NDLI: X-ray photoelectron spectroscopic study on the goethites with variations in crystallinity and morphology: their effects on surface hydroxyl concentration

Content Provider	Springer Nature Link
Author	Echigo, Takuya Hatta, Tamao Nemoto, Seiko Takizawa, Shigeru
Copyright Year	2012
Abstract	We examined the effects of crystallinity and crystal morphology on surface hydroxyl concentration of goethite using four kinds of goethite samples prepared by aging a hydrous ferric oxide (ferrihydrite) at different temperatures ranging from 4 to 70 °C. These samples were analyzed with the following methods: powder X-ray diffraction, Brunauer–Emmett–Teller surface area analyzer, atomic force microscopy, attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and high-resolution X-ray photoelectron spectroscopy (XPS). The first three analyses showed that the goethite aged at lower temperature has lower crystallinity, smaller particle size and lower aspect ratio. The ATR-FTIR analysis revealed that the OH-stretching band of goethite aged at 4 °C moves to slightly higher wavenumber than those of the samples aged at higher temperatures. Their XPS analyses demonstrated that variation in the concentration of surface hydroxyl group ranges from 6.6 (nm−2) for the sample aged at 4 °C to 7.7 (nm−2) for the sample aged at 70 °C. Considering the analytical depth of the XPS (~5 nm), photoelectrons are emitted from the uppermost layers of the analyte. Hence, XPS results are interpreted to reflect variations in the morphology of fine crystals (<100 nm thick). The morphology of the present goethites can be characterized by their aspect ratio, in other words, the degree of development of (110)–(110) intersection edges at which protons preferentially accumulate. This variation in the concentration of surface hydroxyl group revealed by XPS analysis offers experimental evidence for the effects of crystallinity and morphology on the surface chemical properties of goethite.
Starting Page	769
Ending Page	778
Page Count	10
File Format	PDF
ISSN	03421791
Journal	Physics and Chemistry of Minerals
Volume Number	39
Issue Number	9
e-ISSN	14322021
Language	English
Publisher	Springer-Verlag
Publisher Date	2012-08-03
Publisher Place	Berlin, Heidelberg
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Goethite X-ray photoelectron spectroscopy Attenuated total reflectance-Fourier transform infrared spectroscopy Surface hydroxyl group Specific surface area Crystallinity Morphology Crystallography Mineralogy Mineral Resources Geochemistry
Content Type	Text
Resource Type	Article
Subject	Geochemistry and Petrology Materials Science

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