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Controlled covalent functionalization of graphene is difficult. This study introduces a hexylation method for graphene, with thermogravimetric analysis proving effective for detecting low concentrations of functional groups.

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TGA-GC/MSgrapheneoxo-functionalized graphenereductive functionalizationstatistical Raman spectroscopy

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Area of Science:

  • Materials Science
  • Nanotechnology
  • Organic Chemistry

Background:

  • Controlled covalent functionalization of graphene is challenging due to material heterogeneity.
  • Existing methods often lack quantification or fail to distinguish covalent from non-covalent functionalization.

Purpose of the Study:

  • To develop a reliable method for controlled covalent functionalization of graphene.
  • To accurately quantify the degree of functionalization, specifically hexylation.

Main Methods:

  • A three-step procedure involving oxidation and exfoliation of graphite.
  • Subsequent reduction and hexylation of the exfoliated graphene.
  • Analysis using Raman spectroscopy and thermogravimetric analysis coupled with gas chromatography and mass spectrometry (TGA-GC/MS).

Main Results:

  • Raman spectroscopy could not detect hexyl groups at 0.03% concentration due to pre-existing defects (0.7%).
  • TGA-GC/MS successfully detected and confirmed the hexylation reaction.
  • The functionalization efficiency was comparable to established methods on chemical vapor deposition (CVD)-graphene and bulk graphite.

Conclusions:

  • Thermogravimetric analysis coupled with GC-MS is a sensitive method for detecting low-level covalent functionalization on graphene.
  • The developed hexylation process offers a viable route for controlled graphene functionalization.
  • This work addresses limitations in quantifying covalent functionalization on graphene materials.