Doped Bismuth Silicate Crystals via Controlled Devitrification

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Solution Overview

Problem

Current methods for producing bismuth-silicate crystals are energy-intensive and result in significant by-products, with high operating temperatures and long processing times, limiting their scalability and efficiency for applications in automotive enamels and optical materials.

Innovation Solution

A method involving the controlled crystallization of bismuth-silicate glass compositions using specific dopants like lanthanum, neodymium, and samarium oxides, with a glass melting process followed by heat treatment, to produce high-purity doped-bismuth-silicate crystals with controlled dimensionality and nucleation, reducing energy consumption and by-product formation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If solid state reaction is used to make anti-stick seed crystals, then crystal formation is achieved, but energy consumption increases and processing time exceeds 48 hours

Engineering Contradiction:
Improvecrystal formationVSAvoidenergy consumption
Core Design Contradiction:
Ease of manufactureVSUse of energy by moving object

Solution Approach 1:

The patent changes the temperature parameter from above 1000°C to a controlled range of 900-1100°C, and reduces processing time from >48 hours to 12-24 hours while maintaining crystal formation effectiveness

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces specific nucleating agents (CaO, MgO, Al2O3, TiO2, ZrO2) as intermediaries that facilitate crystal formation at lower temperatures and shorter times, acting as catalysts for the phase transition

Inventive Principle:
Principle #24Intermediary (Mediator)

2Ease of manufacture

If solid state reaction is used to make anti-stick seed crystals, then crystal formation is achieved, but processing time exceeds 48 hours

Engineering Contradiction:
Improvecrystal formationVSAvoidprocessing time
Core Design Contradiction:
Ease of manufactureVSLoss of time

Solution Approach 1:

The patent optimizes the temperature-time parameters by conducting the reaction at 900-1100°C for 12-24 hours, which significantly accelerates the reaction kinetics compared to conventional methods while maintaining crystal quality

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent performs preliminary mixing of reagents in specific ratios and pre-heating treatments before the main crystallization process, which prepares the material system for faster and more efficient crystal formation

Inventive Principle:
Principle #10Preliminary action

3Ease of manufacture

If high temperature processing is used, then crystal formation is achieved, but by-product formation increases

Engineering Contradiction:
Improvecrystal formationVSAvoidby-product formation
Core Design Contradiction:
Ease of manufactureVSObject-generated harmful factors

Solution Approach 1:

The patent restricts the temperature range to 900-1100°C, which is lower than conventional >1000°C processing, thereby suppressing the formation of unwanted by-products while still achieving complete crystal formation

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses specific nucleating agents as intermediaries that promote direct formation of desired crystals at lower temperatures, preventing the formation of intermediate by-products that would form at higher temperatures

Inventive Principle:
Principle #24Intermediary (Mediator)

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 approach significantly reduces energy consumption and processing time, achieving higher crystal conversion rates and solubility of dopants, while minimizing impurities and waste, making the production more cost-effective and efficient.

Implementation Method 1

This work is representative of devitrification (or controlled crystallization) of a glass forming liquid, in this case a bismuth-silicate melt. The temperature profile for controlled crystallization includes at least two steps: nucleation at temperatures slightly above the annealing temperature, and then crystallization at higher temperatures.

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 2

The nucleating agents can affect the crystallization by acting either as seeds, catalysts of phase separation, or reducing the interfacial tension between solid and liquid phases.

Methodology Applied
Scientific EffectNucleation: Nucleation

Implementation Method 3

This work is representative of devitrification (or controlled crystallization) of a glass forming liquid, in this case a bismuth-silicate melt.

Methodology Applied
Scientific EffectDevitrification: Crystallisation

Implementation Method 4

A method involving the controlled crystallization of bismuth-silicate glass compositions using specific dopants like lanthanum, neodymium, and samarium oxides

Methodology Applied
Scientific EffectDoping: Dopants

Implementation Method 5

with a glass melting process followed by heat treatment, to produce high-purity doped-bismuth-silicate crystals

Methodology Applied
Scientific EffectHeat treatment: Heat Treatment

Data Source

PatentEP3765423B1Doped bismuth silicate crystals via devitrification of glass forming liquids
Publication Date: 2023.11.15 GLASS COATINGS & CONCEPTS LLC
  • EP3765423B1 patent drawingFigure 1
  • EP3765423B1 patent drawingFigure 2
  • EP3765423B1 patent drawingFigure 3

AI summary

This technology is directed to the preparation of doped-bismuth-silicate seed crystals through controlled crystallization (e.g. dimensionality of growth and nucleation mechanism) and the method of forming high purity single seed (particle size ranges from micrometers to millimeters) for various uses. These seed crystals have a nominal stoichiometry of Bi2-xAxSi05, Bi2-xAxSi309, Bi4-xAxSi309, and Bi12-xAxSi020, where A is a rare earth dopant selected from La, Ce, Nd, Pr, and/or Sm.