Nanostructural characterization of geopolymers by advanced beamline techniques

John L. Provis; Ailar Hajimohammadi; Claire E. White; Susan A. Bernal; Rupert J. Myers; Robert P. Winarski; Volker Rose; Thomas E. Proffen; Anna Llobet; Jannie S.J. Van Deventer

doi:10.1016/j.cemconcomp.2012.07.003

Nanostructural characterization of geopolymers by advanced beamline techniques

John L. Provis, Ailar Hajimohammadi, Claire E. White, Susan A. Bernal, Rupert J. Myers, Robert P. Winarski, Volker Rose, Thomas E. Proffen, Anna Llobet, Jannie S.J. Van Deventer

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Abstract

This paper presents the outcomes of a series of beamline-based studies, the results of which are combined to provide a more detailed multiscale understanding of the structure and chemistry of geopolymer binders. The range of beamline-based characterization techniques which have been applied to the study of geopolymer binders is increasing rapidly; although no single technique can provide a holistic view of binder structure across all the length scales which are of importance in determining strength development and durability, the synergy achievable through the combination of multiple beamline techniques is leading to rapid advances in knowledge in this area. Studies based around beamline infrared and X-ray fluorescence microscopy, in situ and ex situ neutron pair distribution function analysis, and nano- and micro-tomography, are combined to provide an understanding of geopolymer gel chemistry, nano- and microstructure in two and three dimensions, and the influences of seeded nucleation and precursor chemistry in these key areas. The application of advanced characterization methods in recent years has brought the understanding of geopolymer chemistry from a point, not more than a decade ago, when the analysis of the detailed chemistry of the aluminosilicate binder gel was considered intractable due to its disordered ("X-ray amorphous") nature, to the present day where the influence of key compositional parameters on nanostructure is well understood, and both gel structure and reaction kinetics can be manipulated through methods including seeding, temperature variation, and careful mix design. This paper therefore provides a review outlining the value of nanotechnology-and particularly nanostructural characterization-in the development and optimization of a new class of environmentally beneficial cements and concretes. Key engineering parameters, in particularly strength development and permeability, are determined at a nanostructural level, and so it is essential that gel structures can be analyzed and manipulated at this level; beamline-based characterization techniques are critical in providing the ability to achieve this goal.

Original language	English
Pages (from-to)	56-64
Number of pages	9
Journal	Cement and Concrete Composites
Volume	36
Issue number	1
DOIs	https://doi.org/10.1016/j.cemconcomp.2012.07.003
State	Published - Feb 2013

Funding

The program of work summarized in this paper has been funded through grants from the Australian Research Council, including some support via the Particulate Fluids Processing Centre, as well as through a Linkage Grant co-sponsored by Zeobond Pty Ltd. The infrared miscroscopy component of this research was undertaken on the IR beamline at the Australian Synchrotron, Victoria, Australia. This work has also benefited from the use of HIPD at the Lujan Center at Los Alamos Neutron Science Center, funded by the DOE Office of Basic Energy Sciences. The participation of CEW and AL in this work was supported by Los Alamos National Laboratory. Los Alamos National Laboratory is operated by Los Alamos National Security LLC under DOE Contract DE-AC52-06NA25396. CEW gratefully acknowledges the support of the U.S. Department of Energy through the LANL/LDRD Program. Use of the Advanced Photon Source and the Center for Nanoscale Materials was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357. Travel funding for experimental work was provided by the Brian Robinson Fellowship awarded to JLP, as well as through the Australian Synchrotron International Access Program, and through the Access to Major Research Facilities Program administered by ANSTO. The authors thank Dr. Hyunjeong Kim, Dr. Mark Tobin, Dr. Ljiljana Puskar and Dr. Katherine Page for assistance with experimental work.

Funders	Funder number
Zeobond Pty Ltd
U.S. Department of Energy	DE-AC52-06NA25396
Office of Science
Basic Energy Sciences	DE-AC02-06CH11357
Laboratory Directed Research and Development
Australian Nuclear Science and Technology Organisation
Los Alamos National Laboratory
Australian Research Council

Keywords

Alkali-activated binder
Geopolymer
Microstructure
Nanostructure
Neutron scattering
Synchrotron radiation

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title = "Nanostructural characterization of geopolymers by advanced beamline techniques",

abstract = "This paper presents the outcomes of a series of beamline-based studies, the results of which are combined to provide a more detailed multiscale understanding of the structure and chemistry of geopolymer binders. The range of beamline-based characterization techniques which have been applied to the study of geopolymer binders is increasing rapidly; although no single technique can provide a holistic view of binder structure across all the length scales which are of importance in determining strength development and durability, the synergy achievable through the combination of multiple beamline techniques is leading to rapid advances in knowledge in this area. Studies based around beamline infrared and X-ray fluorescence microscopy, in situ and ex situ neutron pair distribution function analysis, and nano- and micro-tomography, are combined to provide an understanding of geopolymer gel chemistry, nano- and microstructure in two and three dimensions, and the influences of seeded nucleation and precursor chemistry in these key areas. The application of advanced characterization methods in recent years has brought the understanding of geopolymer chemistry from a point, not more than a decade ago, when the analysis of the detailed chemistry of the aluminosilicate binder gel was considered intractable due to its disordered ({"}X-ray amorphous{"}) nature, to the present day where the influence of key compositional parameters on nanostructure is well understood, and both gel structure and reaction kinetics can be manipulated through methods including seeding, temperature variation, and careful mix design. This paper therefore provides a review outlining the value of nanotechnology-and particularly nanostructural characterization-in the development and optimization of a new class of environmentally beneficial cements and concretes. Key engineering parameters, in particularly strength development and permeability, are determined at a nanostructural level, and so it is essential that gel structures can be analyzed and manipulated at this level; beamline-based characterization techniques are critical in providing the ability to achieve this goal.",

keywords = "Alkali-activated binder, Geopolymer, Microstructure, Nanostructure, Neutron scattering, Synchrotron radiation",

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AU - Myers, Rupert J.

AU - Winarski, Robert P.

AU - Rose, Volker

AU - Proffen, Thomas E.

AU - Llobet, Anna

AU - Van Deventer, Jannie S.J.

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AB - This paper presents the outcomes of a series of beamline-based studies, the results of which are combined to provide a more detailed multiscale understanding of the structure and chemistry of geopolymer binders. The range of beamline-based characterization techniques which have been applied to the study of geopolymer binders is increasing rapidly; although no single technique can provide a holistic view of binder structure across all the length scales which are of importance in determining strength development and durability, the synergy achievable through the combination of multiple beamline techniques is leading to rapid advances in knowledge in this area. Studies based around beamline infrared and X-ray fluorescence microscopy, in situ and ex situ neutron pair distribution function analysis, and nano- and micro-tomography, are combined to provide an understanding of geopolymer gel chemistry, nano- and microstructure in two and three dimensions, and the influences of seeded nucleation and precursor chemistry in these key areas. The application of advanced characterization methods in recent years has brought the understanding of geopolymer chemistry from a point, not more than a decade ago, when the analysis of the detailed chemistry of the aluminosilicate binder gel was considered intractable due to its disordered ("X-ray amorphous") nature, to the present day where the influence of key compositional parameters on nanostructure is well understood, and both gel structure and reaction kinetics can be manipulated through methods including seeding, temperature variation, and careful mix design. This paper therefore provides a review outlining the value of nanotechnology-and particularly nanostructural characterization-in the development and optimization of a new class of environmentally beneficial cements and concretes. Key engineering parameters, in particularly strength development and permeability, are determined at a nanostructural level, and so it is essential that gel structures can be analyzed and manipulated at this level; beamline-based characterization techniques are critical in providing the ability to achieve this goal.

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Nanostructural characterization of geopolymers by advanced beamline techniques

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