Sulfur Concentration Evaluation in Polymer Composites via Dynamic Nuclear Polarization

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Solution Overview

Problem

Existing methods struggle to accurately quantify the concentration of sulfur in polymer composite materials with non-uniform polymer concentrations due to variations in composition throughout the sample.

Innovation Solution

The method employs small-angle neutron scattering combined with 1H dynamic nuclear spin polarization, where a polymer composite material is immersed in a deuterated solvent and subjected to 1H dynamic nuclear spin polarization, allowing for accurate measurement of sulfur concentration without errors from position dependence or degree of swelling.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If conventional neutron scattering methods are used to analyze multicomponent systems, then structural analysis capability is improved, but measurement precision of sulfur concentration deteriorates due to composition variations and swelling effects

Engineering Contradiction:
Improvestructural analysis capabilityVSAvoidsulfur concentration measurement precision
Core Design Contradiction:
Adaptability or versatilityVSMeasurement precision

Solution Approach 1:

The patent changes the nuclear spin state parameter of protons in the polymer matrix from thermal equilibrium to polarized state through dynamic nuclear polarization. This parameter change creates a binary contrast effect where polarized protons scatter neutrons differently than non-polarized protons, enabling sulfur concentration measurement independent of polymer concentration variations and swelling effects. The scattering intensity becomes directly proportional to sulfur concentration regardless of sample composition variations.

Inventive Principle:
Principle #35Parameter changes

2Measurement precision

If 1H dynamic nuclear polarization is applied to enhance contrast, then measurement precision of sulfur concentration is improved, but device complexity increases due to additional polarization equipment

Engineering Contradiction:
Improvesulfur concentration measurement precisionVSAvoidpolarization equipment complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent replaces conventional mechanical/sample preparation approaches (multiple swelling solvents, manual concentration control) with a physical field-based approach using dynamic nuclear polarization. Instead of mechanically controlling sample composition to achieve contrast, the invention uses microwave irradiation and magnetic fields to polarize nuclear spins, substituting mechanical control with electromagnetic field control. This reduces the need for complex sample preparation equipment while enhancing measurement precision.

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

This approach enables precise evaluation of sulfur concentration in polymer composite materials, even when sulfur is present in amounts as low as 1% by mass, with a large contrast difference between sulfur and the polymer, ensuring accurate measurement of sulfur concentration levels.

Implementation Method 1

a paramagnetic radical is introduced into a material, and then the material is irradiated with microwaves at an extremely low temperature under a magnetic field to polarize the proton spins in the material

Methodology Applied
Scientific EffectDynamic nuclear polarization:

Implementation Method 2

the material is irradiated with microwaves at an extremely low temperature under a magnetic field

Methodology Applied
Scientific EffectMicrowave irradiation: Microwave Radiation

Implementation Method 3

the material is irradiated with microwaves at an extremely low temperature under a magnetic field

Methodology Applied
Scientific EffectMagnetic field: Magnetic Field

Implementation Method 4

Contrast variation neutron scattering is a dominant technique for the structural analysis of multicomponent systems

Methodology Applied
Scientific EffectNeutron scattering: Scattering

Implementation Method 5

a method of evaluating a concentration of sulfur in a polymer composite material by small-angle neutron scattering with 1H dynamic nuclear spin polarization

Methodology Applied
Scientific EffectSmall-angle neutron scattering:

Data Source

PatentUS12306117B2Method of evaluating concentration of sulfur
Publication Date: 2025.05.20 SUMITOMO RUBBER INDUSTRIES LTD
  • US12306117B2 patent drawing
  • US12306117B2 patent drawing
  • US12306117B2 patent drawing

AI summary

Provided is a method of evaluating a concentration of sulfur in a polymer composite material. The present disclosure relates to a method of evaluating a concentration of sulfur in a polymer composite material by small-angle neutron scattering with 1H dynamic nuclear spin polarization.