Solid-Solution Nanoparticles: Use of a Nonhydrolytic Sol−Gel Synthesis To Prepare HfO2 and HfxZr1-xO2 Nanocrystals

Tang, Jing; Fabbri, Jason; Robinson, Richard D.; Zhu, Yimei; Herman, Irving P.; Steigerwald, Michael L.; Brus, Louis E.

doi:10.1021/cm049945w

Cited by 154Chemical and Physical Properties of MaterialsSemiconductor materials and devicesQuantum Dots Synthesis And Properties

Solid-Solution Nanoparticles: Use of a Nonhydrolytic Sol−Gel Synthesis To Prepare HfO2 and HfxZr1-xO2 Nanocrystals

Tang, Jing, Fabbri, Jason, Robinson, Richard D., Zhu, Yimei, Herman, Irving P., Steigerwald, Michael L., Brus, Louis E.·2004·Chemistry of Materials

DOI 10.1021/cm049945w

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Abstract

A nonhydrolytic sol−gel process closely following that of Hyeon et al. for the synthesis of ZrO 2 nanocrystals ( J. Am. Chem. Soc. 2003, 125, 6553−6557) was used to synthesize highly crystalline and monodisperse HfO 2 nanoparticles. Reactions of hafnium isopropoxide with hafnium halides at high temperature in a strongly coordinating solvent yield nanometer-sized particles of HfO 2 . The size, shape, and crystalline phase of the hafnia particles depend on both the reaction temperature and the halide. The nonhydrolytic cross-condensation method was also extended to the binary metal oxides nanocrystals, i.e., HfO 2 −ZrO 2, ZrO 2 −TiO 2, and HfO 2 −TiO 2 . Efforts to prepare nanocrystals of Hf x Zr 1 - x O 2 over a wide range of x were successful; however, this method could not be used to prepare either Zr x Ti 1 - x O 2 or Hf x Ti 1 - x O 2 . In conjunction with X-ray powder diffraction and high-resolution transmission electron microscopy, Raman spectroscopy identifies the structural phase of the nanocrystals and also proves the formation of the Hf−Zr solid solution nanoparticles via the cross-condensation method. In the case of Hf x Zr 1 - x O 2, for x < 0.5, highly monodisperse, roughly spherical particles of tetragonal Hf x Zr 1 - x O 2 were formed, while for x > 0.5, small nanorods of the monoclinic phase of the binary oxide were obtained.

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TiO2, ZrO2, and HfO2 can create diverse nanostructures with controlled dimensions and distinctive morphologies using surfactant-mediated synthesis.
“TiO2, ZrO2, and HfO2 exhibits the ability to create diverse nanostructures with controlled dimensions and distinctive morphologies using surfactant-mediated synthesis [46,54,55].”
From Recent Advances in Metal-Oxide-Based Photoresists for EUV Lithography (2024) · cites this paper as [55]

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“TiO 2 , ZrO 2 , and HfO 2 exhibits the ability to create diverse nanostructures with controlled dimensions and distinctive morphologies using surfactant-mediated synthesis [46,54,55].”
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Authors: Tang, J., Fabbri, J., Robinson, R. D., Zhu, Y., Herman, I. P., Steigerwald, M. L., & Brus, L. E.
Affiliations: Brookhaven National Laboratory (US)
Corresponding author: Steigerwald, Michael L.
ORCID: Fabbri, Jason
Zhu, Yimei
Herman, Irving P.
Steigerwald, Michael L.
Brus, Louis E.
Venue: Chemistry of Materials
Publisher: American Chemical Society (ACS)
Published: 2004-03-11
Volume: 16
Issue: 7
Pages: 1336-1342
ISSN: 0897-4756 (ISSN-L)
1520-5002
DOI: 10.1021/cm049945w
OpenAlex: W1965145270
Cited by: 154
References: 16
Citations by year: 2026: 2 · 2025: 4 · 2024: 12 · 2023: 5 · 2022: 3 · 2021: 7 · 2020: 5 · 2019: 9 · 2018: 7 · 2017: 5 · 2016: 10 · 2015: 6 · 2014: 5 · 2013: 6 · 2012: 6
FWCI: 7.28
Type: journal article
Language: en
Open access: closed
Locations: Chemistry of Materials (publishedVersion)
Funders: Division of Materials Research
Topics: Physical Sciences › Materials Science › Materials Chemistry › Chemical and Physical Properties of Materials
Physical Sciences › Engineering › Electrical and Electronic Engineering › Semiconductor materials and devices
Physical Sciences › Materials Science › Materials Chemistry › Quantum Dots Synthesis And Properties
Keywords: hafnium oxide nanoparticles, cross-condensation, ZrO2 nanocrystals, nanocrystalline TiO2, monoclinic and tetragonal phases, nanorods, monodisperse particles, crystalline phase

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Solid-Solution Nanoparticles: Use of a Nonhydrolytic Sol−Gel Synthesis To Prepare HfO2 and HfxZr1-xO2 Nanocrystals

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