Polymer Deterioration Analysis via X-ray Absorption

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Solution Overview

Problem

Current methods, such as XPS and FT-IR, struggle to analyze the deterioration of each diene polymer in a polymer blend, as they provide bulk information or overlap peaks, making it difficult to distinguish between oxygen and ozone deterioration, and individual polymer analysis.

Innovation Solution

A method involving high-intensity monochromatic x-rays is used to irradiate polymer materials, measuring x-ray absorption while varying energy, calculating normalization constants, and performing waveform separation to determine the degree of deterioration of each diene polymer, including separating peaks for π* transitions and distinguishing oxygen and ozone contributions.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Illumination intensity

If XPS is used to analyze surface deterioration, then surface sensitivity is improved, but the ability to distinguish individual polymer components deteriorates due to peak overlap

Engineering Contradiction:
Improvesurface sensitivityVSAvoidcomponent differentiation precision
Core Design Contradiction:
Illumination intensityVSMeasurement precision

Solution Approach 1:

The invention segments the analysis by performing waveform separation on x-ray absorption spectra to resolve overlapping peaks into individual polymer component contributions. This allows differentiation of isoprene and butadiene polymers despite their overlapping C=C and C-O peaks in the 280-300 eV range, enabling precise measurement of each component's deterioration state

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The invention introduces x-ray absorption spectroscopy as an intermediary technique between surface sensitivity requirements and component differentiation needs. By using near-edge x-ray absorption fine structure (NEXAFS) spectroscopy, the method achieves both surface sensitivity and the ability to distinguish individual polymer components through their unique absorption spectra

Inventive Principle:
Principle #24Intermediary (Mediator)

2Loss of information

If FT-IR or NMR is used for detailed chemical analysis, then chemical state information is improved, but surface sensitivity deteriorates due to bulk information dominance

Engineering Contradiction:
Improvechemical state informationVSAvoidsurface sensitivity
Core Design Contradiction:
Loss of informationVSIllumination intensity

Solution Approach 1:

The invention replaces traditional FT-IR or NMR mechanical measurement systems with x-ray absorption spectroscopy. This substitution maintains detailed chemical state information capability while achieving surface sensitivity, as x-rays interact with core electrons and the resulting photoelectrons provide depth-resolved chemical information

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

3Reliability

If conventional x-ray absorption spectra are measured, then overall deterioration detection is improved, but the ability to analyze individual polymer components and deterioration mechanisms deteriorates

Engineering Contradiction:
Improvedeterioration detection reliabilityVSAvoidcomponent and mechanism analysis precision
Core Design Contradiction:
ReliabilityVSMeasurement precision

Solution Approach 1:

The invention changes the measurement parameters by using monochromatic high-intensity x-rays with brilliance of at least 10^10 photons/s/mrad^2/0.1% bandwidth and photon flux of at least 10^12 photons/s/cm^2. This enables detection of subtle spectral features and facilitates waveform separation to resolve individual polymer components and their specific deterioration mechanisms

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention employs dynamic waveform separation techniques that adaptively resolve overlapping spectral features. By dynamically adjusting the separation parameters based on the measured spectra, the method can distinguish between C=C and C-O bonds and differentiate oxygen deterioration from ozone deterioration in each polymer component

Inventive Principle:
Principle #15Dynamics

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 allows for detailed analysis of each diene polymer's deterioration, determining the degree of deterioration, contribution rates of oxygen and ozone, and the amount of bonded oxygen and ozone, enabling precise evaluation of polymer blend degradation.

Implementation Method 1

measuring x-ray absorption in a micro area of the polymer material while varying the energy of the x-rays

Methodology Applied
Scientific EffectX-ray absorption: Absorption (EM radiation)

Implementation Method 2

measuring x-ray absorption spectra near an absorption edge of a specific element

Methodology Applied
Scientific EffectNear-edge x-ray absorption fine structure (NEXAFS): Absorption Spectroscopy

Data Source

PatentEP2775294B1Deterioration analyzing method
Publication Date: 2019.02.20 SUMITOMO RUBBER INDUSTRIES LTD
  • EP2775294B1 patent drawingFigure 1-1~1-2
  • EP2775294B1 patent drawingFigure 1-3~1-4
  • EP2775294B1 patent drawingFigure 1-5~1-6

AI summary

The present invention provides a method of deterioration analysis that enables detailed analysis of the deterioration, especially of the surface, of a polymer material containing at least two diene polymers. The present invention relates to a method of deterioration analysis including: irradiating a polymer material containing at least two diene polymers with high intensity x-rays; and measuring x-ray absorption while varying the energy of the x-rays, to analyze the deterioration of each diene polymer.