Quantification of the boron speciation in alkali borosilicate glasses by electron energy loss spectroscopy

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Abstract

Transmission electron microscopy and related analytical techniques have been widely used to study the microstructure of different materials. However, few research works have been performed in the field of glasses, possibly due to the electron-beam irradiation damage. In this paper, we have developed a method based on electron energy loss spectroscopy (EELS) data acquisition and analyses, which enables determination of the boron speciation in a series of ternary alkali borosilicate glasses with constant molar ratios. A script for the fast acquisition of EELS has been designed, from which the fraction of BO ₄ tetrahedra can be obtained by fitting the experimental data with linear combinations of the reference spectra. The BO ₄ fractions (N ₄) obtained by EELS are consistent with those from ¹¹B MAS NMR spectra, suggesting that EELS can be an alternative and convenient way to determine the N ₄ fraction in glasses. In addition, the boron speciation of a CeO ₂ doped potassium borosilicate glass has been analyzed by using the time-resolved EELS spectra. The results clearly demonstrate that the BO ₄ to BO ₃ transformation induced by the electron beam irradiation can be efficiently suppressed by doping CeO ₂ to the borosilicate glasses.

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Topological principles of borosilicate glass chemistry.

Morten Smedskjaer, John Mauro, Randall E. Youngman … (2011)

Borosilicate glasses display a rich complexity of chemical behavior depending on the details of their composition and thermal history. Noted for their high chemical durability and thermal shock resistance, borosilicate glasses have found a variety of important uses from common household and laboratory glassware to high-tech applications such as liquid crystal displays. In this paper, we investigate the topological principles of borosilicate glass chemistry covering the extremes from pure borate to pure silicate end members. Based on NMR measurements, we present a two-state statistical mechanical model of boron speciation in which addition of network modifiers leads to a competition between the formation of nonbridging oxygen and the conversion of boron from trigonal to tetrahedral configuration. Using this model, we derive a detailed topological representation of alkali-alkaline earth-borosilicate glasses that enables the accurate prediction of properties such as glass transition temperature, liquid fragility, and hardness. The modeling approach enables an understanding of the microscopic mechanisms governing macroscopic properties. The implications of the glass topology are discussed in terms of both the temperature and thermal history dependence of the atomic bond constraints and the influence on relaxation behavior. We also observe a nonlinear evolution of the jump in isobaric heat capacity at the glass transition when substituting SiO(2) for B(2)O(3), which can be accurately predicted using a combined topological and thermodynamic modeling approach.

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Cerium and boron chemistry in doped borosilicate glasses examined by EELS

G. Yang, G Möbus, R.J. Hand (2006)

Spatially resolved measurements of boron coordination and cerium valency in a doped borosilicate glass with crystalline nano-precipitates are described. The fine structure of the boron K-edge and the white-line ratio of the cerium M-edge doublet were evaluated from EELS line scans. Due to high beam sensitivity it was found that reliable boron-coordination measurements in some of the glasses studied required extrapolation of results acquired after different periods of irradiation back to a zero-irradiation. However, borosilicates that contained heavy alkali atoms were found to suffer very little structural change. The Ce valency of a 4% (molar) doped alkali-borosilicate glass was found to be mixed +III/+IV in the glass matrix and purely +IV (indicative of CeO2) in the precipitates. A significant dependency of the valence results on the data processing method was found and explained.

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Software techniques for EELS to realize about 0.3 eV energy resolution using 300 kV FEG-TEM.

Y MATSUI, K Kimoto (2002)

In this short communication we describe some software techniques for electron energy-loss spectrum measurement. We prepared DigitalMicrograph (Gatan) scripts for multiple spectrum acquisitions, quasi-simultaneous acquisition of low-loss and core-loss spectra, energy drift correction, and other operations. Narrow zero-loss spread of 0.27 eV is demonstrated using a 300 kV field-emission transmission electron microscope (TEM) (Hitachi, HF-3000) and a post-column energy filter (Gatan, GIF2002). The core-loss spectrum is acquired with an energy resolution of 0.36 eV with high reproducibility. The present software techniques effectively achieve the intrinsic energy resolution of electron sources. Sample scripts are provided in the Appendix.

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Journal

Journal ID (nlm-ta): Sci Rep

Journal ID (iso-abbrev): Sci Rep

Title: Scientific Reports

Publisher: Nature Publishing Group

ISSN (Electronic): 2045-2322

Publication date (Electronic): 08 December 2015

Publication date Collection: 2015

Volume: 5

Electronic Location Identifier: 17526

Affiliations

[1 ]Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education & International Center for Dielectric Research, Xi’an Jiaotong University , Xi’an, 710049, China

[2 ]State Key Laboratory of Luminescent Materials and Devices, South China University of Technology , Guangzhou, 510640, China

[3 ]Department of Chemistry and Interdisciplinary Nanoscience Center (iNANO), Aarhus University , Aarhus, DK-8000, Denmark

[4 ]Section of Chemistry, Aalborg University , Aalborg, DK-9000, Denmark

[5 ]State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology , Wuhan, 430070, China

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[a ] g.yang@ 123456mail.xjtu.edu.cn

Article

Publisher Item ID: srep17526

DOI: 10.1038/srep17526

PMC ID: 4672332

PubMed ID: 26643370

SO-VID: 7fb08592-949b-4e99-8dd6-680ddf0a7756

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Quantification of the boron speciation in alkali borosilicate glasses by electron energy loss spectroscopy

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Most cited references 3

Topological principles of borosilicate glass chemistry.

Cerium and boron chemistry in doped borosilicate glasses examined by EELS

Software techniques for EELS to realize about 0.3 eV energy resolution using 300 kV FEG-TEM.

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