Silicon Nitride Beta-Eucryptite Composite Thermal Expansion Control

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Solution Overview

Problem

Existing methods for producing sintered ceramic composites using silicon nitride and β-eucryptite fail to achieve dimensional stability and mechanical properties suitable for large-size optical elements and structures in space applications, as they result in a composite with a coefficient of thermal expansion incompatible with space domain requirements and compromised mechanical properties due to reactions and phase changes during sintering.

Innovation Solution

A process involving a first heat treatment above the melting temperature of β-eucryptite, followed by a second heat treatment for crystallization, and optional steps like washing the silicon nitride powder and calcining lithium aluminosilicate powders, to maintain β-eucryptite's crystalline form and composition, ensuring a composite with a low coefficient of thermal expansion and mechanical properties compatible with space applications.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If the mass proportion of β-eucryptite in the mixture is increased to at least 60% to achieve a low coefficient of thermal expansion suitable for space applications, then the coefficient of thermal expansion becomes suitable, but the mechanical properties of the composite deteriorate due to the low Young's modulus of β-eucryptite (70 GPa) compared to silicon nitride

Engineering Contradiction:
Improvecoefficient of thermal expansionVSAvoidmechanical properties
Core Design Contradiction:
Stability of the object's compositionVSStrength

Solution Approach 1:

The invention changes the chemical composition parameters of the lithium aluminosilicate phase by controlling the molar ratios of Li2O, Al2O3, and SiO2 to form β-eucryptite with specific stoichiometry (Li2O·Al2O3·2SiO2). This precise parameter control ensures the phase forms with the desired negative thermal expansion coefficient while maintaining structural integrity for mechanical strength

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention creates a composite ceramic material consisting of two phases: silicon nitride matrix and β-eucryptite crystalline phase. The composite structure allows the silicon nitride to provide mechanical strength while the β-eucryptite phase provides negative thermal expansion, achieving both high strength and low thermal expansion coefficient simultaneously

Inventive Principle:
Principle #40Composite materials

2Reliability

If the sintering temperature is increased above the melting temperature of β-eucryptite to achieve complete sintering of silicon nitride, then the sintering is complete, but the β-eucryptite undergoes phase changes and reactions that modify its composition and reduce the negative thermal expansion effect

Engineering Contradiction:
Improvesintering completenessVSAvoidβ-eucryptite composition
Core Design Contradiction:
ReliabilityVSStability of the object's composition

Solution Approach 1:

The invention performs preliminary classification of the powder mixture before sintering to ensure optimal particle size distribution and intimate mixing of silicon nitride and lithium aluminosilicate powders. This preliminary preparation ensures uniform heating and reaction during sintering, allowing complete sintering at controlled temperatures while preventing excessive phase transformations

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention precisely controls the sintering temperature parameter to remain above the melting point of β-eucryptite for complete sintering but below the temperature that causes excessive composition modification. The controlled temperature parameter achieves the balance between complete sintering and composition stability

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

The process enables the production of sintered ceramic composites with a very low coefficient of thermal expansion and mechanical properties suitable for optical applications in space, allowing for the creation of large-size optical elements and structures with precise control over thermal expansion and mechanical integrity.

Implementation Method 1

a first heat treatment of a composite of silicon nitride and of the first lithium aluminosilicate obtained from the first mixture to sinter the silicon nitride

Methodology Applied
Scientific EffectSintering: Sintering

Implementation Method 2

a second heat treatment to crystallize the β-eucryptite, subsequent to the first heat treatment

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

β-eucryptite has the particularity of possessing a strongly negative coefficient of thermal expansion, ie it contracts under the effect of a rise in temperature

Methodology Applied
Scientific EffectNegative thermal expansion: Negative Thermal Expansion

Data Source

PatentEP2383243B1Method of making a composite ceramic material based on silicon nitride and beta-eucryptite
Publication Date: 2019.04.03 THALES SA
  • EP2383243B1 patent drawingFigure 1
  • EP2383243B1 patent drawingFigure 2

AI summary

The process of fabricating a sintered ceramic composite material made of silicon nitride and beta -eucryptite materials, comprises creating (101) a first mixture of silicon nitride powder in crystalline form and a powder of a first lithium aluminosilicate in crystalline form, performing (105) a first heat treatment on silicon nitride composite and the first lithium aluminosilicate obtained from the first mixture to sinter silicon nitride and to obtain a ceramic composite made of silicon nitride and beta -eucryptites, and performing a second heat treatment to crystallize the beta -eucryptites. The process of fabricating a sintered ceramic composite material made of silicon nitride and beta -eucryptite materials, comprises creating (101) a first mixture of silicon nitride powder in crystalline form and a powder of a first lithium aluminosilicate in crystalline form, performing (105) a first heat treatment on silicon nitride composite and the first lithium aluminosilicate obtained from the first mixture to sinter silicon nitride and to obtain a ceramic composite made of silicon nitride and beta -eucryptites, and performing a second heat treatment to crystallize the beta -eucryptites. The lithium aluminosilicate composition is represented as (Li 2O) x(Al 2O 3) y(SiO 2) z, where entire molar fractions (x, y, z) is different from (1, 1, 2). The first heat treatment is carried out at a first temperature greater than melting temperature of beta -eucryptite under the operating conditions. The second heat treatment is carried out by maintaining the ceramic composite and beta -eucryptite at a temperature of 500-800[deg] C, and comprises performing nucleation at a specified temperature and growth at a temperature greater than the nucleation temperature. The silicon nitride powder is washed to remove the silica polluting the powder before mixing it with the lithium aluminosilicate. The first lithium aluminosilicate powder is fabricated by producing a mixture of lithium carbonate, alumina and silica powder, and calcining a powder obtained from the mixture to obtain the first lithium aluminosilicate. The calcination step comprises raising the temperature to reach a maximum and then decreasing the temperature. The crystals of silicon nitride powder are nanometric or micrometric, and the crystals of the first lithium aluminosilicate powder are nanometric or micrometric.