Monoclinic TiO2(B) Preparation with Lower-Temperature Sintering

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Solution Overview

Problem

The preparation of monoclinic titanium dioxide (TiO2(B)) is challenging due to its metastable crystal phase, and existing methods require high sintering temperatures and excess potassium carbonate, making the manufacturing process difficult to scale up and costly.

Innovation Solution

A method involving the use of a specific potassium to titanium molar ratio (2.0/4.0 < K/Ti < 2.0/2.4) and sintering temperatures between 750°C to 900°C, followed by ion-exchange and thermal treatment, to produce TiO2(B) with a predominantly monoclinic crystal structure.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If high sintering temperature (≥950°C) and excess K2CO3 are used, then pure phase TiO2(B) can be obtained, but the manufacturing process becomes difficult to scale up and energy consumption increases

Engineering Contradiction:
Improvepurity of TiO2(B) phaseVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The patent changes the sintering temperature parameter from conventional high temperature (≥950°C) to a lower range (700-900°C), and adjusts the K/Ti molar ratio parameter to optimize the reaction. This parameter optimization allows obtaining pure TiO2(B) phase while reducing energy consumption and avoiding the need for excess K2CO3, thus resolving the contradiction between purity and energy consumption

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If high sintering temperature (≥950°C) is used, then pure phase TiO2(B) can be obtained, but the manufacturing process becomes difficult to scale up

Engineering Contradiction:
Improvepurity of TiO2(B) phaseVSAvoidscalability of manufacturing process
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent optimizes the sintering temperature parameter to a lower range (700-900°C) and adjusts the K/Ti molar ratio to achieve pure TiO2(B) phase formation under milder conditions. This makes the manufacturing process more scalable and easier to implement in industrial settings while maintaining high product purity

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If excess K2CO3 is used to compensate for high evaporation rate, then pure phase TiO2(B) can be obtained, but the process conditions become complex and scale-up becomes challenging

Engineering Contradiction:
Improvepurity of TiO2(B) phaseVSAvoidcomplexity of process conditions
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent changes the K/Ti molar ratio parameter to an optimized range (2.0/4.0 to 2.0/2.4) and reduces the sintering temperature, which together eliminate the need for using excess K2CO3. This simplifies the process conditions and removes the complexity associated with compensating for K2CO3 evaporation, while still achieving pure TiO2(B) phase

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

This method allows for the production of high-purity TiO2(B) with improved electrochemical performance, reducing energy consumption and manufacturing costs while maintaining competitive capacity with existing anode active materials.

Implementation Method 1

ion-exchange to replace the alkaline metal ion with a proton ion, thereby, forming a hydrogen titanate

Methodology Applied
Scientific EffectIon-exchange: Ion Exchange

Implementation Method 2

dehydration of the hydrogen titanates at moderate temperature leads to the formation of TiO2(B)

Methodology Applied
Scientific EffectDehydration:

Implementation Method 3

mixing the at least one titanium precursor with the one or more potassium precursors to form a mixture

Methodology Applied
Scientific EffectMixing:

Implementation Method 4

sintering temperatures between 750°C to 900°C

Methodology Applied
Scientific EffectSintering: Sintering

Implementation Method 5

production of high-purity TiO2(B) with improved electrochemical performance

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS20250313489A1A preparation process for monoclinic titanium dioxide
Publication Date: 2025.10.09 PACIFIC IND DEVELOPMENT CORP
  • US20250313489A1 patent drawing
  • US20250313489A1 patent drawing
  • US20250313489A1 patent drawing

AI summary

A method for preparing titanium dioxide that includes the steps of providing at least one titanium precursor: providing one or more potassium precursors: mixing the at least one titanium precursor with the one or more potassium precursors to form a mixture: wherein the mixture has a potassium to titanium (K/Ti) molar ratio of 2.0/4.0&lt;K/Ti&lt;2.0/2.4; sintering the mixture at a temperature in the range of 750° C. to 900° C. for a predetermined time to form a powder: soaking the heated powder in an acidic solution: collecting and drying the acid-soaked powder: and treating the collected powder thermally at a temperature in the range of 300° C. to 500° C. for a predetermined time to form the TiO2. The titanium oxide formed has a monoclinic crystal structure. TiO2(B), as its major crystal phase with a mass percentage that is &gt;50% of the overall mas of the TiO2.