Raman Spectroscopy for Glass Ceramic Phase Quality Control

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Solution Overview

Problem

Current methods for determining crystal phases in glass ceramics, such as XRD, are costly, time-consuming, and prone to false positives, making them unsuitable for quality control in manufacturing, especially in 3D forming processes where temperature variations can lead to undesirable haze and affect mechanical and chemical properties.

Innovation Solution

The use of Raman spectroscopy for determining crystal phases, calibrated by XRD, which involves applying energy to the sample, detecting Raman spectral energy, determining predetermined energy peaks, applying a baseline, and calculating corrected peak values to identify crystal phases, offering a faster, more cost-effective, and accurate method for quality control.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If XRD is used to determine crystal phases, then measurement precision is improved, but device complexity and cost increase

Engineering Contradiction:
Improvecrystal phase determination accuracyVSAvoidinstrument complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent replaces the mechanical XRD system with an optical Raman spectroscopy system. Instead of using X-ray diffraction machinery, the invention uses laser excitation and optical detection to obtain crystal phase information through Raman scattering, thereby reducing device complexity while maintaining measurement capability.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent creates a simplified optical copy of the XRD measurement process. By using Raman spectroscopy to detect vibrational modes of crystal phases, the system obtains equivalent phase identification information without requiring the complex mechanical XRD apparatus, effectively copying the analytical function with simpler technology.

Inventive Principle:
Principle #26Copying

2Measurement precision

If XRD is used for quality control, then measurement precision is improved, but loss of time increases

Engineering Contradiction:
Improvephase identification accuracyVSAvoidanalysis time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The substitution of XRD with Raman spectroscopy inherently reduces analysis time because the optical measurement can be performed rapidly without the time-consuming sample preparation and data collection required for XRD, enabling faster quality control decisions.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The Raman measurement process allows for continuous or rapid sequential measurements without interrupting the manufacturing flow. The system can quickly scan and identify phases continuously, maintaining productive action throughout the quality control process unlike the more discrete and time-consuming XRD measurements.

Inventive Principle:
Principle #20Continuity of useful action

3Measurement precision

If XRD is used for phase determination, then measurement precision is improved, but object-affected harmful factors increase

Engineering Contradiction:
Improvecrystal phase detection accuracyVSAvoidradiation exposure
Core Design Contradiction:
Measurement precisionVSObject-affected harmful factors

Solution Approach 1:

The patent eliminates harmful X-ray radiation by substituting the measurement technique with optical Raman spectroscopy. Instead of exposing samples to ionizing radiation, the system uses laser excitation that induces Raman scattering, a non-harmful optical interaction that provides the same phase identification capability without radiation risks.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

4Device complexity

If Raman spectroscopy is used, then device complexity is reduced, but measurement precision may worsen

Engineering Contradiction:
Improveinstrument simplicityVSAvoidphase quantification accuracy
Core Design Contradiction:
Device complexityVSMeasurement precision

Solution Approach 1:

The patent implements feedback through calibration curves that relate Raman signal intensity to crystal phase concentration. By measuring standard samples and creating calibration relationships, the system continuously adjusts and refines its quantification results, ensuring accurate phase determination despite the simplicity of the underlying optical measurement technique.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent introduces calibration curves as an intermediary between the simple Raman measurements and the accurate phase quantification. These calibration relationships, established through comparison with reference materials, serve as a mediator that translates the straightforward optical signals into precise phase concentration values, bridging the gap between measurement simplicity and result accuracy.

Inventive Principle:
Principle #24Intermediary (Mediator)

5Loss of time

If Raman spectroscopy is used for quality control, then loss of time is reduced, but device complexity may increase

Engineering Contradiction:
Improvequality control measurement timeVSAvoidspectroscopy equipment complexity
Core Design Contradiction:
Loss of timeVSDevice complexity

Solution Approach 1:

The patent replaces complex mechanical XRD equipment with a simpler optical Raman system that achieves faster measurements. The substitution of measurement physics enables rapid data collection while maintaining or improving measurement speed, directly addressing the time loss issue without requiring complex instrumentation.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

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

Raman spectroscopy provides a lower-cost, faster, and more accurate method for determining crystal phases, reducing radiation exposure and sensitivity to sample geometry, allowing for real-time quality control and detection of undesirable phases, thereby improving the manufacturing process and product quality.

Implementation Method 1

detecting raw Raman spectral energy that is given off by the sample using a detector

Methodology Applied
Scientific EffectRaman scattering:

Data Source

PatentUS11204280B2Method of phase quality control for glass ceramics in manufacturing
Publication Date: 2021.12.21 CORNING INC
  • US11204280B2 patent drawing
  • US11204280B2 patent drawing
  • US11204280B2 patent drawing

AI summary

A method for determining crystal phases of a glass ceramic sample, including the steps of applying energy to the sample using an excitation source, detecting raw Raman spectral energy that is given off by the sample using a detector, wherein the raw Raman spectral energy includes peak values, determining a plurality of predetermined energy peaks based off a composition of the sample, superimposing the plurality of predetermined energy peaks over the raw Raman spectral energy, applying a baseline value between each predetermined energy peak, subtracting the baseline value from the raw Raman spectral energy, calculating corrected peak values based on the raw Raman spectral energy and baseline value, and determining the crystal phases of the glass ceramic sample based on the corrected peak values.