• Applied Microscopy
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• 제35권4호
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• pp.1-9
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• 2005

이 논문에서 Al-Cu-Mg 합금의 미세 석출 입자의 S-상 ($Al_2CuMg$) 결정구조에 대해 전자회절실험에 의한 포괄적인 연구 결과가 보고 되어 있다. 이 실험에는 한 S-상 입자를 포함하는 최소 영역의 일정 zone축의 회절패턴(SAED) 관찰과 이에 대응되는 운동학적 이론을 기초로 한 패턴의 시물레이션과의 비교 분석, 그리고 관측된 회절 패턴 필름으로부터 각 Bragg회절 점의 강도의 정량적 데이터 추출과 운동학적 및 동역학적 회절 강도 계산과의 비교 검토의 과정을 포함하고 있다. 이러한 연구의 한 결과 S-상의 결정구조는 일찍이 X-ray 방법으로부터 얻은 PW 모델결정(Perlitz and Westgren, 1943)과 일치함을 보여주고 있고, HREM 방법에 의해 새로이 구한 RaVel (Radmilovic et al., 1999) 모델과는 전혀 맞지않음이 판명되었다.

• 한국세라믹학회지
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• 제53권5호
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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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• 제33권3호
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• pp.187-193
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• 2003

투과식 전자현미경에서 상과 그 회절패턴은 현미경의 자기렌즈 작용에 의하여 상오 회전되어 나타난다. 이 회전각의 측정 결정은 결정 시료의 결함 관찰 분석에서 중요하다. 이 회전각 측정에 대해 잘 알려진 방법은 $MoO_3$의 분말 결정을 이용하는 것이다. 그러나 이 방법에는 측정된 각에 항상 $180^{\circ}$의 불확실성이 따른다. 따라서 이 불확실성을 제거하기 위한 또 다른 방안이 강구되어야 한다. 본 논문에서는 결정시료의 LACBED 패턴을 얻는 과정을 통해 간단하게 이 회전각을 측정하는 새로운 방법을 제시한다. 이 방법은 특정 결정을 필요로 하지 않는다. 이 방법을 통해 JEM 2010 TEM에서 상(image)과 그 회절패턴의 회전각은 $180^{\circ}$로 측정되었고, 이 각은 확대 배율이나 카메라 길이의 변화에도 변하지 않음이 관찰되었다.

• Carbon letters
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• 제21권
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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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• 제47권1호
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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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• 제1권1호
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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.

• 한국주조공학회지
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• 제15권5호
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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.

• 열처리공학회지
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• 제9권2호
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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.

• 한국재료학회지
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• 제10권7호
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• pp.478-481
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• 2000

$Pb(Mg_{1/3}Nb_{2/3})O_3$의 $Pb_{2+}$ 자리에 치환되어 전자주게 역할을 하는 $La^3,\; Pr^{3+,4+},\; Nd^{3+},\; Sm^{3+}$ 등이 10mol% 첨가된 단일상의 $Pb(Mg_{1/3}Nb_{2/3})O_3$ 소결체를 합성하여 이들의 B자리 양이온 질서배열구조를 XRD와 TEM을 이용하여 분석하였다. 전자 주게가 첨가되지 않았을 때에는 XRD패턴에서 공간군 Pm3m에 해당하는 기본 회절선(fundamental reflection) 만 검출되었으나 전자 주게가 첨가된 경우에는 $Mg_{2+}$와 $Nb_{5+}$의 1:1 질서배열로 인하여 단위포의 체적이 8배가 되어(h/2 k/2 l/2)(h,k,l 모두 홀수) 조격자 회절선(superlattice reflection)이 검출되었다. TEM 제한시야회절패턴(selected area diffraction pattern)에서는 전자 주게의 첨가 여부에 관계없이 초격자 회절점이 검출되었으나 전자 주게가 첨가된 경우에 기본 회절점에 대한 초격자 반사점의 상대적인 강도가 현저히 증가하였다. TEM 암시양상(dark field image)에서는 전자 주게가 첨가되었을 때에만 반상경계(antiphase boundary)가 관찰되었다. 이로부터 전자 주게인 $La^3,\; Pr^{3+,4+},\; Nd^{3+},\; Sm^{3+}$등이 $Pb_{2+}$를 치환함에 따라 $Pb(Mg_{1/3}Nb_{2/3})O_3$의 B자리 양이온 1:1 질서배열이 강화됨을 실험적으로 증명하였다. 얻어진 결과는 전하보상기구에 근거하여 해석하였다.

• 한국재료학회지
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• 제3권6호
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• pp.678-683
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• 1993

MBE법으로 $580^{\circ}C$에서 성장한 $GaAs_{0.5}Sb_{0.5}$/(001)GaAs 에피층의 원자 배열을 TEM을 이용하여 분석하였다. 1/2(111) 형의 장범위 규칙상이 $GaAs_{0.5}Sb_{0.5}$/(001)GaAs 에피층에서 발견되었다. 이 규칙상의 원자 배열은 As의 농도가 높은 {111}As 면과 Sb의 농도가 높은 {l1l}Sb 면이 V족 소격자에 교대로 나열된 구조이며, 주기는 {111} 면간 거리의 2배이다. 이 구조는 R3m 의 공간군에 속하며, 단위포는 능면체정이다.