Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>

Liquid phase exfoliation (LPE) is widely used to produce colloidal dispersions of nanomaterials, in particular two-dimensional nanosheets. The degree of exfoliation, i.e., the length to thickness aspect ratio was shown to be intrinsically limited by the ratio of in-plane to out-of-plane binding stre...

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Main Authors: Steffen Ott, Melanie Lakmann, Claudia Backes
Format: Article
Language:English
Published: MDPI AG 2021-04-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/11/5/1072
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spelling doaj-88e7affab8b942f88cc7e07c20b96d802021-04-22T23:00:42ZengMDPI AGNanomaterials2079-49912021-04-01111072107210.3390/nano11051072Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>Steffen Ott0Melanie Lakmann1Claudia Backes2Applied Physical Chemistry, Institute for Physical Chemistry, Faculty of Chemistry and Earth Sciences, Heidelberg University, Im Neuenheimer Feld 253, 69120 Heidelberg, GermanyApplied Physical Chemistry, Institute for Physical Chemistry, Faculty of Chemistry and Earth Sciences, Heidelberg University, Im Neuenheimer Feld 253, 69120 Heidelberg, GermanyApplied Physical Chemistry, Institute for Physical Chemistry, Faculty of Chemistry and Earth Sciences, Heidelberg University, Im Neuenheimer Feld 253, 69120 Heidelberg, GermanyLiquid phase exfoliation (LPE) is widely used to produce colloidal dispersions of nanomaterials, in particular two-dimensional nanosheets. The degree of exfoliation, i.e., the length to thickness aspect ratio was shown to be intrinsically limited by the ratio of in-plane to out-of-plane binding strength. In this work, we investigate whether simple pretreatment of the starting material can be used to change the in-plane to out-of-plane binding strength through mild intercalation to improve the sample quality in sonication-assisted LPE. Five different pretreatment conditions of WS<sub>2</sub> were tested and the dispersions size-selected through centrifugation. From optical spectroscopy (extinction, Raman, photoluminescence), information on nanosheet dimension (average lateral size, layer number, monolayer size) and optical quality (relative photoluminescence quantum yield) was extracted. We find that the pretreatment has a minor impact on the length/thickness aspect ratio, but that photoluminescence quantum yield can be increased in particular using mild sonication conditions. We attribute this to the successful exfoliation of nanosheets with a lower degree of basal plane defectiveness. This work emphasizes the complexity of the exfoliation process and suggests that the role of defects has to be considered for a comprehensive picture.https://www.mdpi.com/2079-4991/11/5/1072liquid phase exfoliation2D materialsoptical propertiesintercalation
collection DOAJ
language English
format Article
sources DOAJ
author Steffen Ott
Melanie Lakmann
Claudia Backes
spellingShingle Steffen Ott
Melanie Lakmann
Claudia Backes
Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>
Nanomaterials
liquid phase exfoliation
2D materials
optical properties
intercalation
author_facet Steffen Ott
Melanie Lakmann
Claudia Backes
author_sort Steffen Ott
title Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>
title_short Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>
title_full Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>
title_fullStr Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>
title_full_unstemmed Impact of Pretreatment of the Bulk Starting Material on the Efficiency of Liquid Phase Exfoliation of WS<sub>2</sub>
title_sort impact of pretreatment of the bulk starting material on the efficiency of liquid phase exfoliation of ws<sub>2</sub>
publisher MDPI AG
series Nanomaterials
issn 2079-4991
publishDate 2021-04-01
description Liquid phase exfoliation (LPE) is widely used to produce colloidal dispersions of nanomaterials, in particular two-dimensional nanosheets. The degree of exfoliation, i.e., the length to thickness aspect ratio was shown to be intrinsically limited by the ratio of in-plane to out-of-plane binding strength. In this work, we investigate whether simple pretreatment of the starting material can be used to change the in-plane to out-of-plane binding strength through mild intercalation to improve the sample quality in sonication-assisted LPE. Five different pretreatment conditions of WS<sub>2</sub> were tested and the dispersions size-selected through centrifugation. From optical spectroscopy (extinction, Raman, photoluminescence), information on nanosheet dimension (average lateral size, layer number, monolayer size) and optical quality (relative photoluminescence quantum yield) was extracted. We find that the pretreatment has a minor impact on the length/thickness aspect ratio, but that photoluminescence quantum yield can be increased in particular using mild sonication conditions. We attribute this to the successful exfoliation of nanosheets with a lower degree of basal plane defectiveness. This work emphasizes the complexity of the exfoliation process and suggests that the role of defects has to be considered for a comprehensive picture.
topic liquid phase exfoliation
2D materials
optical properties
intercalation
url https://www.mdpi.com/2079-4991/11/5/1072
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