Surface functional groups and degree of carbonization of selected chars from different processes and feedstock.

The knowledge of the structural and chemical properties of biochars is decisive for their application as technical products. For this reason, methods for the characterization of biochars that are generally applicable and allow quality control are highly desired. Several methods that have shown potential in other studies were used to investigate two activated carbons and seven biochars from different processes and feedstock. The chars were chosen to cover a wide range of chemical composition and structural properties as a hardness test for the analytical methods used in this study. Specific problems connected with the pretreatment of samples and drawbacks of some methods for some types of chars could be identified in an integrated consideration of the results from different methods. None of the spectroscopic methods was found to be suitable for the quality control of all types of chars. The most valuable results were obtained by chemical analysis that, however, required the complete determination of the main elements, including that of oxygen, and of inorganic components for adequate results. The combination of X-ray photoelectron spectroscopy (XPS) and FT-IR spectroscopy allows a rough characterization of surface functional groups, but cannot discriminate aliphatic and aromatic OH groups. FT-IR might be a suitable method for the quality control of biochars made at lower temperature. The results of Raman spectroscopy did not well correlate with the amount of sp2 hybridized carbon determined by XPS. A better correlation of XPS data was found with the electrical polarization determined by the method of spectral induced polarization that was used for the first time in conjunction with extensive analytical characterization.

Polymorphism in micro-, submicro-, and nanocrystalline NaNbO3.

NaNbO(3) powders with various particle sizes (ranging from 30 nm to several microns) and well-controlled stoichiometry were obtained through microemulsion-mediated synthesis. The effect of particle size on the phase transformation of the prepared NaNbO(3) powders was studied using X-ray powder diffraction, Raman spectroscopy, and nuclear site group analysis based on these spectroscopic data. Coarsened particles exhibit an orthorhombic Pbcm (D(2h)(11), no. 57) structure corresponding to the bulk structure, as observed for single crystals or powders prepared by conventional solid-state reaction. The crystal symmetry of submicron powders was refined with the space group Pmc2(1) (C(2v)(2), no. 26). The reduced perovskite cell volumes of these submicron powders were most expanded compared to all the other structures. Fine particles with a diameter of less than 70 nm as measured from SEM observations showed an orthorhombic Pmma (D(2h)(5), no. 51) crystal symmetry. The perovskite formula cell of this structure was pseudocubic and was the most compact one. A possible mechanism of the phase transformation is suggested.