Graphene Precursor Identification via XRD Peak Separation

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Solution Overview

Problem

The existing methods for distinguishing graphene precursors from graphite raw materials using powder X-ray diffraction patterns face challenges in peak separation, especially when the profiles are gently sloping and overlapping, making it difficult to determine the ratio of hexagonal and rhombohedral crystal structures, which is crucial for producing graphene at low cost using the peeling method.

Innovation Solution

A method that specifies the zero-point of the diffraction angle by assuming equal interplanar spacing and crystal structure within graphene sheets, calculates peak positions and integrated intensities for both crystal systems, and determines the suitability of the graphite raw material as a graphene precursor by comparing the integrated intensity ratio of the 101 diffracted beams, enabling precise peak separation and material identification.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If the existing powder X-ray diffraction method is used to distinguish graphene precursors, then the measurement can be performed, but the peak separation becomes difficult when profiles are gently sloping and overlapping

Engineering Contradiction:
Improvepeak separation accuracyVSAvoidpeak separation difficulty
Core Design Contradiction:
Measurement precisionVSDifficulty of detecting and measuring

Solution Approach 1:

The patent applies preliminary action by performing zero-point specification and peak position calculation before integrated intensity measurement. By pre-calculating peak positions based on diffraction angle and interplanar spacing relationships, the method prepares the data in advance for more accurate peak separation and integration, resolving the difficulty of separating overlapping peaks in gently sloping profiles

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent segments the diffraction pattern analysis into distinct steps: zero-point specification, peak position calculation, and integrated intensity calculation. By dividing the complex peak separation task into these sequential segments, each with specific calculation formulas, the method achieves accurate separation of hexagonal and rhombohedral peaks even when they overlap in gently sloping profiles

Inventive Principle:
Principle #1Segmentation

2Ease of manufacture

If the peeling method is used to produce graphene from graphite, then production cost is reduced, but the suitability of graphite raw material must be precisely determined

Engineering Contradiction:
Improveproduction costVSAvoidmaterial suitability determination
Core Design Contradiction:
Ease of manufactureVSMeasurement precision

Solution Approach 1:

The patent replaces manual or qualitative assessment of graphite suitability with an automated calculation system based on XRD data. By substituting mechanical/subjective judgment with computational analysis of diffraction patterns, the method provides precise, objective determination of whether graphite raw material is suitable for the peeling method, ensuring low-cost production only when material suitability is confirmed

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

Solution Approach 2:

The patent uses parameter changes by calculating the ratio of integrated intensities of specific diffraction peaks (100 and 101 peaks) to determine material suitability. By transforming the suitability assessment into a quantitative parameter (intensity ratio), the method provides an objective criterion for selecting graphite raw materials appropriate for cost-effective peeling method production

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

This approach allows for accurate differentiation of graphene precursors, enabling low-cost graphene production by ensuring the correct ratio of hexagonal and rhombohedral crystal structures, thereby enhancing the efficiency and productivity of the peeling method.

Implementation Method 1

The crystal structure of graphite can be figured out by a method (X-ray diffraction) of examining a diffraction phenomenon generated by scattering or interference of X-rays when a sample is irradiated with the X-rays.

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Implementation Method 2

examining a diffraction phenomenon generated by scattering or interference of X-rays

Methodology Applied
Scientific EffectDiffraction: Diffraction

Data Source

PatentEP3795985B1Distinguishing method of graphene precursor, and distinguishing apparatus and distinguishing program thereof
Publication Date: 2024.09.04 RIGAKU CORP
  • EP3795985B1 patent drawingFigure 1A~1B
  • EP3795985B1 patent drawingFigure 2
  • EP3795985B1 patent drawingFigure 3

AI summary

Provided is a determination method of distinguishing a graphene precursor, that surely certainly enables peak separation by peak profile fitting via a powder X-ray diffraction pattern with respect to graphite raw material, and also provided are a determination distinguishing device and a determination distinguishing program thereof. There is provided a distinguishing method of a graphene precursor with respect to graphite raw material in which a hexagonal crystal system graphite layer and a rhombohedral crystal system graphite layer are mixed, the method comprising the steps of specifying a zero-point of a diffraction angle for powder X-ray diffraction data of the graphite raw material; calculating peak positions specific to the hexagonal crystal system graphite layer and the rhombohedral crystal system graphite layer from the specified zero-point, by assuming that an interplanar spacing between graphene sheets that form the graphite raw material is the same and a crystal structure inside the graphene sheets is the same in any graphite layer mixed in the graphite raw material; calculating integrated intensities at the calculated peak positions; and determining whether the graphite raw material is a graphene precursor or not based on the calculated integrated intensities.