Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy

There is a practical need, especially from the industrial community, to accurately measure the size and shape of graphene oxide (GO) flakes of commercial origin, in a reliable, simple, and unambiguous way. The sample preparation is a decisive step to obtain a homogeneous distribution of flakes on a...

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Main Authors: Giovanni Chemello, Konstantinos Despotelis, Keith R Paton, Charles A Clifford, Andrew J Pollard, Jörg Radnik, Vasile-Dan Hodoroaba
Format: Article
Language:English
Published: IOP Publishing 2025-01-01
Series:Nano Express
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Online Access:https://doi.org/10.1088/2632-959X/adae28
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author Giovanni Chemello
Konstantinos Despotelis
Keith R Paton
Charles A Clifford
Andrew J Pollard
Jörg Radnik
Vasile-Dan Hodoroaba
author_facet Giovanni Chemello
Konstantinos Despotelis
Keith R Paton
Charles A Clifford
Andrew J Pollard
Jörg Radnik
Vasile-Dan Hodoroaba
author_sort Giovanni Chemello
collection DOAJ
description There is a practical need, especially from the industrial community, to accurately measure the size and shape of graphene oxide (GO) flakes of commercial origin, in a reliable, simple, and unambiguous way. The sample preparation is a decisive step to obtain a homogeneous distribution of flakes on a substrate, which is suitable for image analysis. A certain level of inhomogeneity was still found but could be accepted for the purpose of this lateral size measurement study. A measurement procedure for Scanning Electron Microscopy (SEM) including sample preparation, measurement, image analysis and reporting was developed and validated to be applied for the lateral size analysis of ‘real-world’ 2D flakes. Samples were produced for analysis by drop casting GO dispersions onto Si/SiO _2 substrates. After SEM imaging, the images were analysed using two approaches to derive size and shape parameters. The influence of different operators has been evaluated. A maximum difference of 10% for the size descriptor and 2% for shape descriptor was found for both image analysis approaches when different samples of the same source material are measured and analysed by the same operator, hence indicating variability caused by sample preparation and analysing different sample areas. When different laboratories/operators perform the image analysis on exactly the same images and same flakes, the deviation found for the size descriptor is 2% and 4.6% corresponding to the two approaches applied, while no difference in the shape descriptor is observed.
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spelling doaj-art-acac9c0e5cb240beb597409072f233c92025-02-05T13:38:45ZengIOP PublishingNano Express2632-959X2025-01-016101500610.1088/2632-959X/adae28Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopyGiovanni Chemello0Konstantinos Despotelis1https://orcid.org/0000-0002-2490-7868Keith R Paton2https://orcid.org/0000-0003-0300-8676Charles A Clifford3https://orcid.org/0000-0003-4270-6856Andrew J Pollard4https://orcid.org/0000-0002-6841-2592Jörg Radnik5https://orcid.org/0000-0003-0302-6815Vasile-Dan Hodoroaba6https://orcid.org/0000-0002-7901-6114Federal Institute for Materials Research and Testing (BAM) , Unter den Eichen 44-46, 12203 Berlin, GermanyNational Physical Laboratory (NPL), Hampton Road, Teddington, TW11 0LW, United KingdomNational Physical Laboratory (NPL), Hampton Road, Teddington, TW11 0LW, United KingdomNational Physical Laboratory (NPL), Hampton Road, Teddington, TW11 0LW, United KingdomNational Physical Laboratory (NPL), Hampton Road, Teddington, TW11 0LW, United KingdomFederal Institute for Materials Research and Testing (BAM) , Unter den Eichen 44-46, 12203 Berlin, GermanyFederal Institute for Materials Research and Testing (BAM) , Unter den Eichen 44-46, 12203 Berlin, GermanyThere is a practical need, especially from the industrial community, to accurately measure the size and shape of graphene oxide (GO) flakes of commercial origin, in a reliable, simple, and unambiguous way. The sample preparation is a decisive step to obtain a homogeneous distribution of flakes on a substrate, which is suitable for image analysis. A certain level of inhomogeneity was still found but could be accepted for the purpose of this lateral size measurement study. A measurement procedure for Scanning Electron Microscopy (SEM) including sample preparation, measurement, image analysis and reporting was developed and validated to be applied for the lateral size analysis of ‘real-world’ 2D flakes. Samples were produced for analysis by drop casting GO dispersions onto Si/SiO _2 substrates. After SEM imaging, the images were analysed using two approaches to derive size and shape parameters. The influence of different operators has been evaluated. A maximum difference of 10% for the size descriptor and 2% for shape descriptor was found for both image analysis approaches when different samples of the same source material are measured and analysed by the same operator, hence indicating variability caused by sample preparation and analysing different sample areas. When different laboratories/operators perform the image analysis on exactly the same images and same flakes, the deviation found for the size descriptor is 2% and 4.6% corresponding to the two approaches applied, while no difference in the shape descriptor is observed.https://doi.org/10.1088/2632-959X/adae28graphene oxideSEMlateral dimensionstandardizationimaging
spellingShingle Giovanni Chemello
Konstantinos Despotelis
Keith R Paton
Charles A Clifford
Andrew J Pollard
Jörg Radnik
Vasile-Dan Hodoroaba
Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
Nano Express
graphene oxide
SEM
lateral dimension
standardization
imaging
title Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
title_full Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
title_fullStr Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
title_full_unstemmed Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
title_short Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
title_sort approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy
topic graphene oxide
SEM
lateral dimension
standardization
imaging
url https://doi.org/10.1088/2632-959X/adae28
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