Macroporous Titanium Monolith with Controlled Pores and Conductivity

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Solution Overview

Problem

Current methods for producing porous monoliths, particularly those composed of titanium compounds other than titanium dioxide, face challenges in achieving controlled macropores and single-phase oxygen-deficient structures with electron conductivity.

Innovation Solution

A method involving a sol-gel reaction with phase separation controllers, chelating agents, and strong acid salts, followed by gas-phase reduction using metals with titanium-reducing abilities, to form macroporous titanium compound monoliths with co-continuous structures of oxygen-deficient titanium oxide, titanium oxynitride, or titanium nitride, ensuring controlled macropores and electron conductivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If a porous monolith is produced by conventional sol-gel methods using titanium compounds other than titanium dioxide, then the monolith can be formed, but the pores cannot be controlled and the structure becomes a powder aggregate rather than a controlled macroporous structure

Engineering Contradiction:
Improvepore controlVSAvoidproduction difficulty
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent uses an intermediary substance (polymer or surfactant) as a template to control macropore formation. This intermediary acts as a mediator between the sol-gel reaction and the desired porous structure, allowing precise control of macropore size and distribution while maintaining ease of manufacture through standard sol-gel procedures.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent controls macropore characteristics by changing parameters such as polymer concentration, surfactant type, and sol-gel reaction conditions. By systematically adjusting these parameters, the method achieves precise pore control while maintaining manufacturability through optimized but not overly complex processing.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If a porous monolith is produced by mixing titanium dioxide powder with organic solvent containing polymer material and sintering, then macropores are formed by burning off the polymer, but the resulting structure is a powder aggregate without controlled macropores and does not achieve single crystalline phase

Engineering Contradiction:
Improvestructural uniformityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent performs preliminary action by forming the macroporous structure through sol-gel reaction before sintering, rather than creating pores after sintering as in conventional methods. The polymer template is incorporated during gel formation, ensuring uniform macropore distribution is established before the sintering process, thereby achieving structural uniformity without excessive complexity.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent creates a composite structure during sol-gel processing where the inorganic matrix and organic template coexist, allowing the macroporous structure to be built into the material framework itself. This composite approach during formation ensures both structural uniformity and controlled porosity, avoiding the powder aggregate problem of conventional methods.

Inventive Principle:
Principle #40Composite materials

3Reliability

If titanium dioxide is used as the starting material, then a stable oxide framework is formed, but oxygen-deficient structures with electron conductivity cannot be achieved without additional reducing treatment

Engineering Contradiction:
Improveframework stabilityVSAvoidelectron conductivity
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The patent changes the chemical composition parameter by using titanium compounds other than titanium dioxide (such as titanium alkoxides or titanium salts) as starting materials. This parameter change allows the formation of oxygen-deficient titanium oxide structures directly during the sol-gel process, achieving both framework stability and electron conductivity without requiring additional reducing treatments, thereby improving productivity.

Inventive Principle:
Principle #35Parameter changes

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 successfully produces macroporous titanium compound monoliths with uniform macropores and single-phase frameworks, achieving high electron conductivity and versatility in applications such as electrodes and photocatalysts.

Implementation Method 1

an aggregate or a polymer of an oxide is obtained by a sol-gel reaction, that is, by hydrolysis of the compound followed by polycondensation

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

an aggregate or a polymer of an oxide is obtained by a sol-gel reaction, that is, by hydrolysis of the compound followed by polycondensation

Methodology Applied
Scientific EffectPolycondensation: Chemical Bonding

Implementation Method 3

heating the monolith and the metal to cause gas-phase reduction that removes oxygen atom from the titanium dioxide composing the monolith by the metal acting as an oxygen getter

Methodology Applied
Scientific EffectReduction: Reduction

Implementation Method 4

heating the monolith and the metal to cause gas-phase reduction that removes oxygen atom from the titanium dioxide composing the monolith by the metal acting as an oxygen getter

Methodology Applied
Scientific EffectGettering: Gettering

Data Source

PatentEP2816012B1Macroporous titanium compound monolith and method for manufacturing same
Publication Date: 2021.12.15 THE JAPAN SCI & TECH AGENCY
  • EP2816012B1 patent drawingFigure 1~2
  • EP2816012B1 patent drawingFigure 3
  • EP2816012B1 patent drawingFigure 4

AI summary

Provided are a macroporous titanium compound monolith and a production method thereof, the macroporous titanium compound monolith having a framework that is composed of a titanium compound other than titanium dioxide, having controlled macropores, and having electron conductivity, the titanium compound being oxygen-deficient titanium oxide, titanium oxynitride, or titanium nitride. Provided is a method including: placing a macroporous titanium dioxide monolith and a metal having titanium-reducing ability in a container, the macroporous titanium dioxide monolith having a co-continuous structure of a macropore and a framework that is composed of titanium dioxide; creating a vacuum atmosphere or an inert gas atmosphere within the container; and heating the monolith and the metal to cause gas-phase reduction that removes oxygen atom from the titanium dioxide composing the monolith by the metal acting as an oxygen getter, thereby obtaining a macroporous oxygen-deficient titanium oxide monolith having a co-continuous structure of the macropore and a framework that is composed of oxygen-deficient titanium oxide, the macroporous oxygen-deficient titanium oxide monolith having electron conductivity derived from the oxygen-deficient titanium oxide.