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Size tunable synthesis and surface chemistry of metastable TiO2-bronze nanocrystals

(2018) CHEMISTRY OF MATERIALS. 30(13). p.4298-4306
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Abstract
The metastable titania phase, bronze, has great potential as photocatalyst or as anode material in Li-ion batteries. Here, we report the first synthesis of colloidally stable, size-tunable TiO2-bronze (TiO2-B) nanocrystals, via a hydrothermal process. By employing definitive screening design, the experimental parameters affecting the size and agglomeration of the nanocrystals are identified. The size is mostly determined by the reaction temperature, resulting in 3-8 nm NCs in the range of 130-180 degrees C. To avoid irreversible aggregation, short reaction times are desired, and in this respect, microwave heating proved essential due to its fast heating and cooling rates. The resulting nanocrystals are deaggregated and stabilized in polar solvents using either positive or negative surface charges. In nonpolar solvents, steric stabilization is provided by long chain amines and carboxylic acids. Furthermore, we study this peculiar postsynthetic surface modification through solution H-1 NMR and elemental analysis. Surprisingly, we find ion-pairs of alkylammonium carboxylates bound to the surface, contrasting with earlier reports on carboxylic acid stabilized metal oxide nanocrystals. To rationalize this, a general framework of acid/base chemistry with metal oxide nanocrystals is constructed and discussed.
Keywords
SOLUBLE TITANIUM COMPLEX, METAL-OXIDE NANOCRYSTALS, LITHIUM-ION BATTERIES, LIGAND-EXCHANGE, NANOSTRUCTURED TIO2(B), BINDING, NANOWIRES, STABILIZATION, NANOMATERIALS, DISPLACEMENT

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Citation

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Chicago
Billet, Jonas, Wouter Dujardin, Katrien De Keukeleere, Klaartje De Buysser, Jonathan De Roo, and Isabel Van Driessche. 2018. “Size Tunable Synthesis and Surface Chemistry of Metastable TiO2-bronze Nanocrystals.” Chemistry of Materials 30 (13): 4298–4306.
APA
Billet, J., Dujardin, W., De Keukeleere, K., De Buysser, K., De Roo, J., & Van Driessche, I. (2018). Size tunable synthesis and surface chemistry of metastable TiO2-bronze nanocrystals. CHEMISTRY OF MATERIALS, 30(13), 4298–4306.
Vancouver
1.
Billet J, Dujardin W, De Keukeleere K, De Buysser K, De Roo J, Van Driessche I. Size tunable synthesis and surface chemistry of metastable TiO2-bronze nanocrystals. CHEMISTRY OF MATERIALS. 2018;30(13):4298–306.
MLA
Billet, Jonas, Wouter Dujardin, Katrien De Keukeleere, et al. “Size Tunable Synthesis and Surface Chemistry of Metastable TiO2-bronze Nanocrystals.” CHEMISTRY OF MATERIALS 30.13 (2018): 4298–4306. Print.
@article{8566854,
  abstract     = {The metastable titania phase, bronze, has great potential as photocatalyst or as anode material in Li-ion batteries. Here, we report the first synthesis of colloidally stable, size-tunable TiO2-bronze (TiO2-B) nanocrystals, via a hydrothermal process. By employing definitive screening design, the experimental parameters affecting the size and agglomeration of the nanocrystals are identified. The size is mostly determined by the reaction temperature, resulting in 3-8 nm NCs in the range of 130-180 degrees C. To avoid irreversible aggregation, short reaction times are desired, and in this respect, microwave heating proved essential due to its fast heating and cooling rates. The resulting nanocrystals are deaggregated and stabilized in polar solvents using either positive or negative surface charges. In nonpolar solvents, steric stabilization is provided by long chain amines and carboxylic acids. Furthermore, we study this peculiar postsynthetic surface modification through solution H-1 NMR and elemental analysis. Surprisingly, we find ion-pairs of alkylammonium carboxylates bound to the surface, contrasting with earlier reports on carboxylic acid stabilized metal oxide nanocrystals. To rationalize this, a general framework of acid/base chemistry with metal oxide nanocrystals is constructed and discussed.},
  author       = {Billet, Jonas and Dujardin, Wouter and De Keukeleere, Katrien and De Buysser, Klaartje and De Roo, Jonathan and Van Driessche, Isabel},
  issn         = {0897-4756},
  journal      = {CHEMISTRY OF MATERIALS},
  language     = {eng},
  number       = {13},
  pages        = {4298--4306},
  title        = {Size tunable synthesis and surface chemistry of metastable TiO2-bronze nanocrystals},
  url          = {http://dx.doi.org/10.1021/acs.chemmater.8b01296},
  volume       = {30},
  year         = {2018},
}

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