Self-Assembled Colloidal Crystals from ZrO2 Nanoparticles

Ordered three-dimensional (3-D) assemblies of nanocrystalline zirconia were synthesized from aqueous suspensions of ZrO2 nanoparticles without the need for hydrocarbon surfactants or solvents to control colloidal crystal growth. Nanoparticles were suspended in mild acid and subsequently titrated fro...

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Bibliographic Details
Published in:The journal of physical chemistry. B 2006-10, Vol.110 (39), p.19456-19460
Main Authors: Woodward, Jonathan D, Pickel, Joseph M, Anovitz, Lawrence M, Heller, William T, Rondinone, Adam J
Format: Article
Language:English
Subjects:
CRYSTAL GROWTH
HEAT TREATMENTS
HYDROCARBONS
INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY
INTERSTITIALS
SCATTERING
SOLUBILITY
SOLVENTS
STABILITY
SURFACE AREA
SURFACTANTS
WATER
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Summary:Ordered three-dimensional (3-D) assemblies of nanocrystalline zirconia were synthesized from aqueous suspensions of ZrO2 nanoparticles without the need for hydrocarbon surfactants or solvents to control colloidal crystal growth. Nanoparticles were suspended in mild acid and subsequently titrated from low to neutral pH. The solubility was reduced as the surfaces were neutralized, promoting assembly of the nanoparticles into ordered monoliths. TEM measurements indicated the formation of three-dimensional, hexagonal faceted, micrometer-sized colloidal crystals composed of 4 nm diameter ZrO2 nanoparticles. Lacking organic surfactants, the colloidal crystals were exceptionally robust and were sintered at high temperatures (300−500 °C) for further stability. Small-angle X-ray scattering (SAXS) measurements demonstrate that the samples become progressively more amorphous above 350 °C, although some ordered domains of nanoparticles persist. Additionally, the heat treatment dramatically increases the surface area of the colloidal crystals as water and residual organics are desorbed, revealing highly controlled interstitial spaces and pores.
ISSN:1520-6106
1520-5207
DOI:10.1021/jp062471z