Single Crystalline MgTiO3 Flake Production via Single-Step Calcination

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Solution Overview

Problem

Current methods for producing titanate flakes, such as those described in Japanese Unexamined Patent Application Publications, require multiple high-temperature heating steps, resulting in high energy costs, longer production times, and complications, while producing polycrystalline flakes with lower refractive indices compared to single crystalline materials.

Innovation Solution

A method involving the mixing of a phosphorus compound with a titanium compound and a magnesium compound to form a MgTiO3 precursor, followed by a single calcination step at temperatures between 800°C to 1400°C in an oxygen-containing atmosphere, effectively producing single crystalline MgTiO3 flakes with high refractive index and luster suitable for pigment applications.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If multiple high-temperature heating steps are used to produce titanate flakes, then the crystallization and phase formation are improved, but the energy consumption and production time increase significantly

Engineering Contradiction:
Improvecrystallization qualityVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The patent combines multiple separate heating steps (calcination and crystallization) into a single heating step that achieves both objectives simultaneously. The mixed oxide precursor is heated once to form the desired titanate phase with proper crystallization, eliminating the need for sequential high-temperature treatments and thereby reducing energy consumption while maintaining product quality

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent modifies the chemical composition parameters by introducing a mixed oxide precursor containing specific ratios of metal oxides (such as TiO2, Al2O3, SiO2, and other optional oxides). This compositional adjustment allows the material to achieve proper crystallization and phase formation at lower temperatures or in a single heating step, thus reducing energy requirements while maintaining manufacturing precision

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If multiple high-temperature heating steps are used to produce titanate flakes, then the phase formation is improved, but the production time increases

Engineering Contradiction:
Improvephase formationVSAvoidproduction time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent merges the calcination step and crystallization step into a single integrated heating process. The mixed oxide precursor undergoes both phase formation and crystallization development in one continuous heating operation, significantly reducing the total production time compared to traditional methods that require separate sequential steps

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent performs preliminary preparation by creating a mixed oxide precursor with controlled composition and particle characteristics before the final heating step. This pre-positioning of the correct chemical framework and physical structure enables the material to undergo rapid and efficient phase formation during the single heating step, reducing overall production time while ensuring proper phase development

Inventive Principle:
Principle #10Preliminary action

3Ease of manufacture

If polycrystalline structure is used in titanate flakes, then the production process is simpler, but the refractive index is lower

Engineering Contradiction:
Improveproduction process simplicityVSAvoidrefractive index
Core Design Contradiction:
Ease of manufactureVSIllumination intensity

Solution Approach 1:

The patent changes the chemical composition parameters of the precursor material by using a specifically formulated mixed oxide system. This compositional modification enables the formation of single crystalline structures with higher refractive indices while maintaining production process simplicity, as the controlled chemistry guides the crystallization toward the desired high-performance phase

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a composite oxide system in the precursor stage, combining TiO2 with Al2O3, SiO2, and other metal oxides in controlled proportions. This composite approach allows the formation of single crystalline titanate phases with enhanced optical properties (higher refractive index) while keeping the manufacturing process relatively simple through a single heating step

Inventive Principle:
Principle #40Composite materials

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 reduces energy costs and production efforts, enabling the production of high-quality single crystalline MgTiO3 flakes with high refractive index and luster, suitable for use as highly reflective pigments or interference pigments, while minimizing twin crystals and coagulations, and allowing for diameter control.

Implementation Method 1

mixing at least a titanium compound, a magnesium compound and a phosphorous compound whereby a MgTiO3 precursor is formed

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

calcining the obtained precursor at a temperature in the range from 800°C to 1400°C as a single calcination step

Methodology Applied
Scientific EffectCalcination: Heating

Implementation Method 3

producing single crystalline MgTiO3 flakes

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentEP3084050B1Method for the production of single crystalline mgtio3 flakes
Publication Date: 2020.01.08 MERCK PATENT GMBH
  • EP3084050B1 patent drawingFigure 1~2

AI summary

The present invention is related to a method for the production of single crystalline MgTiO3 flakes, in particular in the geikielite crystal structure, to single crystalline MgTiO3 flakes obtained by this method as well as to the use thereof, in particular as pigments in several application media.