Zirconium-Doped Silicon Nitride Sintering for Lower Firing Energy

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Solution Overview

Problem

Existing methods for producing silicon nitride sintered bodies at high temperatures result in high energy consumption and carbon dioxide emissions, while attempts to reduce firing temperatures lead to insufficient strength for applications in wear-resistant members and semiconductor substrates.

Innovation Solution

Incorporating not less than 0.1 mass % and not more than 10 mass % of zirconium when converted to oxide into the silicon nitride sintered body, which forms a liquid phase at around 1,300° C, allowing for low-temperature firing of less than 1,650° C while maintaining high strength.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If high temperature firing (1600-2000°C) is used to produce silicon nitride sintered bodies, then high strength (≥700 MPa or ≥900 MPa) is achieved, but energy consumption and carbon dioxide emissions increase

Engineering Contradiction:
Improvethree-point bending strengthVSAvoidenergy consumption
Core Design Contradiction:
StrengthVSUse of energy by stationary object

Solution Approach 1:

The patent changes the chemical composition parameters by adding specific amounts of zirconium (0.1-10 mass%) and controlling the ratio of α-silicon nitride to β-silicon nitride crystal grains. This compositional parameter change enables the material to achieve high strength at lower firing temperatures (1200-1650°C), thus resolving the contradiction between strength and energy consumption

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite microstructure consisting of both α-silicon nitride and β-silicon nitride crystal grains in specific ratios, along with zirconium additions. This composite material approach allows the sintered body to achieve high strength at reduced firing temperatures, addressing the energy consumption issue while maintaining mechanical performance

Inventive Principle:
Principle #40Composite materials

2Use of energy by stationary object

If firing temperature is reduced to decrease energy consumption, then carbon dioxide emissions are reduced, but strength becomes insufficient (≈140 MPa at 1300-1375°C)

Engineering Contradiction:
Improveenergy consumptionVSAvoidthree-point bending strength
Core Design Contradiction:
Use of energy by stationary objectVSStrength

Solution Approach 1:

The patent modifies the chemical composition by adding zirconium (0.1-10 mass%) and controlling the crystal grain ratio, which fundamentally changes the sintering behavior of the material. This enables low-temperature sintering (1200-1650°C) to produce bodies with strength ≥600 MPa, resolving the contradiction between energy consumption and strength

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates local structural optimization by controlling the distribution and ratio of α-silicon nitride and β-silicon nitride crystal grains, along with zirconium distribution. This local quality control ensures that even at lower temperatures, the material achieves sufficient strength for practical applications

Inventive Principle:
Principle #3Local quality

3Use of energy by stationary object

If zirconium is added to enable low-temperature firing, then energy consumption is reduced, but manufacturing precision must be controlled to maintain strength ≥600 MPa

Engineering Contradiction:
Improveenergy consumptionVSAvoidfiring temperature control
Core Design Contradiction:
Use of energy by stationary objectVSManufacturing precision

Solution Approach 1:

The patent establishes specific parameter ranges: zirconium content (0.1-10 mass%), α-silicon nitride to β-silicon nitride ratio (0.01 to 0.5), and firing temperature (1200-1650°C). These controlled parameter changes enable low-temperature firing while maintaining manufacturing precision and achieving strength ≥600 MPa, resolving the contradiction between energy consumption and manufacturing precision

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 approach enables the production of silicon nitride sintered bodies with a three-point bending strength of not less than 600 MPa and a dielectric strength of not less than 13 kV/mm, suitable for wear-resistant members and semiconductor substrates, while reducing energy consumption and environmental impact.

Implementation Method 1

Incorporating not less than 0.1 mass % and not more than 10 mass % of zirconium when converted to oxide into the silicon nitride sintered body, which forms a liquid phase at around 1,300° C, allowing for low-temperature firing of less than 1,650° C while maintaining high strength

Methodology Applied
Scientific EffectLiquid phase formation: Phase Change

Data Source

PatentUS20250066258A1Silicon nitride sintered body, wear-resistant member, substrate for semiconductor devices, and method for producing silicon nitride sintered body
Publication Date: 2025.02.27 NITERRA MATERIALS CO LTD
  • US20250066258A1 patent drawing
  • US20250066258A1 patent drawing
  • US20250066258A1 patent drawing

AI summary

A silicon nitride sintered body according to an embodiment includes not less than 0.1 mass % and not more than 10 mass % of zirconium when converted to oxide. In XRD analysis (2θ) of any cross section of the silicon nitride sintered body, 0.01≤I35.3/I27.0≤0.5 and 0≤I33.9/I27.0≤1.0 are satisfied; I35.3 is a maximum peak intensity detected at 35.3±0.2° based on α-silicon nitride crystal grains; I27.0 is a most intense peak detected at 27.0±0.2° based on β-silicon nitride crystal grains; and I33.9 is a most intense peak detected at 33.9±0.2° based on zirconium nitride.