Titanium Oxide Nanomaterial Synthesis via Aqueous Hydrothermal Process

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Solution Overview

Problem

Current methods for synthesizing nanocrystalline titanium oxides with high photocatalytic activity under visible light are limited by the need for organic solvents and high-energy calcination processes, which are environmentally and energetically costly, and often result in unstable anatase structures with lower performance compared to rutile.

Innovation Solution

A method for preparing titanium oxide nanomaterials with a high specific surface area and increased hydroxyl groups using an aqueous medium with non-ionic surfactants like alkenyl ethers of polyoxyethylene glycol and poloxamers, eliminating the need for organic solvents and achieving a rutile nanocrystalline structure without calcination, by synthesizing TiO2 with 80-100 mole % TiO2 and 0-20 mole % of another metal or semi-metal oxide, such as SiO2, ZrO2, at controlled temperatures and pH levels.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If organic solvents and high-temperature calcination are used to synthesize nanocrystalline titanium oxides, then photocatalytic activity can be improved, but environmental cost and energy consumption increase significantly

Engineering Contradiction:
Improvephotocatalytic activityVSAvoidenergy consumption
Core Design Contradiction:
ReliabilityVSLoss of energy

Solution Approach 1:

The invention changes the synthesis parameters by using aqueous medium instead of organic solvents and performing low-temperature hydrothermal treatment (100-200°C) instead of high-temperature calcination (>700°C). This parameter change maintains photocatalytic activity while dramatically reducing energy consumption and environmental impact

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention replaces the thermal-mechanical calcination process with a chemical-hydrothermal process. Instead of using high-temperature thermal treatment to form nanocrystals, the invention uses controlled hydrothermal synthesis in aqueous medium with surfactants, substituting a high-energy mechanical/thermal system with a lower-energy chemical process

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

2Area of stationary object

If organic solvents are used in the synthesis process, then nanomaterials with high specific surface area can be obtained, but ecological disadvantages arise

Engineering Contradiction:
Improvespecific surface areaVSAvoidecological impact
Core Design Contradiction:
Area of stationary objectVSObject-affected harmful factors

Solution Approach 1:

The invention changes the solvent parameter from organic to aqueous medium, eliminating ecological harm while maintaining the ability to produce high specific surface area nanomaterials through controlled hydrothermal synthesis and surfactant use

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces non-ionic surfactants as intermediaries in the aqueous medium to enable effective synthesis. These surfactants act as mediators that facilitate nanomaterial formation and surface area development in water-based systems, replacing the role previously filled by organic solvents

Inventive Principle:
Principle #24Intermediary (Mediator)

3Stability of the object's composition

If anatase structure is obtained through high-temperature calcination, then photocatalytic stability is improved, but synthesis complexity and energy requirements increase

Engineering Contradiction:
Improvestructural stabilityVSAvoidsynthesis process complexity
Core Design Contradiction:
Stability of the object's compositionVSDevice complexity

Solution Approach 1:

The invention changes the temperature and chemical environment parameters to achieve stable nanocrystalline structures at low temperatures. By using hydrothermal conditions with controlled pH and surfactants, the invention obtains structurally stable titanium oxide nanomaterials without requiring high-temperature calcination processes

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary crystal structure formation during the hydrothermal synthesis step itself, rather than requiring a separate subsequent calcination step. The nanocrystalline structure is formed in advance during the low-temperature aqueous synthesis, eliminating the need for high-temperature treatment

Inventive Principle:
Principle #10Preliminary action

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method produces nanomaterials with enhanced photocatalytic performance under both UV and visible light, achieving higher specific surface areas and hydroxyl group densities, leading to improved photocatalytic activity and stability, surpassing commercial titanium dioxides in adsorption and degradation capacities.

Implementation Method 1

the synthesis being made in an aqueous medium with a pH between 0 and 1 and at a temperature varying from 40 to 95° C. in the presence of a non-ionic surfactant chosen from among ankenyl ethers of polyoxyethylene glycol and poloxamers

Methodology Applied
Scientific EffectSurfactant: Surfactant

Implementation Method 2

The addition of ethanol slows the reactivity of the titanium oxide precursor that is hydrolysed immediately

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Data Source

PatentUS10960385B2Method for the production of new nanomaterials
Publication Date: 2021.03.30 COMMISSARIAT A LENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES
  • US10960385B2 patent drawing
  • US10960385B2 patent drawing
  • US10960385B2 patent drawing

AI summary

A method for producing new nanomaterials, 80 to 100 mol % of which are composed of TiO2 and 0 to 20 mol % are composed of another metal or semi-metal oxide that has a specific surface of 100 to 300 m2·g−1 and 1 to 3 hydroxyl groups per nm2.