Abstract When a few drops of acid (hydrochloric, acrylic, propionic, acetic, or formic) are added to a colloid comprised of 1D lepidocrocite titanate nanofilaments (1DLs)–2 × 2 TiO6octahedra in cross‐section–a hydrogel forms, in many cases, within seconds. The 1DL synthesis process requires the reaction between titanium diboride with tetramethylammonium (TMA+), hydroxide. Using quantitative nuclear magnetic resonance (qNMR), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC), the mass percent of TMA+after synthesis is determined to be ≈ 13.1 ± 0.1%. The TMA+is completely removed from the gels after 2 water soak cycles, resulting in the first completely inorganic, TiO2‐based hydrogels. Ion exchanging the TMA+with hydronium results in gels with relatively strong hydrogen bonds. The hydrogels' compression strengths increased linearly with 1DL colloid concentration. At a 1DL concentration of 45 g L−1, the compressive strength, at 80% deformation when acrylic acid is used, is ≈325 kPa. The strengths are ≈ 50% greater after the TMA+is removed. The removal of all residual organic components in the hydrogels, including TMA+, is confirmed by qNMR, Fourier‐transformed infrared spectroscopy (FTIR), and TGA/DSC. The 1DL phase is retained after gelation, TMA+removal, and 80% compression.
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This content will become publicly available on November 20, 2025
Titanium Oxysulfate‐Derived 1D Lepidocrocite Titanate Nanostructures
Abstract Nanostructured titania, TiO2, holds significant importance in various scientific fields and technologies for their distinctive properties and multipurpose characteristics. In this article, the facile, economical, and scalable synthesis of 1D lepidocrocite, 1DL, titania nanostructures derived from a water‐soluble Ti precursor, titanium oxysulfate (with oxidation of Ti+4) at temperature <100 °C under atmospheric pressure is discussed. Titanium oxysulfate with tetramethyl ammonium hydroxide, TMAH, is simply reacted to yield individual lepidocrocite titania‐based chain‐forming nanofilaments, NFs, 6 × 6 Å2in minimal cross‐section and aspect ratios of ≈20 1DLs. If only ethanol is used for washing, the 1DL self‐assemble into ≈10 µm, porous mesostructured particles, PMPs. If water is used, quasi‐2D sheets form instead. Characterization of the resulting powders showed them to be quite similar to those derived from TiB2, and other water‐insoluble Ti precursors. The 1DL bandgap energies are ≈4 eV, due to quantum confinement. They adsorbed rhodamine 6G. The latter also sensitized the 1DLs and allowed for dye degradation using only visible light. Used as electrodes in supercapacitors, the 1DLs can be cycled over 1.6 V and result in high power densities (300 W kg−1). Stronger birefringence started to appear in samples with concentrations >15 gL−1indicating the formation of a liquid crystal phase. This new synthesis protocol enables the cheaper scalable production of 1DLs with significant implications across various fields.
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- Award ID(s):
- 2211319
- PAR ID:
- 10585796
- Publisher / Repository:
- Wiley
- Date Published:
- Journal Name:
- Advanced Materials Interfaces
- ISSN:
- 2196-7350
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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