High-angle triple-axis specimen holder for three-dimensional diffraction contrast imaging in transmission electron microscopy

Hata, Satoshi; Miyazaki, Hiroya; Miyazaki, Shinsuke; Mitsuhara, Masatoshi; Tanaka, Masaki; Kaneko, Kenji; Higashida, Kenji; Ikeda, Ken; Nakashima, Hideharu; Matsumura, Shuichi; Barnard, J. S.; Sharp, J. H.; Midgley, Paul A.

doi:10.1016/j.ultramic.2011.03.021

Cited by 67 publications

(27 citation statements)

References 23 publications

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“…The holder allows a specimen to be tilted in a range of 680 about the longitudinal axis with tilting capability up to 67 about the orthogonal axis. 25 For electron tomography, tilt series of images were acquired using high-angle annular dark field (HAADF) STEM over a tilt range of À65 to þ65 with a tilt increment of 2 . The inner detector angle used was 57 mrad.…”

Section: Methodsmentioning

confidence: 99%

Direct observation of doping incorporation pathways in self-catalytic GaMnAs nanowires

Kasama

Thuvander

Siusys

et al. 2015

Journal of Applied Physics

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Publication date: 2015 Document VersionPublisher's PDF, also known as Version of record Link back to DTU Orbit Citation (APA): Kasama, T., Thuvander, M., Siusys, A., Gontard, L. C., Kovács, A., Yazdi, S., ... Sadowski, J. (2015) Doping mechanisms of Mn in GaAs nanowires (NWs) that have been grown self-catalytically at 600 C by molecular beam epitaxy (MBE) are investigated using advanced electron microscopy techniques and atom probe tomography. Mn is found to be incorporated primarily in the form of non-magnetic tetragonal Ga 0.82 Mn 0.18 nanocrystals in Ga catalyst droplets at the ends of the NWs, while trace amounts of Mn (22 6 4 at. ppm) are also distributed randomly in the NW bodies without forming clusters or precipitates. The nanocrystals are likely to form after switching off the reaction in the MBE chamber, since they are partially embedded in neck regions of the NWs. The Ga 0.82 Mn 0.18 nanocrystals and the low Mn concentration in the NW bodies are insufficient to induce a ferromagnetic phase transition, suggesting that it is difficult to have high Mn contents in GaAs even in 1-D NW growth via the vapor-liquid-solid process. V C 2015 AIP Publishing LLC.

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Section: Methodsmentioning

confidence: 99%

Direct observation of doping incorporation pathways in self-catalytic GaMnAs nanowires

Kasama

Thuvander

Siusys

et al. 2015

Journal of Applied Physics

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“…The contribution of dislocations to the electrical resistance is smaller than that of the grain size, 12) which may make it difficult to accurately determine the dislocation density of fine-grained materials, in which the grain boundary density is high. TEM observations require the preparation of thin-film samples, during which the dislocation density can be reduced near the surface, 14) permitting only local measurement of dislocation densities. In addition, surface effects may be induced that change the dislocation source activity and behavior relative to those of the bulk material.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of Dislocation Density for 1100 Aluminum with Different Grain Size during Tensile Deformation by Using <i>In-Situ</i> X-ray Diffraction Technique

et al. 2015

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Ultra-fine-grained (UFG) aluminum with a grain size of 260 nm was fabricated by annealing a severely plastically deformed A1100 alloy. The resulting UFG aluminum exhibited a 0.2% proof stress (· 0.2 ) that was four times larger than that predicted by the conventional Hall-Petch relation. In this study, the UFG aluminum, the fine-grained aluminum with a grain size of 960 nm and the coarse-grained aluminum with a grain size of 4.47 µm were prepared. The change in the dislocation density, μ was investigated during tensile deformation using in-situ X-ray diffraction measurements at SPring-8. It was found that as the strain increased, the μ changed in four distinct stages. The first stage was characterized by elastic deformation, and little change in the μ occurred. For the coarse-grained aluminum, this stage was almost absent. In the second stage, the μ rapidly increased until the stress reaches ·II in which the plastic deformation begins to occur at a constant strain rate. In the third stage, only a moderate change in the μ occurred. Finally, in the fourth stage, the μ rapidly decreased as the test pieces underwent fracture. Additionally, it was found that the · 0.2 -· I was followed by the conventional Hall-Petch relation in all grain size range.

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“…After the tilt-series dataset acquisition, a 3D representation of the object is reconstructed and visualized using an algorithm such as the back-projection method. Recent advancements in ET technique enable a variety of 3D observations, such as 3D atomic arrangements and nanoparticle morphology, [1][2][3] morphology and spatial distribution of precipitates, [4][5][6] and dislocations [7][8][9][10] in crystalline materials.…”

Section: An Experimental Protocol Development Of Three-dimensional Trmentioning

confidence: 99%

“…3. In the tilt-series dataset acquisition, a high-angle triple-axis specimen holder 10) was used to align a diffracted beam of g(hkl) = 110 α-Fe to the Bragg condition exactly on the specimen tilt axis. As a result, the ADF-STEM tilt-series images visualize both dislocations and carbides precipitated at the martensite lath boundaries.…”

Section: Optimum Conditions For Et Observation Of Precipi-mentioning

confidence: 99%

An Experimental Protocol Development of Three-Dimensional Transmission Electron Microscopy Methods for Ferrous Alloys: Towards Quantitative Microstructural Characterization in Three Dimensions

et al. 2015

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The majority of engineering steels are ferromagnetic and structurally inhomogeneous on scales ranging from nanometers to micrometers, and their physical properties depend on the three-dimensional (3D) features in their microstructures. Thus, obtaining a 3D image with a large field of view is desirable for transmission electron microscopy (TEM) based microstructure characterization in order to establish the relationship between the microstructure and the physical properties with a reasonable statistical relevancy. Here, we use a conventional sample preparation process, i.e., mechanical polishing followed by electropolishing, and optimizing experimental protocols for electron tomography (ET) of ferromagnetic materials, to carry out microstructural characterization of engineering steel. We determined that the sample thickness after the mechanical polishing step is a critical experimental parameter affecting the success rate of tilt-series image acquisitions. For example, for ferritic heat-resistant 9Cr steel, mechanical thinning down to 30 μm or less was necessary to acquire an adequate tilt-series image of the carbide precipitates in the annular dark-field scanning TEM (ADF-STEM) mode. However, acquiring tilt-series images of dislocation structures remains a challenge due to an unavoidable, significant electron beam deflection during specimen tilt, even with a thinned sample. To overcome the electron beam deflection problem, we evaluated several relatively accessible approaches including the "Low-Mag STEM and Lorentz TEM" modes. Although rarely used for ET, both modes reduce or even zero the objective lens current, likely weakening the magnetic interference between the ferromagnetic specimen and the objective lens magnetic field. The advantages and disadvantages of these experimental components are discussed.

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High-angle triple-axis specimen holder for three-dimensional diffraction contrast imaging in transmission electron microscopy

Cited by 67 publications

References 23 publications

Direct observation of doping incorporation pathways in self-catalytic GaMnAs nanowires

Direct observation of doping incorporation pathways in self-catalytic GaMnAs nanowires

Evaluation of Dislocation Density for 1100 Aluminum with Different Grain Size during Tensile Deformation by Using <i>In-Situ</i> X-ray Diffraction Technique

An Experimental Protocol Development of Three-Dimensional Transmission Electron Microscopy Methods for Ferrous Alloys: Towards Quantitative Microstructural Characterization in Three Dimensions

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