caa a22 4500 388021365 CHVBK 20180307124925.0 cr unu---uuuuu 161130e199802 xx s 000 0 eng 10.1557/JMR.1998.0050 doi S0884291400042874 pii (NATIONALLICENCE)cambridge-10.1557/JMR.1998.0050 Composition and chemical width of ultrathin amorphous films at grain boundaries in silicon nitride [Elektronische Daten] Two different electron energy loss spectroscopy (EELS) quantitative analytical methods for obtaining complete compositions from interface regions are applied to ultrathin oxide-based amorphous grain boundary (GB) films of ∼ 1 nm thickness in high-purity HIPed Si3N4 ceramics. The first method, 1, is a quantification of the segregation excess at interfaces for all the elements, including the bulk constituents such as silicon and nitrogen; this yields a GB film composition of SiN0.49±1.4O1.02±0.42 when combined with the average film thickness from high resolution electron microscopy (HREM). The second method, II, is based on an EELS near-edge structure (ELNES) analysis of the Si-L2,3 edge of thin GB films which permits a subtraction procedure that yields a completeEELS spectrum, e.g., that also includes the O-K and N-K edges, explicitly for the GB film. From analysis of these spectra, the film composition is directly obtained as SiN0.63±0.19O1.44±0.33, close to the one obtained by the first method but with much better statistical quality. The improved quality results from the fewer assumptions made in method II; while in method I uniform thickness and illumination condition have to beassumed, and correction of such effects yields an extra systematic error. Method II is convenient as it does not depend on the film thickness detected by HREM, nor suffer from material lost by preferential thinning at the GB. In addition, a chemical width for these films can be deduced as 1.33 ± 0.25 nm, that depends on an estimation of film density based on its composition. Such a chemical width is in good agreement with the structural thickness determined by HREM, with a small difference that is probably due to the different way in which these techniques probe the GB film. The GB film compositions are both nonstoichiometric, but in an opposite sense, this discrepancy is probably due to different ways of treating the surface oxidation layers in both methods. Copyright © Materials Research Society 1998 Gu H. Japan Science and Technology Corporation, "Ceramics Superplasticity” project, JFCC 2F, 2-4-1 Mutsuno, Atusta, Nagoya 456, Japan and Max-Planck-Institut für Metallforschung, Seestraβe 92, 70174, Stuttgart, Germany Cannon R. M. Lawrence Berkeley Laboratory, University of California, Berkeley, California 94720 Rühle M. Max-Planck-Institut für Metallforschung, Seestraβe 92, 70174, Stuttgart, Germany Journal of Materials Research Cambridge University Press 13/2(1998-02), 376-387 0884-2914 13:2<376 1998 13 JMR https://doi.org/10.1557/JMR.1998.0050 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1557/JMR.1998.0050 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Gu H. Japan Science and Technology Corporation, "Ceramics Superplasticity” project, JFCC 2F, 2-4-1 Mutsuno, Atusta, Nagoya 456, Japan and Max-Planck-Institut für Metallforschung, Seestraβe 92, 70174, Stuttgart, Germany NATIONALLICENCE 700 1- Cannon R. M. Lawrence Berkeley Laboratory, University of California, Berkeley, California 94720 NATIONALLICENCE 700 1- Rühle M. Max-Planck-Institut für Metallforschung, Seestraβe 92, 70174, Stuttgart, Germany NATIONALLICENCE 773 0- Journal of Materials Research Cambridge University Press 13/2(1998-02), 376-387 0884-2914 13:2<376 1998 13 JMR CC0 http://creativecommons.org/publicdomain/zero/1.0 nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-cambridge