Epitaxial Alpha-Quartz Layer Preparation via Sol-Gel and Heat Treatment

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Solution Overview

Problem

Current methods for producing thin layers of α-quartz are energy-intensive, inefficient, and unable to achieve thicknesses between 5 nm and 50 μm with high yield and control, while also being costly and requiring extreme conditions or specific materials.

Innovation Solution

A process involving the preparation of a silica precursor composition, deposition on a self-supported substrate, and heat treatment at temperatures above 800 °C in the presence of catalysts like strontium, barium, or calcium to form epitaxial α-quartz layers, allowing for flexible thickness control and integration with micro and nanofabrication techniques.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If hydrothermal synthesis is used to prepare α-quartz, then single crystal quality is improved, but production time increases to about a month and energy consumption increases due to high pressure and temperature requirements

Engineering Contradiction:
Improvesingle crystal qualityVSAvoidproduction time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The invention changes the synthesis parameters from hydrothermal conditions (high pressure and temperature) to sol-gel processing followed by heat treatment at 800-1000°C. This parameter transformation enables α-quartz formation in hours rather than months, directly resolving the time contradiction while maintaining crystal quality through controlled epitaxial growth on seeded substrates

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces an amorphous silica gel layer as an intermediary medium that serves as a precursor for α-quartz formation. This intermediary allows the transformation from amorphous to crystalline state under milder conditions, avoiding the need for prolonged hydrothermal treatment and enabling faster production while preserving crystal quality

Inventive Principle:
Principle #24Intermediary (Mediator)

2Reliability

If hydrothermal synthesis is used to prepare α-quartz, then single crystal quality is improved, but energy consumption increases due to high pressure and temperature requirements

Engineering Contradiction:
Improvesingle crystal qualityVSAvoidenergy consumption
Core Design Contradiction:
ReliabilityVSUse of energy by moving object

Solution Approach 1:

The invention transforms the energy input parameters from high-pressure hydrothermal conditions to atmospheric pressure heat treatment at 800-1000°C. This parameter change significantly reduces energy consumption while maintaining the ability to produce high-quality single crystals through controlled epitaxial growth on seeded substrates

Inventive Principle:
Principle #35Parameter changes

3Reliability

If conventional hydrothermal synthesis is used, then α-quartz crystals can be obtained, but the process yield falls below 10% due to material losses in cutting and polishing steps

Engineering Contradiction:
Improveα-quartz crystal productionVSAvoidprocess yield
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The invention extracts and eliminates the unnecessary cutting and polishing steps from the conventional hydrothermal synthesis process. By directly growing α-quartz as a thin film on the substrate, the method retrieves the full value of the starting material, achieving near 100% yield compared to the below 10% yield of conventional methods

Inventive Principle:
Principle #2Taking out (Extraction)

4Reliability

If conventional hydrothermal synthesis is used, then α-quartz crystals can be obtained, but the minimum thickness of quartz layers is limited to around 50 microns

Engineering Contradiction:
Improveα-quartz crystal productionVSAvoidminimum thickness
Core Design Contradiction:
ReliabilityVSLength of moving object

Solution Approach 1:

The invention changes the growth mode from bulk crystal formation to thin-film epitaxial growth on seeded substrates. This parameter transformation enables control of quartz layer thickness down to nanometer scales, breaking the 50-micron minimum thickness limitation of conventional hydrothermal synthesis

Inventive Principle:
Principle #35Parameter changes

5Manufacturing precision

If sol-gel method is used to prepare thin films of crystalline quartz, then thickness control is improved, but the process complexity increases due to requiring germanium dioxide layer formation and removal

Engineering Contradiction:
Improvethickness controlVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention extracts and removes the complex germanium dioxide intermediary layer step from the sol-gel process. By using seeded substrates with nucleating agents, the method achieves thin-film thickness control without requiring the formation and subsequent removal of germanium layers, significantly simplifying the overall process

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention enables the substrate to self-serve as both the support and the nucleation source for α-quartz growth. The seeded substrate with embedded nucleating agents automatically guides the epitaxial growth, eliminating the need for separate germanium dioxide layer formation and removal steps

Inventive Principle:
Principle #25Self-service

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 production of high-yield, thin epitaxial α-quartz films with controlled thickness and nanostructure, from 5 nm to 10 μm, and is cost-effective and compatible with industrial processes, offering enhanced flexibility and functionality.

Implementation Method 1

a step of depositing a layer of the composition obtained above in step i) on at least part of the surface of a substrate and the formation of a layer of amorphous silica matrix

Methodology Applied
Scientific EffectSol-gel: Sol

Implementation Method 2

a heat treatment step of the amorphous silica matrix layer obtained in step ii) to obtain an epitaxially grown α-quartz layer

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

a heat treatment step of the amorphous silica matrix layer obtained in step ii) to obtain an epitaxially grown α-quartz layer

Methodology Applied
Scientific EffectEpitaxy: Epitaxy

Implementation Method 4

the heat treatment is carried out in the presence of a catalyst capable of catalysing the crystallisation of the amorphous silica matrix in the form of α-quartz

Methodology Applied
Scientific EffectCatalysis: Catalysis

Data Source

PatentEP2875172B1Process for preparing an epitaxial alpha-quartz layer on a solid substrate, material obtained and uses
Publication Date: 2019.11.06 CENT NAT DE LA RECH SCI (C N R S)
  • EP2875172B1 patent drawingFigure 1a~1c
  • EP2875172B1 patent drawingFigure 2a~2d
  • EP2875172B1 patent drawingFigure 3a~3d

AI summary

The present invention relates to a process for preparing epitaxial α-quartz layers on a solid substrate, to the material obtained according to this process, and to the various uses thereof, in particular in the electronics field.