Carbon Black Polymer Composite for Dynamic Nuclear Polarization

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Solution Overview

Problem

Current polymer composite materials, especially those containing carbon black, achieve low proton spin polarization in dynamic nuclear polarization, and existing techniques for structural analysis of multicomponent systems face challenges with solvent contrast variation neutron scattering and require high proton spin polarization.

Innovation Solution

A polymer composite material with a thickness of 0.8 mm or less, doped with a paramagnetic radical compound, and a deuterated solvent is used to achieve high proton spin polarization and accurate structural analysis through 1H dynamic nuclear polarization contrast variation neutron scattering, even when proton spin polarization is less than 60%. The material is produced by diffusing the paramagnetic radical compound in an inert gas or vacuum environment to prevent temperature increases and ensure uniform radical distribution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If a polymer composite material containing carbon black is used for dynamic nuclear polarization, then the material can be applied to neutron scattering experiments, but the proton spin polarization is very low (at most 20%)

Engineering Contradiction:
Improveproton spin polarizationVSAvoidapplicability to neutron scattering experiments
Core Design Contradiction:
ReliabilityVSAdaptability or versatility

Solution Approach 1:

The patent changes the physical and chemical parameters of the polymer composite material by introducing a deuterated solvent with specific properties (deuterium content, molecular weight, viscosity) to optimize the polarization transfer efficiency. This parameter change enables achieving high proton spin polarization (greater than 40%) while maintaining the material's applicability to neutron scattering experiments containing carbon black

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite material system combining polymer matrix, carbon black filler, and deuterated solvent. This multi-component composite structure allows the material to simultaneously achieve high proton spin polarization for NMR experiments and maintain the structural properties needed for neutron scattering experiments, resolving the contradiction between polarization efficiency and experimental applicability

Inventive Principle:
Principle #40Composite materials

2Measurement precision

If solvent contrast variation neutron scattering is performed on polymer composite materials, then structural analysis can be performed, but the technique requires solvent swelling of samples which is difficult to perform on non-swollen samples

Engineering Contradiction:
Improvestructural analysis accuracyVSAvoidsample preparation complexity
Core Design Contradiction:
Measurement precisionVSEase of operation

Solution Approach 1:

The patent develops a polymer composite material that serves multiple functions: it provides high proton spin polarization for NMR experiments, maintains structural integrity for neutron scattering, and enables contrast variation studies. The deuterated solvent integrated into the material allows the same sample to be used for both NMR polarization experiments and neutron scattering structural analysis without requiring separate swelling procedures, achieving multi-functionality that resolves the operational complexity

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 high proton spin polarization and accurate structural analysis of multicomponent systems, improving experimental data quality and contrast conditions in neutron scattering and NMR experiments, despite the incorporation of carbon black.

Implementation Method 1

In dynamic nuclear polarization, electron spins having a large magnetic moment that is at least several hundred times that of a nuclear spin is introduced into a sample, and then the electron spins are polarized at a low temperature under a high magnetic field, followed by transfer of polarization from the electron spins to the nuclear spins by microwave irradiation

Methodology Applied
Scientific EffectDynamic nuclear polarization:

Implementation Method 2

electron spins are polarized at a low temperature under a high magnetic field

Methodology Applied
Scientific EffectElectron spin polarization:

Implementation Method 3

transfer of polarization from the electron spins to the nuclear spins by microwave irradiation

Methodology Applied
Scientific EffectMicrowave irradiation: Microwave Radiation

Implementation Method 4

This technique utilizes the difference in contrast between protium and deuterium, which is the peculiar nature of neutron scattering

Methodology Applied
Scientific EffectNeutron scattering: Scattering

Implementation Method 5

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

Methodology Applied
Scientific EffectSolvent contrast variation:

Implementation Method 6

it has been reported that samples in which a stable vaporized radical compound is diffused into a pure polymer material

Methodology Applied
Scientific EffectVapor diffusion: Diffusion

Implementation Method 7

stable vaporized radical compound

Methodology Applied
Scientific EffectVapor phase:

Implementation Method 8

involves swelling a polymer composite material in a mixture of a protium solvent and a deuterium solvent in varied ratios

Methodology Applied
Scientific EffectSolvent swelling:

Data Source

PatentEP3312233B1Polymer composite material for 1h dynamic nuclear polarization experiments and method for producing the same, and polymer composite material for 1h dynamic nuclear polarization contrast variation neutron scattering experiments
Publication Date: 2020.09.02 SUMITOMO RUBBER INDUSTRIES LTD
  • EP3312233B1 patent drawingFigure 1
  • EP3312233B1 patent drawing
  • EP3312233B1 patent drawing

AI summary

Provided is a polymer composite material which has a high proton spin polarization even though it is a polymer composite material containing carbon black. The present invention relates to a polymer composite material for 1H dynamic nuclear polarization experiments, containing carbon black, having a thickness of 0.8 mm or less, and being doped with a paramagnetic radical compound.