Process for Synthesis of Well-ordered Mesoporous Titania having Monoclinic and Anatase Phases

Technology: Synthesis Of Well-ordered Mesoporous Titania; Industry: Semiconductor, Catalyst/Photocatalyst, Chemical Engineering;

Applications: Catalyst, Porous Materials, etc.

Market: The Global Titanium Market is projected to $33.5B by 2026, at a CAGR of 6.3% during 2022-2026.

In the present era, semiconductor-based photo-catalysts are being explored worldwide for many purposes and the photocatalytic activity of such materials depends on many properties, viz., surface area, recombination rate of excitons, crystal phase, crystallite size, morphology, etc.
One of the major challenges lies in the synthesis of high-quality mesoporous materials like titania precursor during hydrolysis leading to uncontrolled phase separation, which normally results in disordered phases.
Hence, there is a need to mitigate these issues.

The Present Patent discloses a process for the synthesis of well-ordered mesoporous titania having monoclinic and anatase phases under optimal conditions.

The claimed process further explains that the solvent is allowed to evaporate in the oven at 40⁰C for at least 7 days during which inorganic precursors get hydrolyzed & and polymerized into a metal oxide framework.
The as-synthesized sample obtained can be finally calcined at 350°C for 4h in the air at 0.5°C/min to remove the surfactant and obtain well-ordered highly ordered 2D hexagonal mesoporous titania. i.e., mesoporous TiO2 (TMF-127).
The Rietveld refined XRD pattern clearly depicts the phase composition ratio in which monoclinic (59 wt.%) and anatase (41 wt.%) phases. (Refer Fig.1)

Technical Perspective

The obtained mesoporous titania (TMF-127) confirmed the long-range ordered channels as well as the hexagonal pore system, and the inset selected area electron diffraction (SAED) confirms structure is well crystallized.
The use of a non-aqueous medium (ethanol) and block copolymer surfactant F127, the rate of hydrolysis, condensation, phase transformation, and phase separation between surfactant and titania precursor is minimized.
A controlled aging process leads to the form of a well-ordered mesoporous matrix with monoclinic, TiO2(B), and anatase, TiO2 phases.

Industrial Perspective:

Provides a cost-effective improved process for the synthesis of well-ordered mesoporous titania having monoclinic (bronze) and tetragonal (anatase) phases.

Prof. P. Selvam

NCCR & Department of Chemistry

TRL- 3/4

Technology validated in Lab

Technology Transfer