactor pressure yielding particles as small as 3.5 nm, below the predicted thermodynamic stability limit for γ-Al2O3.",

keywords = "gamma alumina, nonthermal plasma, size-control",

author = "Zichang Xiong and Andaraarachchi, {Himashi P.} and Held, {Jacob T.} and Dorn, {Rick W.} and Jeong, {Yong Jin} and Aaron Rossini and Kortshagen, {Uwe R.}",

note = "Funding Information: This research was supported by the Army Research Office under MURI Grant W911NF-18-1-0240. Parts of this work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from the US National Science Foundation through the MRSEC (Award Number DMR-2011401) and the NNCI (Award Number ECCS-2025124) programs. Solid-State NMR Spectroscopy (R.D. and A.R.) was supported work was supported by the National Science Foundation under Grant No. CBET-1916809. 19.6 T NMR experiments were performed at the National High Magnetic Field Laboratory. The National High Magnetic Field Laboratory is supported by the National Science Foundation through NSF/DMR-1644779 and the State of Florida. Publisher Copyright: {\textcopyright} 2023 by the authors.",

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AU - Xiong, Zichang

AU - Andaraarachchi, Himashi P.

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AU - Dorn, Rick W.

AU - Jeong, Yong Jin

AU - Rossini, Aaron

AU - Kortshagen, Uwe R.

N1 - Funding Information: This research was supported by the Army Research Office under MURI Grant W911NF-18-1-0240. Parts of this work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from the US National Science Foundation through the MRSEC (Award Number DMR-2011401) and the NNCI (Award Number ECCS-2025124) programs. Solid-State NMR Spectroscopy (R.D. and A.R.) was supported work was supported by the National Science Foundation under Grant No. CBET-1916809. 19.6 T NMR experiments were performed at the National High Magnetic Field Laboratory. The National High Magnetic Field Laboratory is supported by the National Science Foundation through NSF/DMR-1644779 and the State of Florida. Publisher Copyright: © 2023 by the authors.

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N2 - Gamma alumina (γ-Al2O3) is widely used as a catalyst and catalytic support due to its high specific surface area and porosity. However, synthesis of γ-Al2O3 nanocrystals is often a complicated process requiring high temperatures or additional post-synthetic steps. Here, we report a single-step synthesis of size-controlled and monodisperse, facetted γ-Al2O3 nanocrystals in an inductively coupled nonthermal plasma reactor using trimethylaluminum and oxygen as precursors. Under optimized conditions, we observed phase-pure, cuboctahedral γ-Al2O3 nanocrystals with defined surface facets. Nuclear magnetic resonance studies revealed that nanocrystal surfaces are populated with AlO6, AlO5 and AlO4 units with clusters of hydroxyl groups. Nanocrystal size tuning was achieved by varying the total reactor pressure yielding particles as small as 3.5 nm, below the predicted thermodynamic stability limit for γ-Al2O3.

AB - Gamma alumina (γ-Al2O3) is widely used as a catalyst and catalytic support due to its high specific surface area and porosity. However, synthesis of γ-Al2O3 nanocrystals is often a complicated process requiring high temperatures or additional post-synthetic steps. Here, we report a single-step synthesis of size-controlled and monodisperse, facetted γ-Al2O3 nanocrystals in an inductively coupled nonthermal plasma reactor using trimethylaluminum and oxygen as precursors. Under optimized conditions, we observed phase-pure, cuboctahedral γ-Al2O3 nanocrystals with defined surface facets. Nuclear magnetic resonance studies revealed that nanocrystal surfaces are populated with AlO6, AlO5 and AlO4 units with clusters of hydroxyl groups. Nanocrystal size tuning was achieved by varying the total reactor pressure yielding particles as small as 3.5 nm, below the predicted thermodynamic stability limit for γ-Al2O3.

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Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al₂O₃ Nanocrystals

Abstract

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Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al2O3 Nanocrystals

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Bibliographical note

Keywords

MRSEC Support

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University of Minnesota Materials Research Science and Engineering Center (DMR-2011401)

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Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al₂O₃ Nanocrystals