Kossel and pseudo Kossel CCD pattern in comparison with electron backscattering diffraction diagrams

Däbritz, S.; Langer, Enrico; Hauffe, W.

doi:10.1016/s0169-4332(01)00260-4

Cited by 16 publications

(12 citation statements)

References 11 publications

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“…4096 gray values, one can find more about the specifications in [12]) with two-stage Peltier cooling (-12 • C) in a self-designed and developed EBSD system [13,14] was used for observation. Accelerating voltages up to 40 kV could be adjusted using the SEM CamScan CS44 with LaB 6 cathode.…”

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Investigation of HOLZ rings in EBSD patterns

Langer

Däbritz

2007

Phys. Status Solidi (c)

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PACS 61.14. Lj, 61.66.Bi Higher-Order Laue Zone (HOLZ) rings and their appearance in Electron Backscattered Diffraction (EBSD) pattern from molybdenum were fundamentally investigated in the Scanning Electron Microscope. HOLZ rings of the type 100 , 110 , 111 , 113 and 133 could be unambiguous detected in EBSD pattern of different pure Mo crystals. The [100] HOLZ ring was observed more in detail in dependence on the accelerating energy in the pattern center, and the lattice spacing was determined for all energies. A relatively good accuracy could be obtained for Mo as model sample for problematical high atomic number materials.1 Introduction Electron Backscattered Diffraction (EBSD) is a method to determine crystallographic parameter in the micro and nano range of bulk specimens in the Scanning Electron Microscope (SEM). The main applications are the automatic mapping of the crystal orientation of polycrystalline specimens with known crystal structures, an overview is given e.g. in Ref. [1,2], and the study of interfaces, especially grain boundaries [3,4]. It is also possible to distinguish between different previously selected crystallographic phases, see for example [5,6]. A further advantage is the high lateral resolution of up to 6 nm, which, in this case, could be achieved for a thin platinum film deposited on silicon [7].However, the accuracy in the lattice parameter determination obtained by measuring the width of Kikuchi bands is generally very low and at best only about 5% in dependence on the Kikuchi reflections used, sometimes only 10% [8]. Here, an improvement can allow the exploitation of the so-called HigherOrder Laue Zone (HOLZ) rings. The great advantage of the HOLZ rings are the sharp edges and that their diameter is sensitively dependent on the interplanar spacing perpendicular to the zone axis belonging to it. Conventionally, these HOLZ rings were observed in Kossel-Möllenstedt patterns at convergent beam electron diffraction (CBED) [9] in the Transmission Electron Microscopy (TEM). In some cases HOLZ rings can be observed also in EBSD patterns, but they are not as high in contrast as those in the TEM. HOLZ rings in EBSD patterns have not been sufficiently investigated so far. Baba-Kishi suggested to use HOLZ rings for the measurement of lattice constants, and he recorded a First-Order Laue Zone (FOLZ) ring on film from a marcasite crystal (FeS 2 , orthorhombic) [8]. In Ref.[10] it was shown on GaN thin films that HOLZ rings become more clearly visible by cooling the samples. There is only one paper by Michael and Eades [11] which deals with an evaluation of HOLZ rings. In this contribution, reciprocal lattice layer spacings were measured by means of observed HOLZ rings from different crystal systems using a CCD-based camera system. For compounds with a lower average ordinal number in some cases a good agreement between measured and calculated interplanar crystal spacings could be obtained. However, for higher atomic number materials like Mo, Ta and W the difference between measured and calc...

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Investigation of HOLZ rings in EBSD patterns

Langer

Däbritz

2007

Phys. Status Solidi (c)

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“…Electron backscattering depends on the thickness of the scattering material, and thus differs between the centre and edge of the object. Moreover, Monte Carlo simulation shows that electron backscattering also depends on the location depth and the size of Au particles (Däbritz, Langer & Hauffe, 2001). Therefore, the beam broadening affects both the particle size and shape measurement.…”

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Visualization and characterization of engineered nanoparticles in complex environmental and food matrices using atmospheric scanning electron microscopy

Luo

Morrison

Dudkiewicz

et al. 2013

Journal of Microscopy

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Summary Imaging and characterization of engineered nanoparticles (ENPs) in water, soils, sediment and food matrices is very important for research into the risks of ENPs to consumers and the environment. However, these analyses pose a significant challenge as most existing techniques require some form of sample manipulation prior to imaging and characterization, which can result in changes in the ENPs in a sample and in the introduction of analytical artefacts. This study therefore explored the application of a newly designed instrument, the atmospheric scanning electron microscope (ASEM), which allows the direct characterization of ENPs in liquid matrices and which therefore overcomes some of the limitations associated with existing imaging methods. ASEM was used to characterize the size distribution of a range of ENPs in a selection of environmental and food matrices, including supernatant of natural sediment, test medium used in ecotoxicology studies, bovine serum albumin and tomato soup under atmospheric conditions. The obtained imaging results were compared to results obtained using conventional imaging by transmission electron microscope (TEM) and SEM as well as to size distribution data derived from nanoparticle tracking analysis (NTA). ASEM analysis was found to be a complementary technique to existing methods that is able to visualize ENPs in complex liquid matrices and to provide ENP size information without extensive sample preparation. ASEM images can detect ENPs in liquids down to 30 nm and to a level of 1 mg L−1 (9×108 particles mL−1, 50 nm Au ENPs). The results indicate ASEM is a highly complementary method to existing approaches for analyzing ENPs in complex media and that its use will allow those studying to study ENP behavior in situ, something that is currently extremely challenging to do.

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“…In spite of the low line intensity/ background ratio no effort has been spared to accumulate the KOSSEL patterns by means of a CCD camera [13,14,15]. However, the X-ray film is still the best detector on account of the high lateral resolution (it corresponds to high angular resolution of the reflections).…”

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confidence: 99%