Cubic Sesquioxide Single-Crystal Growth via Flux Method

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Solution Overview

Problem

Current methods for producing cubic sesquioxides of scandium, yttrium, or rare earth metals doped with lanthanide ions result in small crystal sizes and inadequate optical quality, requiring extreme temperature and pressure conditions, which are costly, dangerous, and inefficient.

Innovation Solution

A process involving a chemically inert crucible and a synthesis solvent like Li6(R1-xR2)(BO3)3, where R1 and R2 are scandium, yttrium, or lanthanide elements, to grow single-crystals by controlled crystallization at moderate temperatures (1000-1200°C) using a mechanical mixture of sesquioxides, allowing for larger crystal sizes with improved optical quality.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If extreme temperature and pressure conditions are used to grow cubic sesquioxide crystals, then crystal growth is achieved, but the process becomes costly, dangerous, and inefficient

Engineering Contradiction:
Improvecrystal growth successVSAvoidextreme conditions cost and danger
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The patent changes the temperature parameter from extreme conditions (>2400°C) to moderate conditions (1000-1250°C) by using a flux growth technique with a synthesized solvent. This parameter change makes the process safer, less costly, and more efficient while still achieving successful crystal growth of cubic sesquioxides with high optical quality

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces a synthesized flux solvent with formula Li6(R1-xR2)(BO3)3 as an intermediary medium to facilitate crystal growth. This intermediary enables the dissolution of sesquioxide solutes and controlled crystallization at moderate temperatures, avoiding the need for extreme conditions that are costly and dangerous

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If conventional methods are used to produce cubic sesquioxides, then crystal growth occurs, but crystal size remains small and optical quality is inadequate

Engineering Contradiction:
Improveoptical qualityVSAvoidcrystal size
Core Design Contradiction:
Manufacturing precisionVSVolume of moving object

Solution Approach 1:

The patent changes the temperature parameter to a specific moderate range (1000-1250°C) and controls the cooling rate (maximum 1°C/hour) to optimize crystal growth. These parameter changes enable the formation of large single crystals with high optical quality, resolving the contradiction between crystal size and optical quality

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a periodic cooling process with a controlled maximum rate of 1°C/hour after reaching the synthesis temperature. This periodic, controlled cooling allows for gradual crystallization, enabling large crystal sizes to form while maintaining high optical quality throughout the crystal structure

Inventive Principle:
Principle #19Periodic action

3Manufacturing precision

If high-temperature flux growth is used, then single-crystal growth is achieved, but post-growth treatments are required

Engineering Contradiction:
Improvesingle-crystal qualityVSAvoidpost-growth treatment time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent performs preliminary doping during the crystal growth process itself by incorporating lanthanide ions into the flux solvent and sesquioxide mixture before growth. This preliminary action ensures uniform doping throughout the crystal structure, eliminating the need for subsequent post-growth doping treatments and reducing overall processing time

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

This method enables the growth of single-crystals with high crystalline quality and larger sizes, suitable for industrial applications, without the need for extreme conditions, and allows for easy doping and reduced post-growth treatments.

Implementation Method 1

bringing the pulverulent mixture PM1 obtained above in stage 1) to a temperature TPM1 at least equal to the melting point (TM.p.) of said mixture and ≦1250° C., in order to bring about the dissolution of the solute in the solvent of formula (III)

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 2

the controlled cooling of the liquid solution from the temperature TPM1 down to a temperature TExp between the saturation temperature (TSat) of the liquid solution and the critical supersaturation temperature (CTSuper) of the liquid solution or the temperature of solidification of the solution, in order to bring about the controlled crystallization of the expected sesquioxide of formula (I)

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

maintaining the temperature of the liquid solution at the temperature TPM1 for a period of time of at least 6 hours, with stirring by means of a solid support subjected to rotation around a vertical axis

Methodology Applied
Scientific EffectStirring: Stirring

Data Source

PatentUS9187845B2Method for preparing single-crystal cubic sesquioxides and uses thereof
Publication Date: 2015.11.17 CENT NAT DE LA RECH SCI (C N R S)
  • US9187845B2 patent drawing
  • US9187845B2 patent drawing
  • US9187845B2 patent drawing

AI summary

A method is provided for preparing solid or thin-film single-crystals of cubic sesquioxides (space group no. 206, Ia-3) of scandium, yttrium or rare earth elements doped with lanthanide ions with valence +III, using a high-temperature flux growth technique, and to the various uses of the single-crystals obtained according to said method, in particular in the field of optics.