• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.183-187
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• 2009

The structure of nano-crystalline $MnFe_2O_4$ was determined and refined with electron powder diffraction data employing the Rietveld refinement technique. A nano-crystalline sample (with average crystal size of about 10.9 nm) was characterized by selected area electron diffraction in an energy-filtering transmission electron microscope operated at 120 kV. All reflection intensities were extracted from a digitized image plate using the program ELD and then used in the course of structure refinements employing the program FULLPROF for the Rietveld analysis. The final structure was refined in space group Fd-3m (# 227) with lattice parameters a=8.3413(7) $\AA$. The reliability factors of the refinement are $R_F$=7.98% and $R_B$=3.55%. Comparison of crystallographic data between electron powder diffraction data and reference data resulted in better agreement with ICSD-56121 rather than with ICSD-28517 which assumes an initial structure model.

• Applied Microscopy
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• v.41 no.1
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• pp.75-79
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• 2011

For quantitative analysis of nano-crystal structure, we reported the accuracy improvement method of lattice parameters measured from electron diffraction. For calculation of Au lattice parameters used as a standard crystal structure, it was considered two different acquisition methods (detector and enegy-filter) and three different calculation methods (conventional, least-square and regression fit). As a result, the measurement reliability could be enhanced by using CCD camera which gives higher performance, while energy-filtering did not affect the improvement the camera constant accuracy. Also, the accuracy of lattice parameters could be improved up to $10^{-4}$ order by regression fitting with correction formula. Finally, it is expected that the combination of regression fitting and intensity extraction from energy-filtered precession electron diffraction gives a solution of quantitative structure analysis for unknown nano-crystals.

• Applied Microscopy
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• v.47 no.4
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• pp.223-225
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• 2017

Cryo-electron microscopy (cryo-EM) is arguably the most powerful tool used in structural biology. It is an important analytical technique that is used for gaining insight into the functional and molecular mechanisms of biomolecules involved in several physiological processes. Cryo-EM can be separated into the following three groups according to the analytical purposes and the features of the biological samples: cryo-electron tomography (cryo-ET), cryo-single-particle reconstruction, and cryo-electron crystallography. Cryo-tomography is a unique EM technique that is used to study intact biomolecular complexes within their original environments; it can provide mechanistic insights that are challenging for other EM-methods. However, the resolution of reconstructed three-dimensional (3D) models generated by cryo-ET is relatively low, while single-particle reconstruction can reproduce biomolecular structures having near-atomic resolution without the need for crystallization unless the samples are large (>200 kDa) and highly symmetrical. Cryo-electron crystallography is subdivided into the following two categories according to the types of samples: one category that deals with two-dimensional (2D) crystalline arrays and the other category that uses 3D crystals. These two categories of electron-crystallographic techniques use different diffraction data obtained from still diffraction and continuous-rotation diffraction. In this paper, we review crystal-based cryo-EM techniques and focus on the recently developed 3D electron-crystallographic technique called microcrystal-electron diffraction.

• Applied Microscopy
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• v.45 no.3
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• pp.131-134
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• 2015

Here we show how by processing energy dispersive X-ray spectrometry (EDS) data obtained using highly sensitive, new generation EDS detectors in the AZtec LayerProbe software we can obtain data of sufficiently high quality to non-destructively measure the number of layers in two-dimensional (2D) $MoS_2$ and $MoS_2/WSe_2$ and thereby enable the characterization of working devices based on 2D materials. We compare the thickness measurements with EDS to results from atomic force microscopy measurements. We also show how we can use electron backscatter diffraction (EBSD) to address fabrication challenges of 2D materials. Results from EBSD analysis of individual flakes of exfoliated $MoS_2$ obtained using the Nordlys Nano detector are shown to aid a better understanding of the exfoliation process which is still widely used to produce 2D materials for research purposes.

• Applied Microscopy
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• v.33 no.3
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• pp.195-204
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• 2003

The Experimental calibration method has been investigated to correct d-spacing estimation and to identify phases in the electron diffraction data acquired by imaging plates. When the diffraction data from the imaging plate was corrected by the d-spacing calibration method with the radial intensity distribution plotting in this experiment, The accuracy of d-spacing estimation was significantly increased in errors of about 0.5%. The experimental calibration equation followed up the first order exponential decay function was derived from the trace of d-spacing deviation between the measured and the calculated values. It was applied to the analysis of d-spacing and the phase identification of the transitional phases formed from [001] gibbsite specimen by electron beam irradiation effect. In this case more accurate phase identification and d-spacing evaluation is possible for the transitional phases whose diffraction patterns are complicatedly superimposed. It is concluded that ${\chi}$-alumina, ${\gamma}$-alumina and ${\sigma}$-alumina are clearly identified as the major transitional phases formed from gibbsite by electron beam irradiation for 120 min.

• Applied Microscopy
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• v.35 no.4
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• pp.1-9
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• 2005

In this paper it is reported that a comprehensive study of the crystal structure of the fine size S-phase ($Al_2CuMg$) precipitate in Al-Cu-Mg alloy by electron diffraction experiments. The experiments involve taking the selected area diffraction pattern for a S-phase particle, simulations of the pattern based on the kinematical diffraction theory and quantitative data collection from the zone axis diffraction patterns for the comparison with calculated diffraction intensity using both the kinematical and the dynamical diffraction theory. As a result, a good fitting model of the S-phase structure turns out to be the model reported early by X-ray methods (Perlitz & Westgren, 1943), not the new model determined by HRTEM methods (Radmilovic et al., 1999).

• Applied Microscopy
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• v.45 no.4
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• pp.218-224
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• 2015

A technical overview on the various sample preparation methods for electron backscattered diffraction (EBSD) analysis is carried out. The mechanical polishing with colloidal silica finish, electro-chemical polishing, dual layer coating and ion beam milling are introduced for the common sample preparation methods for EBSD observation and some issues that are frequently neglected by the common EBSD users but should be considered to get a reliable EBSD data are discussed. This overview would be especially helpful to the people who know what EBSD technique is but do not get a reliable EBSD data because of difficulties in sample preparation.

• Journal of the Korean Chemical Society
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• v.48 no.4
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• pp.339-350
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• 2004

The simplified cumulant method was applied to diffraction data of $CClF_3$ to study the equilibrium molecular parameters over a range of temperatures. The molecular parameters of $CClF_3$ by the simplified cumulant method were compared with those from the traditional method. Also the instrumentation of picosecond time resolved electron diffraction (TRED) and the experimental details are described. The total experimental temporal resolution was discussed in terms of the electron pulse width. The TRED system was applied to study the molecular structures for $CClF_3$ at room temperature. The molecular structural parameters $CClF_3$ from TRED are compared with those from GED/RT. The molecular parameters ($r_e$)of bonded C-F and C-Cl for $CClF_3$ by simplified CA are 132.00(2) pm and 175.20(3) pm, respectively, by using GED/RT. From the results of TRED experiments $r_a$ for bonded C-F and C-Cl are 132.23(13) pm and 177.23(19) pm.

• Bulletin of the Korean Chemical Society
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• v.34 no.3
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• pp.788-792
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• 2013

A shortcoming of using transmission electron microscopy (TEM) for structural analysis via electron diffraction is the relatively large error of the measurements as compared to X-ray diffraction. To reduce these errors, various internal standard methods from earlier studies have been widely used. We developed a new device to facilitate the application of internal standard methods in preparation of TEM grids used for nanopowder analysis. Through the application of a partial mask on the TEM grid, both the internal standards and the research materials can be loaded on the same grid. Through this process, we conducted a TEM analysis that compared synthetic hydroxyapatite (HAp) nanopowder to bone apatite from a bovine femur. We determined that the accuracy of the d-spacing measurements of the HAp and bone powders could be improved to better than 1% after statistical treatments of the experimental data. By applying a quarter mask, we loaded four different nanoparticles on a single TEM grid, with one section designated for the internal standard.

• Bulletin of the Korean Chemical Society
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• v.33 no.2
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• pp.505-510
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• 2012

Cobalt oxide nanostructure materials have been prepared by adding several concentrations of spectator Ni ions in solution, and analyzed by electron microscopy, X-day diffraction, calorimetry/thermogravimetric analysis, UV-vis absorption, Raman, and X-ray photoelectron spectroscopy. The electron microscopy results show that the morphology of the nanostructures is dramatically altered by changing the concentration of spectator ions. The bulk XRD patterns of $350^{\circ}C$-annealed samples indicate that the structure of the cobalt oxide is all of cubic Fd-3m $Co_3O_4$, and show that the major XRD peaks shift slightly with the concentration of Ni ions. In Raman spectroscopy, we can confirm the XRD data through a more obvious change in peak position, broadness, and intensity. For the un-sputtered samples in the XPS measurement process, the XPS peaks of Co 2p and O 1s for the samples prepared without Ni ions exhibit higher binding energies than those for the sample prepared with Ni ions. Upon $Ar^+$ ion sputtering, we found $Co_3O_4$ reduces to CoO, on the basis of XPS data. Our study could be further applied to controlling morphology and surface oxidation state.