Identification of functional groups and determination of carboxyl formation temperature in graphene oxide using the XPS O 1s spectrum

Experimental information on the O 1s spectra of GO by X-ray photoelectron spectrometry is limited and this will prove to be a liability when analyzing samples that have high carbon to oxygen ratios. Here, the binding energy (B.E.) information of electrons from the O 1s orbital of oxygen atoms in dif...

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Published inThin solid films Vol. 590; pp. 40 - 48
Main Authors Kwan, Yue Chau Garen, Ng, Ging Meng, Huan, Cheng Hon Alfred
Format Journal Article
LanguageEnglish
Published Elsevier B.V 01.09.2015
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Abstract Experimental information on the O 1s spectra of GO by X-ray photoelectron spectrometry is limited and this will prove to be a liability when analyzing samples that have high carbon to oxygen ratios. Here, the binding energy (B.E.) information of electrons from the O 1s orbital of oxygen atoms in different functional groups were identified by characterizing GO in an in-situ heating and characterization experiment, performed in a vacuum between 473 and 573K, and chemically modified GO. The B.E.s of the O 1s electrons in hydroxyls, epoxides, carbonyls and carboxyls on GO were determined and carboxyl formation on GO was found to occur between 543 and 561K. Here, carboxyl formation is a decrease in the proportion of oxygen atoms bound to GO as hydroxyls and epoxides groups, accompanied by a greater than proportional increase in the proportion of oxygen atoms bound as carboxyls, and this results in the formation of vacancies on the graphene basal plane. •Identification of functional groups in graphene oxide from O 1s spectra•Identification of carboxylation temperature regime in graphene oxide•Verification of the functional groups by chemical modification of GO
AbstractList Experimental information on the O 1s spectra of GO by X-ray photoelectron spectrometry is limited and this will prove to be a liability when analyzing samples that have high carbon to oxygen ratios. Here, the binding energy (B.E.) information of electrons from the O 1s orbital of oxygen atoms in different functional groups were identified by characterizing GO in an in-situ heating and characterization experiment, performed in a vacuum between 473 and 573K, and chemically modified GO. The B.E.s of the O 1s electrons in hydroxyls, epoxides, carbonyls and carboxyls on GO were determined and carboxyl formation on GO was found to occur between 543 and 561K. Here, carboxyl formation is a decrease in the proportion of oxygen atoms bound to GO as hydroxyls and epoxides groups, accompanied by a greater than proportional increase in the proportion of oxygen atoms bound as carboxyls, and this results in the formation of vacancies on the graphene basal plane.
Experimental information on the O 1s spectra of GO by X-ray photoelectron spectrometry is limited and this will prove to be a liability when analyzing samples that have high carbon to oxygen ratios. Here, the binding energy (B.E.) information of electrons from the O 1s orbital of oxygen atoms in different functional groups were identified by characterizing GO in an in-situ heating and characterization experiment, performed in a vacuum between 473 and 573K, and chemically modified GO. The B.E.s of the O 1s electrons in hydroxyls, epoxides, carbonyls and carboxyls on GO were determined and carboxyl formation on GO was found to occur between 543 and 561K. Here, carboxyl formation is a decrease in the proportion of oxygen atoms bound to GO as hydroxyls and epoxides groups, accompanied by a greater than proportional increase in the proportion of oxygen atoms bound as carboxyls, and this results in the formation of vacancies on the graphene basal plane. •Identification of functional groups in graphene oxide from O 1s spectra•Identification of carboxylation temperature regime in graphene oxide•Verification of the functional groups by chemical modification of GO
Author Ng, Ging Meng
Kwan, Yue Chau Garen
Huan, Cheng Hon Alfred
Author_xml – sequence: 1
  givenname: Yue Chau Garen
  orcidid: 0000-0002-9546-3053
  surname: Kwan
  fullname: Kwan, Yue Chau Garen
  email: kwanyuechau@gmail.com
  organization: Division of Physics and Applied Physics, School of Physical and Mathematical Sciences, Nanyang Technological University, 21 Nanyang Link, Singapore 637371, Singapore
– sequence: 2
  givenname: Ging Meng
  surname: Ng
  fullname: Ng, Ging Meng
  email: gingmeng.ng@sg.bosch.com
  organization: Research and Technology Center 1 (Asia Pacific), Corporate Research, Robert Bosch (SEA) Pte Ltd, 11 Bishan Street 21, Singapore 573943, Singapore
– sequence: 3
  givenname: Cheng Hon Alfred
  surname: Huan
  fullname: Huan, Cheng Hon Alfred
  email: alfred@ntu.edu.sg
  organization: Division of Physics and Applied Physics, School of Physical and Mathematical Sciences, Nanyang Technological University, 21 Nanyang Link, Singapore 637371, Singapore
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Tue Jul 01 00:50:55 EDT 2025
Thu Apr 24 22:56:52 EDT 2025
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IsPeerReviewed true
IsScholarly true
Keywords Carboxylation on graphene oxide
Graphene oxide
Functional group identification
Thermal annealing
X-ray photoelectron spectroscopy
O 1s spectra of graphene oxide
Language English
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  year: 2015
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Snippet Experimental information on the O 1s spectra of GO by X-ray photoelectron spectrometry is limited and this will prove to be a liability when analyzing samples...
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SubjectTerms Carbon
Carboxylation on graphene oxide
Formations
Functional group identification
Functional groups
Graphene
Graphene oxide
Heating
O 1s spectra of graphene oxide
Orbitals
Oxygen atoms
Thermal annealing
X-ray photoelectron spectroscopy
Title Identification of functional groups and determination of carboxyl formation temperature in graphene oxide using the XPS O 1s spectrum
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