Large-Diameter Garnet Crystal Growth via Axial Temperature Gradient

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Solution Overview

Problem

Current methods for growing large-diameter yttrium and lutetium aluminate crystals with garnet structure, such as the Czochralski method, face challenges in achieving optical quality and uniformity due to temperature gradients and dopant incorporation issues, leading to inhomogeneous crystals and high production costs.

Innovation Solution

A method involving the homogenization and pressing of oxide mixtures into blocks, followed by melting and stirring with a differential axial temperature gradient or mechanical stirring, with a single crystal seed contacted to the melt surface in a crucible, allowing for controlled crystal growth and temperature regulation to achieve large, optically homogeneous crystals.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Volume of moving object

If the Czochralski method is used to grow large-diameter crystals, then crystal size can be increased, but temperature gradients cause inhomogeneity and optical quality deteriorates

Engineering Contradiction:
Improvecrystal sizeVSAvoidoptical homogeneity
Core Design Contradiction:
Volume of moving objectVSManufacturing precision

Solution Approach 1:

The patent changes the temperature gradient parameter from the conventional Czochralski method to a specifically controlled axial gradient (1-10°C/cm) in the new method. This parameter change allows large crystals to grow while maintaining thermal conditions that promote uniform dopant distribution and optical homogeneity throughout the crystal structure.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent applies preliminary homogenization to the oxide mixture before crystal growth by pressing it into blocks and pre-sintering. This preliminary action ensures uniform dopant distribution in the starting material, which prevents inhomogeneity issues during subsequent large-scale crystal growth.

Inventive Principle:
Principle #10Preliminary action

2Temperature

If iridium crucibles are used for high-temperature crystal growth, then melting point requirements are met, but radial temperature gradients increase causing growth difficulties

Engineering Contradiction:
Improvemelting point capabilityVSAvoidcrystal growth ease
Core Design Contradiction:
TemperatureVSEase of manufacture

Solution Approach 1:

The patent applies local quality by creating different temperature zones within the crucible - a steep axial gradient (1-10°C/cm) for controlled growth at the crystal-melt interface, while maintaining overall high temperature for melting. This localized temperature control enables easy growth of large crystals despite the high melting point requirements.

Inventive Principle:
Principle #3Local quality

3Quantity of substance

If dopants are added to achieve desired concentration, then crystal functionality is improved, but inhomogeneous distribution occurs in large crystals

Engineering Contradiction:
Improvedopant concentrationVSAvoidcompositional uniformity
Core Design Contradiction:
Quantity of substanceVSStability of the object's composition

Solution Approach 1:

The patent performs preliminary homogenization by pressing oxide mixtures into blocks and pre-sintering them before crystal growth. This preliminary action ensures uniform dopant distribution throughout the starting material, which maintains compositional uniformity even when growing large-diameter crystals with significant volumes.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes the temperature gradient parameter to a specifically controlled axial gradient (1-10°C/cm) that promotes uniform dopant incorporation throughout the growing crystal. This parameter change prevents the segregation and inhomogeneity that typically occurs in large crystals grown with conventional temperature profiles.

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 enables the growth of large-diameter, optically homogeneous garnet structure crystals with improved homogeneity and reduced thermal stress, achieving crystal sizes up to 500 mm with enhanced optical properties and reduced production costs compared to existing techniques.

Implementation Method 1

melt flow due to a differential axial temperature gradient

Methodology Applied
Scientific EffectTemperature gradient: Temperature Gradient

Implementation Method 2

melt flow due to a differential axial temperature gradient

Methodology Applied
Scientific EffectConvection: Convection

Implementation Method 3

a single crystal seed is contacted with the surface of the homogenised melt contained within the crucible and placed within a growing furnace

Methodology Applied
Scientific EffectCrystallisation: Crystallisation

Data Source

PatentUS9499923B2Method for the preparation of doped garnet structure single crystals with diameters of up to 500 mm
Publication Date: 2016.11.22 CRYTUR SPOL SRO
  • US9499923B2 patent drawing
  • US9499923B2 patent drawing
  • US9499923B2 patent drawing

AI summary

Preparation of lutetium and yttrium aluminate single crystals doped with rare earth oxides and transition elements consists in the preparation of oxide mixture sinter which is melted throughout and homogenized for a period of at least one hour. The crystal growth rate and broadening of the crystal cone are maintained uniform at an angle of at least 60° from the crystal axis up to a diameter of at least 80% of the crucible diameter which is at least 100 mm. The completion of the process occurs by separating the crystal from the melt while the crystal continues to be positioned inside the crucible in the zone wherein it was grown, and wherein final tempering of the crystal also takes place.