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Toward a Correlative Metrology Approach on the Same 2D Flake: Graphene Oxide Case Study-Sample Preparation and
Lydia Chibane1,2, Alexandra Delvallée1, Nolwenn Fleurence1
1Laboratoire National de Métrologie et D'Essais (LNE), 29 Avenue Roger Hennequin, 78190 Trappes, France.
Nanomaterials (Basel, Switzerland)
|December 24, 2025
Summary
Producing graphene oxide (GO) via reduction is common, but controlling it needs better characterization. This study offers a correlative metrology strategy using multiple microscopy techniques to monitor GO reduction reliably.
Area of Science:
- Materials Science
- Nanotechnology
- Surface Science
Background:
- Graphene production is complex, hindering widespread applications.
- Reduction of graphene oxide (GO) is a common method for graphene synthesis.
- Current characterization lacks a comprehensive methodology for GO reduction monitoring.
Purpose of the Study:
- To propose a correlative metrology strategy for characterizing graphene oxide reduction.
- To provide guidelines for substrate selection and technique-specific precautions.
- To establish a reliable method for monitoring the GO reduction process.
Main Methods:
- Correlative metrology integrating Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM), Raman Microscopy/Spectroscopy, Scanning Microwave Microscopy (SMM), and Scanning Thermal Microscopy (SThM).
- Evaluation of substrate suitability, focusing on silicon and silicon dioxide on silicon.
- Analysis of potential sample degradation caused by each microscopy technique.
Main Results:
- Identified silicon and silicon dioxide on silicon as suitable substrates.
- Determined optimal sequence and precautions for applying multiple microscopy techniques to GO flakes.
- Developed a strategy to obtain reliable data for monitoring GO reduction.
Conclusions:
- A comprehensive correlative metrology approach is essential for reliable GO characterization.
- Careful substrate selection and technique sequencing minimize degradation and ensure data integrity.
- The proposed methodology enables effective monitoring of the graphene oxide reduction process.

