Analysis of the Chemical Distribution of Self-Assembled Microdomains with the Selective Localization of Amine-Functionalized Graphene Nanoplatelets by Optical Photothermal Infrared Microspectroscopy

Suihua He; Pascaline Bouzy; Nicholas Stone; Carwyn Ward; Ian Hamerton

doi:10.1021/acs.analchem.2c02306

Analysis of the Chemical Distribution of Self-Assembled Microdomains with the Selective Localization of Amine-Functionalized Graphene Nanoplatelets by Optical Photothermal Infrared Microspectroscopy

Suihua He, Pascaline Bouzy, Nicholas Stone, Carwyn Ward, Ian Hamerton^*

^*Corresponding author for this work

Research output: Contribution to journal › Article (Academic Journal) › peer-review

4 Citations (Scopus)

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Abstract

By incorporating 1-(2-aminoethyl)piperazine (AEPIP) into a commercial epoxy blend, a bi-continuous microstructure is produced with selective localization of amine-functionalized graphene nanoplatelets (A-GNPs). This cured blend underwent self-assembly, and the morphology and topology were observed via spectral imaging techniques. As the selective localization of nanofillers in thermoset blends is rarely achieved, and the mechanism remains largely unknown, the optical photothermal infrared (O-PTIR) spectroscopy technique was employed to identify the compositions of microdomains. The A-GNP tends to be located in the region containing higher concentrations of both secondary amine and secondary alcohol; additionally, the phase morphology was found to be influenced by the amine concentration. With the addition of AEPIP, the size of the graphene domains becomes smaller and secondary phase separation is detected within the graphene domain evidenced by the chemical contrast shown in the high-resolution chemical map. The corresponding chemical mapping clearly shows that this phenomenon was mainly induced by the chemical contrast in related regions. The findings reported here provide new insight into a complicated, self-assembled nanofiller domain formed in a multi-component epoxy blend, demonstrating the potential of O-PTIR as a powerful and useful approach for assessing the mechanism of selectively locating nanofillers in the phase structure of complex thermoset systems.

Original language	English
Article number	2c02306
Pages (from-to)	11848-11855
Number of pages	8
Journal	Analytical Chemistry
Volume	94
Issue number	34
Early online date	16 Aug 2022
DOIs	https://doi.org/10.1021/acs.analchem.2c02306
Publication status	Published - 30 Aug 2022

Bibliographical note

Funding Information:
S.H. was supported through the China Scholarship Council/University of Bristol (CSC-UOB) Joint Research Scholarship and wishes to thank the Faculty of Engineering Research Pump Priming Fund (UOB). The authors are very grateful to Dr. Mustafa Kansiz of Photothermal Spectroscopy Corporation, Santa Barbara, CA 93101, USA, who carried out some of the O-PTIR data contained in this manuscript, undertook data analysis, and participated in very productive discussions. S.H., C.W., and I.H. would like to acknowledge the support of the Henry Royce Institute through the Royce PhD Equipment Access Scheme, enabling access to imaging and characterization facilities at Royce@Sheffield, EPSRC Grant Number EP/R00661X/1. S.H., C.W., and I.H. also wish to thank Dr. Germinal Margo and Dr. Annela Seddon for access to the spin coater and useful discussions.

Funding Information:
S.H. was supported through the China Scholarship Council/University of Bristol (CSC-UOB) Joint Research Scholarship and wishes to thank the Faculty of Engineering Research Pump Priming Fund (UOB). The authors are very grateful to Dr. Mustafa Kansiz of Photothermal Spectroscopy Corporation, Santa Barbara, CA 93101, USA, who carried out some of the O-PTIR data contained in this manuscript, undertook data analysis and participated in very productive discussions. S.H., C.W., and I.H. would like to acknowledge the support of the Henry Royce Institute through the Royce PhD Equipment Access Scheme, enabling access to imaging and characterization facilities at Royce@Sheffield, EPSRC Grant Number EP/R00661X/1. S.H., C.W., and I.H. also wish to thank Dr. Germinal Margo and Dr. Annela Seddon for access to the spin coater and useful discussions.

Publisher Copyright:
© 2022 American Chemical Society. All rights reserved.

Keywords

Epoxy resin
Nanomaterials
Self Assembly
Optical Photothermal Infrared Microspectroscopy
Graphene nanoplatelets

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Investigating the phase morphology and distribution of different nanofillers within the reaction induced phase separated structure of an epoxy blend
He, S. (Author), Hamerton, I. (Supervisor) & Ward, C. (Supervisor), 21 Mar 2023
Student thesis: Doctoral Thesis › Doctor of Philosophy (PhD)

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title = "Analysis of the Chemical Distribution of Self-Assembled Microdomains with the Selective Localization of Amine-Functionalized Graphene Nanoplatelets by Optical Photothermal Infrared Microspectroscopy",

abstract = "By incorporating 1-(2-aminoethyl)piperazine (AEPIP) into a commercial epoxy blend, a bi-continuous microstructure is produced with selective localization of amine-functionalized graphene nanoplatelets (A-GNPs). This cured blend underwent self-assembly, and the morphology and topology were observed via spectral imaging techniques. As the selective localization of nanofillers in thermoset blends is rarely achieved, and the mechanism remains largely unknown, the optical photothermal infrared (O-PTIR) spectroscopy technique was employed to identify the compositions of microdomains. The A-GNP tends to be located in the region containing higher concentrations of both secondary amine and secondary alcohol; additionally, the phase morphology was found to be influenced by the amine concentration. With the addition of AEPIP, the size of the graphene domains becomes smaller and secondary phase separation is detected within the graphene domain evidenced by the chemical contrast shown in the high-resolution chemical map. The corresponding chemical mapping clearly shows that this phenomenon was mainly induced by the chemical contrast in related regions. The findings reported here provide new insight into a complicated, self-assembled nanofiller domain formed in a multi-component epoxy blend, demonstrating the potential of O-PTIR as a powerful and useful approach for assessing the mechanism of selectively locating nanofillers in the phase structure of complex thermoset systems.",

keywords = "Epoxy resin, Nanomaterials, Self Assembly, Optical Photothermal Infrared Microspectroscopy, Graphene nanoplatelets",

author = "Suihua He and Pascaline Bouzy and Nicholas Stone and Carwyn Ward and Ian Hamerton",

note = "Funding Information: S.H. was supported through the China Scholarship Council/University of Bristol (CSC-UOB) Joint Research Scholarship and wishes to thank the Faculty of Engineering Research Pump Priming Fund (UOB). The authors are very grateful to Dr. Mustafa Kansiz of Photothermal Spectroscopy Corporation, Santa Barbara, CA 93101, USA, who carried out some of the O-PTIR data contained in this manuscript, undertook data analysis, and participated in very productive discussions. S.H., C.W., and I.H. would like to acknowledge the support of the Henry Royce Institute through the Royce PhD Equipment Access Scheme, enabling access to imaging and characterization facilities at Royce@Sheffield, EPSRC Grant Number EP/R00661X/1. S.H., C.W., and I.H. also wish to thank Dr. Germinal Margo and Dr. Annela Seddon for access to the spin coater and useful discussions. Funding Information: S.H. was supported through the China Scholarship Council/University of Bristol (CSC-UOB) Joint Research Scholarship and wishes to thank the Faculty of Engineering Research Pump Priming Fund (UOB). The authors are very grateful to Dr. Mustafa Kansiz of Photothermal Spectroscopy Corporation, Santa Barbara, CA 93101, USA, who carried out some of the O-PTIR data contained in this manuscript, undertook data analysis and participated in very productive discussions. S.H., C.W., and I.H. would like to acknowledge the support of the Henry Royce Institute through the Royce PhD Equipment Access Scheme, enabling access to imaging and characterization facilities at Royce@Sheffield, EPSRC Grant Number EP/R00661X/1. S.H., C.W., and I.H. also wish to thank Dr. Germinal Margo and Dr. Annela Seddon for access to the spin coater and useful discussions. Publisher Copyright: {\textcopyright} 2022 American Chemical Society. All rights reserved.",

year = "2022",

month = aug,

day = "30",

doi = "10.1021/acs.analchem.2c02306",

language = "English",

volume = "94",

pages = "11848--11855",

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Analysis of the Chemical Distribution of Self-Assembled Microdomains with the Selective Localization of Amine-Functionalized Graphene Nanoplatelets by Optical Photothermal Infrared Microspectroscopy. / He, Suihua; Bouzy, Pascaline; Stone, Nicholas et al.
In: Analytical Chemistry, Vol. 94, No. 34, 2c02306, 30.08.2022, p. 11848-11855.

Research output: Contribution to journal › Article (Academic Journal) › peer-review

TY - JOUR

T1 - Analysis of the Chemical Distribution of Self-Assembled Microdomains with the Selective Localization of Amine-Functionalized Graphene Nanoplatelets by Optical Photothermal Infrared Microspectroscopy

AU - He, Suihua

AU - Bouzy, Pascaline

AU - Stone, Nicholas

AU - Ward, Carwyn

AU - Hamerton, Ian

N1 - Funding Information: S.H. was supported through the China Scholarship Council/University of Bristol (CSC-UOB) Joint Research Scholarship and wishes to thank the Faculty of Engineering Research Pump Priming Fund (UOB). The authors are very grateful to Dr. Mustafa Kansiz of Photothermal Spectroscopy Corporation, Santa Barbara, CA 93101, USA, who carried out some of the O-PTIR data contained in this manuscript, undertook data analysis, and participated in very productive discussions. S.H., C.W., and I.H. would like to acknowledge the support of the Henry Royce Institute through the Royce PhD Equipment Access Scheme, enabling access to imaging and characterization facilities at Royce@Sheffield, EPSRC Grant Number EP/R00661X/1. S.H., C.W., and I.H. also wish to thank Dr. Germinal Margo and Dr. Annela Seddon for access to the spin coater and useful discussions. Funding Information: S.H. was supported through the China Scholarship Council/University of Bristol (CSC-UOB) Joint Research Scholarship and wishes to thank the Faculty of Engineering Research Pump Priming Fund (UOB). The authors are very grateful to Dr. Mustafa Kansiz of Photothermal Spectroscopy Corporation, Santa Barbara, CA 93101, USA, who carried out some of the O-PTIR data contained in this manuscript, undertook data analysis and participated in very productive discussions. S.H., C.W., and I.H. would like to acknowledge the support of the Henry Royce Institute through the Royce PhD Equipment Access Scheme, enabling access to imaging and characterization facilities at Royce@Sheffield, EPSRC Grant Number EP/R00661X/1. S.H., C.W., and I.H. also wish to thank Dr. Germinal Margo and Dr. Annela Seddon for access to the spin coater and useful discussions. Publisher Copyright: © 2022 American Chemical Society. All rights reserved.

PY - 2022/8/30

Y1 - 2022/8/30

N2 - By incorporating 1-(2-aminoethyl)piperazine (AEPIP) into a commercial epoxy blend, a bi-continuous microstructure is produced with selective localization of amine-functionalized graphene nanoplatelets (A-GNPs). This cured blend underwent self-assembly, and the morphology and topology were observed via spectral imaging techniques. As the selective localization of nanofillers in thermoset blends is rarely achieved, and the mechanism remains largely unknown, the optical photothermal infrared (O-PTIR) spectroscopy technique was employed to identify the compositions of microdomains. The A-GNP tends to be located in the region containing higher concentrations of both secondary amine and secondary alcohol; additionally, the phase morphology was found to be influenced by the amine concentration. With the addition of AEPIP, the size of the graphene domains becomes smaller and secondary phase separation is detected within the graphene domain evidenced by the chemical contrast shown in the high-resolution chemical map. The corresponding chemical mapping clearly shows that this phenomenon was mainly induced by the chemical contrast in related regions. The findings reported here provide new insight into a complicated, self-assembled nanofiller domain formed in a multi-component epoxy blend, demonstrating the potential of O-PTIR as a powerful and useful approach for assessing the mechanism of selectively locating nanofillers in the phase structure of complex thermoset systems.

AB - By incorporating 1-(2-aminoethyl)piperazine (AEPIP) into a commercial epoxy blend, a bi-continuous microstructure is produced with selective localization of amine-functionalized graphene nanoplatelets (A-GNPs). This cured blend underwent self-assembly, and the morphology and topology were observed via spectral imaging techniques. As the selective localization of nanofillers in thermoset blends is rarely achieved, and the mechanism remains largely unknown, the optical photothermal infrared (O-PTIR) spectroscopy technique was employed to identify the compositions of microdomains. The A-GNP tends to be located in the region containing higher concentrations of both secondary amine and secondary alcohol; additionally, the phase morphology was found to be influenced by the amine concentration. With the addition of AEPIP, the size of the graphene domains becomes smaller and secondary phase separation is detected within the graphene domain evidenced by the chemical contrast shown in the high-resolution chemical map. The corresponding chemical mapping clearly shows that this phenomenon was mainly induced by the chemical contrast in related regions. The findings reported here provide new insight into a complicated, self-assembled nanofiller domain formed in a multi-component epoxy blend, demonstrating the potential of O-PTIR as a powerful and useful approach for assessing the mechanism of selectively locating nanofillers in the phase structure of complex thermoset systems.

KW - Epoxy resin

KW - Nanomaterials

KW - Self Assembly

KW - Optical Photothermal Infrared Microspectroscopy

KW - Graphene nanoplatelets

U2 - 10.1021/acs.analchem.2c02306

DO - 10.1021/acs.analchem.2c02306

M3 - Article (Academic Journal)

C2 - 35972471

SN - 0003-2700

VL - 94

SP - 11848

EP - 11855

JO - Analytical Chemistry

JF - Analytical Chemistry

IS - 34

M1 - 2c02306

ER -

Analysis of the Chemical Distribution of Self-Assembled Microdomains with the Selective Localization of Amine-Functionalized Graphene Nanoplatelets by Optical Photothermal Infrared Microspectroscopy

Abstract

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Keywords

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Investigating the phase morphology and distribution of different nanofillers within the reaction induced phase separated structure of an epoxy blend

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