Comparative STEM and FEGSTEM analysis of grain boundaries in steels

Faulkner, R. G.; Little, E. A.; Adetunji, G.J.

doi:10.1016/1044-5803(90)90022-c

Cited by 6 publications

(4 citation statements)

References 15 publications

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“…A similar STEM method was applied in the EELS analysis of the grain boundary impurities in Si 3 N 4 (Gu et al ., 1998a,b). Many other microanalyses of interfaces in various compounds were also carried out based on similar strategies using a dedicated STEM (Doig & Flewitt, 1978, 1982; Baumann & Williams, 1981; Michael & Williams, 1987; Faulkner et al ., 1990; Michael et al ., 1990; Williams et al ., 1992; Westwood et al ., 1992; Alber et al ., 1997; Keast & Williams, 2000). In a different approach, Michael and Williams studied Bi segregation in Cu grain boundaries using spot EDS (Michael & Williams, 1984).…”

Section: Introductionmentioning

confidence: 85%

“…The beam–specimen interaction volume is determined by d, D and t. Beam spreading can be calculated using Monte Carlo electron trajectory simulations (Faulkner & Norgaard, 1978; Kyser, 1979; Newbury & Myklebust, 1980; Newbury, 1981), or multiple scattering calculation (transport equation theory) (Rez, 1983). However, the single‐scattering approximation proposed by Goldstein (1979) and refined by Reed (1982) has been frequently adopted as sufficient (Doig & Flewitt, 1978; Faulkner et al ., 1990; Williams et al ., 1992; Watanabe & Williams, 1999; Keast & Williams, 2000). The experimental measurements of the spatial resolution using the single‐scattering model agreed well with the Monte Carlo simulations (Williams et al ., 1992).…”

Section: Theoretical Treatmentmentioning

confidence: 99%

“…Quantitative EDS and EELS have been used widely (Doig & Flewitt, 1982; Michael & Williams, 1984; Bonnell et al ., 1986; Faulkner et al ., 1990; Ikeda et al ., 1993; Chiang et al ., 1994; Clark et al ., 1981; Alber et al ., 1997; Gu et al ., 1998a; Keast & Williams, 2000). One of the typical applications is determining grain boundary impurity contents in polycrystalline ceramics.…”

Section: Introductionmentioning

confidence: 99%

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Energy dispersive spectroscopy analysis of aluminium segregation in silicon carbide grain boundaries

Zhang

Yang

Jonghe

et al. 2002

Journal of Microscopy

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SummaryThe aluminium distribution in polycrystalline SiC hot-pressed with aluminium, boron and carbon additives was studied using X-ray energy-dispersive spectroscopy (EDS) and transmission electron microscopy (TEM). The Al excess in homophase SiC grain boundary films was determined, taking into account dissolved Al in the SiC lattice. In the spot-EDS analysis, an electron beam probe with a calibrated diameter was formed, and the total beam-specimen interaction volume was defined, taking the beam spreading through crystalline TEM foil into consideration. EDS spectra were collected from regions containing intergranular films and adjacent matrix grains, respectively. A theoretical treatment was presented and experimental errors were estimated, with a further discussion about the effects of foil thickness. Experimental examples are given, followed by statistical EDS analyses for grain boundary films in SiC samples hot-pressed with increased amounts of Al additions. The results demonstrated a substantial Al segregation in the nanometer-wide intergranular films in all samples. Al additions higher than 3 wt% saturated the Al concentrations in SiC grains and in grain boundary films. The effect of foil thickness, and the parameters for determining the optimum incident beam diameter in the EDS analysis are discussed.

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Section: Introductionmentioning

confidence: 85%

Section: Theoretical Treatmentmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Energy dispersive spectroscopy analysis of aluminium segregation in silicon carbide grain boundaries

Zhang

Yang

Jonghe

et al. 2002

Journal of Microscopy

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“…There is no real rule for choosing the points giving I 1 and I 2 % of the maximum intensity ( I max ). It depends on the authors and the material, but these approximations make it possible to obtain a rapid, easy, and generally satisfactory evaluation of the interface resolution (Kirschner, 1977; Faulkner et al, 1990). According to Michael & Williams (1987), the FWTM, which is given by the horizontal distance between the 2 and 98% levels on the traverse output curve, can be used to define the lateral resolution.…”

Section: Introductionmentioning

confidence: 99%

Interfacial Energy-Dispersive Spectroscopy Profile X-Ray Resolution Measurements in Variable Pressure SEM

Zoukel

Khouchaf

Martino³

et al. 2014

Microsc Microanal

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A procedure has been developed to follow degradation of energy-dispersive spectroscopy (EDS) X-ray lateral resolution in a variable pressure scanning electron microscope. This procedure is based on evaluation of the EDS profile shape change for different experimental conditions. Some parameters affecting the X-ray resolution in high-vacuum mode have been taken into account. Good agreement between the simulated and experimental EDS profiles shows the reliability of the proposed procedure. A significant improvement in measurement of the EDS profile interfacial distance (DINT) has been achieved.

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Analytical electron microscopy of thin segregated layers

1994

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Analytical convolution methods used to explain the interaction of a fine electron beam with a thin segregated layer in a typical electron microscope specimen are described. Expressions are derived which quantify the shape of the measured concentration profile determined in the microscope by scanning the beam acrass the segregated layer. The expression contains parameters concerned with the beam profile and the thickness of the segregated layer. The method is applied to grain boundary segregation studies of neutron-irradiated femticmartensitic steels. S P CrNi MO v Nb Wt.% Balance 0.10 0.38 1.01 0.016 0.006 10.65 0.64 0.64 0.16 0.30

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Comparative STEM and FEGSTEM analysis of grain boundaries in steels

Cited by 6 publications

References 15 publications

Energy dispersive spectroscopy analysis of aluminium segregation in silicon carbide grain boundaries

Energy dispersive spectroscopy analysis of aluminium segregation in silicon carbide grain boundaries

Interfacial Energy-Dispersive Spectroscopy Profile X-Ray Resolution Measurements in Variable Pressure SEM

Analytical electron microscopy of thin segregated layers

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