Quantifying the Covalent Functionalization of Black Phosphorus

A straightforward quantification method to consistently determine the overall functionalization degree of covalently modified two‐dimensional (2D) black phosphorus (BP) by Raman spectroscopy has been carried out. Indeed, the successful reductive methylation of the BP lattice using sodium intercalati...

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Bibliographic Details
Published in:Angewandte Chemie International Edition 2020-11, Vol.59 (45), p.20230-20234
Main Authors: Wild, Stefan, Dinh, Xuan Thong, Maid, Harald, Hauke, Frank, Abellán, Gonzalo, Hirsch, Andreas
Format: Article
Language:English
Subjects:
31P-MAS NMR spectroscopy
black phosphorus
Covalence
covalent functionalization
Graphene
Immunoglobulins
Intercalation compounds
Magnetic resonance spectroscopy
Methylation
NMR
NMR spectroscopy
Nuclear magnetic resonance
Phosphorus
Raman spectra
Raman spectroscopy
reduction
Spectroscopy
Spectrum analysis
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Summary:A straightforward quantification method to consistently determine the overall functionalization degree of covalently modified two‐dimensional (2D) black phosphorus (BP) by Raman spectroscopy has been carried out. Indeed, the successful reductive methylation of the BP lattice using sodium intercalation compounds and exhibiting different functionalization degrees has been demonstrated by 31P‐magic angle spinning (MAS) NMR spectroscopy. Furthermore, the correlation of 31P‐MAS NMR spectroscopy and statistical Raman spectroscopy (SRS) revealed the first method to determine the functionalization degree of BP solely by evaluating the intensities of distinct peaks in the Raman spectra of the covalently modified material, in a similar way to the widely employed ID/IG ratio of graphene research. The covalent functionalization of black phosphorus intercalation compounds (BPICs) with iodomethane has been developed. Starting from BPICs with different amounts of alkali metal the methylation can be achieved in varying functionalization degrees, which can be determined directly by Raman spectroscopy.
ISSN:1433-7851
1521-3773
DOI:10.1002/anie.202008646