• 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).

• Journal of the Korean Ceramic Society
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• v.53 no.5
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• pp.568-573
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• 2016

We explore the crystalline structure and phase transition of lithium thiophosphate ($Li_7P_3S_{11}$) solid electrolyte using electron microscopy and X-ray diffraction. The glass-like $Li_7P_3S_{11}$ powder is prepared by the high-energy mechanical milling process. According to the energy dispersive X-ray spectroscopy (EDS) and selected area diffraction (SAD) analysis, the glass powder shows chemical homogeneity without noticeable contrast variation at any specific spot in the specimen and amorphous SAD ring patterns. Upon heating up to $260^{\circ}C$ the glass $Li_7P_3S_{11}$ powder becomes crystallized, clearly representing crystal plane diffraction contrast in the high-resolution transmission electron microscopy image. We further confirm that each diffraction spot precisely corresponds to the diffraction from a particular $Li_7P_3S_{11}$ crystallographic structure, which is also in good agreement with the previous X-ray diffraction results. We expect that the microscopic analysis with EDS and SAD patterns would permit a new approach to study in the atomic scale of other lithium ion conducting sulfides.

• Applied Microscopy
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• v.33 no.3
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• pp.187-193
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• 2003

When electron microscope images and selected area diffraction patterns of crystalline materials are being compared, it is important to know for the rotation of the diffraction pattern with respect to the image caused by the magnetic lens in the Electron Microscope. A well-known method to determine this rotation is to use a test crystal of $MoO_3$. But this method of determination of the rotation angle contains an uncertainty of $180^{\circ}$. Thus one has to devise another way to eliminate this uncertainty. In this paper we present a new and simple method of determining this rotation without any complexity. The method involves a process of obtaining LACBED patterns of crystalline materials. For the J2010 electron microscope, the rotation is determined to be $180^{\circ}$ and this angle remains unchanged for changing of the magnification and the camera length.

• Carbon letters
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• v.21
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• pp.33-50
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• 2017

In this study, Fe-Ni bimetallic catalyst supported on kaolin is prepared by a wet impregnation method. The effects of mass of kaolin support, pre-calcination time, pre-calcination temperature and stirring speed on catalyst yields are examined. Then, the optimal supported Fe-Ni catalyst is utilised to produce multi-walled carbon nanotubes (MWCNTs) using catalytic chemical vapour deposition (CCVD) method. The catalysts and MWCNTs prepared using the optimal conditions are characterized using high resolution transmission electron microscope (HRTEM), high-resolution scanning electron microscope (HRSEM), electron diffraction spectrometer (EDS), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and X-ray diffraction (XRD). The XRD/EDS patterns of the prepared catalyst confirm the formation of a purely crystalline ternary oxide ($NiFe_2O_4$). The statistical analysis of the variance demonstrates that the combined effects of the reaction temperature and acetylene flow rate predominantly influenced the MWCNT yield. The $N_2$ adsorption (BET) and TGA analyses reveal high surface areas and thermally stable MWCNTs. The HRTEM/HRSEM micrographs confirm the formation of tangled MWCNTs with a particle size of less than 62 nm. The XRD patterns of the MWCNTs reveal the formation of a typical graphitized carbon. This study establishes the production of MWCNTs from a bi-metallic catalyst supported on kaolin.

• Applied Microscopy
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• v.47 no.1
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• pp.50-54
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• 2017

The microstructure, the crystallization behavior, and magnetic properties of FeSi-based soft magnetic alloys (FINEMET) were investigated using transmission electron microscopy, X-ray diffraction, and coercive force measurements. The amorphous $Fe_{73.28}Si_{13.43}B_{8.72}Cu_{0.94}Nb_{3.63}$ alloys particles, prepared in $10^{-4}$ torr by gas atomization process, were heat treated at $530^{\circ}C$, $600^{\circ}C$, and $670^{\circ}C$ for 1 hour in a vacuum of $10^{-2}$ torr. Nanocrystalline Fe precipitation was first formed followed by the grain growth. Phase formation and crystallite sizes was compared linked to its magnetic behavior, which showed that excellent soft magnetic property can directly be correlated with its microstructure.

• Rapid Communication in Photoscience
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• v.1 no.1
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• pp.13-15
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• 2012

New porous $TiO_2$ nanostructures with shapes of pearl and rice were synthesized by hydrothermal treatment of $TiO_2$-liposome nanocomposites in acid and base solutions, respectively, as identified by scanning electron microscopy (SEM), transmission electron microscopy (TEM) images and large Brunauer-Emmett-Teller (BET) surface areas. The x-ray diffraction (XRD) patterns and selected area electron diffraction proved them to be well-defined anatase crystals. Their UV-visible reflectance absorption spectra were observed to have low band gap energy (3.03 and 3.07 eV, respectively), exhibiting surface absorption band in the visible range from 400 to 600 nm. The degradation of methylene blue (MB) over the $TiO_2$ nanostructures was observed upon visible-light irradiation, which was found to be very efficient as compared with any other conventional visible-light responsive $TiO_2$ nanostructures.

• Journal of Korea Foundry Society
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• v.15 no.5
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• pp.514-522
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• 1995

The microstructural evolution with isothermal stirring during semi-solid state processing of hypoeutectic Al-6.2wt%Si alloy was studied. Substructure of the individual primary solid particle in the slurry was investigated through transmission electron microscopy(TEM). Formation of subgrain boundaries on the rheocast Al-6.2wt%Si alloy is observed and the misorientation between the grains is shown typically under 2 degrees by analyzing selected area diffraction (SAD) and convergent beam electron diffraction (CBED) patterns. The existence of high angle grain boundaries are also observed in the alloy. Based upon these observations, mechanisms for the primary particles fragmentation are considered. With isothermal stirring, the dislocation density increases, and the evolution of dislocation cell structure takes place, which is interpreted as a process of achieving uniform deformation by dynamic recovery under applied shear stress.

• Journal of the Korean Society for Heat Treatment
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• v.9 no.2
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• pp.91-102
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• 1996

Microstructural control to produce multiphase structure has received much attention to improve the high temperature strength as well as low temperature ductility of intermetallics. Transmission electron microscopic investigation has been carried out concerning the effect of Cr-precipitation on the mechanical properties of B2-ordered NiAl containing 4 to 8 mol% of Cr. By aging at temperatures around 973 K after solution annealing, fine spherical precipitates took place homogeneously in the NiAl matrix and the alloys hardened appreciably. Selected area electron diffraction (SAED) patterns have not revealed any additional extra-spots during aging, because the Cr-particles show cube-cube orientation relationship and keep a perfect coherency with the ordered matrix lattice. Dislocations were confirmed to bypass the particles during deformation. Although the dispersion of Cr-particles increased the yield strength of NiAl at intermediate temperature, the strength decreased appreciably at higher temperatures.

• Korean Journal of Materials Research
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• v.10 no.7
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• pp.478-481
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• 2000

Single phase $Pb(Mg_{1/3}Nb_{2/3})O_3$ ceramics doped by 10 mol% of electron donors such as $La^3,\; Pr^{3+,4+},\; Nd^{3+},\; Sm^{3+}$, were synthesized and their B-site cationic ordering structures were investigated by XRD and TEM. In the XRD patterns, only fundamental reflections were observed for the undoped $Pb(Mg_{1/3}Nb_{2/3})O_3$, while the (h/2 $\textsc{k}$/2ι/2)(h,$\textsc{k}$,ι all odd) superlattice reflections resulting from the 1:1 ordering induced unit cell doubling were also observed for the donor-doped $Pb(Mg_{1/3}Nb_{2/3})O_3$. In the TEM selected area diffraction patterns, the (h/2 k/2 l/2)(h,k,l all odd) superlattice reflection spots as well as the fundamental reflection spots were observed for all the samples, but the relative intensities of the superlattice reflection spots to the fundamental reflection spots were significantly enhanced by the donor-doping. In the TEM dark-field images, antiphase boundaries were observed only for the donor-doped $Pb(Mg_{1/3}Nb_{2/3})O_3$. It was therefore experimentally verified that doping by electron donors such as $La^3,\; Pr^{3+,4+},\; Nd^{3+},\; Sm^{3+}$, enhances the B-site cationic 1:1 ordering in $Pb(Mg_{1/3}Nb_{2/3})O_3$. These experimental results were interpreted in terms of the charge compensation mechanism.

• Korean Journal of Materials Research
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• v.3 no.6
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• pp.678-683
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• 1993

Atomic arral1gement of ordered phase in $GaAs_{0.5}Sb_{0.5}$ epilayer was studied by observation of selected area diffraction patterns and high resolution images. The epilayer was grown on untilted (001) GaAs substrate at $580^{\circ}C$ by molecular beam epitaxy(MBE). A 1/2(111) type long-range ordered phase is formed in the epilayer. Atomic arrangement of the ordered phase is described as an alternative stacking of As-rich and Sb-rich {111} planes in group V sublattice. Space group of the ordred structure belongs to R3m, and unit cell of the ordered structure is rhombohedral.