• Title/Summary/Keyword: High Resolution TEM

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Comparison of the Kinetic Behaviors of Fe2O3 Spherical Submicron Clusters and Fe2O3 Fine Powder Catalysts for CO Oxidation

  • Yoo, Seung-Gyun;Kim, Jin-Hoon;Kim, Un-Ho;Jung, Jin-Seung;Lee, Sung-Han
    • Bulletin of the Korean Chemical Society
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    • v.35 no.5
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    • pp.1379-1384
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    • 2014
  • ${\alpha}-Fe_2O_3$ spherical particles having an average diameter of ca. 420 nm and ${\alpha}-Fe_2O_3$ fine particles (< 10 ${\mu}m$ particle size) were prepared to examine as catalysts for CO oxidation. Kinetic studies on the catalytic reactions were performed in a flow reactor using an on-line gas chromatography system operated at 1 atm. The apparent activation energies and the partial orders with respect to CO and $O_2$ were determined from the rates of CO disappearance in the reaction stage showing a constant catalytic activity. In the temperature range of $150-275^{\circ}C$, the apparent activation energies were calculated to be 13.7 kcal/mol on the ${\alpha}-Fe_2O_3$ spherical submicron clusters and 15.0 kcal/mol on the ${\alpha}-Fe_2O_3$ fine powder. The Pco and $Po_2$ dependencies of rate were investigated at various partial pressures of CO and $O_2$ at $250^{\circ}C$. Zero-order kinetics were observed for $O_2$ on both the catalysts, but the reaction order for CO was observed as first-order on the ${\alpha}-Fe_2O_3$ fine powder and 0.75-order on the ${\alpha}-Fe_2O_3$ spherical submicron clusters. The catalytic processes including the inhibition process by $CO_2$ on the ${\alpha}-Fe_2O_3$ spherical submicron powder are discussed according to the kinetic results. The catalysts were characterized using XRD (X-ray powder diffraction), FE-SEM (field emission-scanning electron microscopy), HR-TEM (high resolution-transmission electron microscopy), and $N_2$ sorption measurements.

Comparative study on the morphological properties of graphene nanoplatelets prepared by an oxidative and non-oxidative route

  • An, Jung-Chul;Lee, Eun Jung;Yoon, So-Young;Lee, Seong-Young;Kim, Yong-Jung
    • Carbon letters
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    • v.26
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    • pp.81-87
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    • 2018
  • Morphological differences in multi-layered graphene flakes or graphene nanoplatelets prepared by oxidative (rGO-NP, reduced graphene oxide-nanoplatelets) and non-oxidative (GIC-NP, graphite intercalation compound-nanoplatelets) routes were investigated with various analytical methods. Both types of NPs have similar specific surface areas but very different structural differences. Therefore, this study proposes an effective and simple method to identify structural differences in graphene-like allotropes. The adsorptive potential peaks of rGO-NP attained by the density functional theory method were found to be more scattered over the basal and non-basal regions than those of GIC-NP. Raman spectra and high resolution TEM images showed more distinctive crystallographic defects in the rGO-NP than in the GIC-NP. Because the R-ratio values of the edge and basal plane of the sample were maintained and relatively similar in the rGO-NP (0.944 for edge & 1.026 for basal), the discrepancy between those values in the GIC-NP were found to be much greater (0.918 for edge & 0.164 for basal). The electrical conductivity results showed a remarkable gap between the rGO-NP and GIC-NP attributed to their inherent morphological and crystallographic properties.

Effect of plasma oxidation time on TMR devices prepared by a ICP sputter (ICP 스퍼터를 이용한 TMR 소자 제작에서 절연막의 플라즈마 산화시간에 따른 미세구조 및 자기적 특성 변화)

  • Lee, Yeong-Min;Song, O-Seong
    • Korean Journal of Materials Research
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    • v.11 no.10
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    • pp.900-906
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    • 2001
  • We prepared tunnel magnetoresistance(TMR) devices of Ta($50\AA$)/NiFe($50\AA$)/IrMn(150$\AA$)/CoFe($50\AA$)/Al ($13\AA$)-O/CoFe($40\AA$)/NiFe($400\AA$)/Ta(50$\AA$) structure which has 100$\times$100 $\mu\textrm{m}^2$ junction area on $2.5\Times2.5 cm^{2}$ $Si/SiO_2$ ($1000\AA$) substrates by a inductively coupled plasma(ICP) magnetron sputter. We fabricated the insulating layer using a ICP plasma oxidation method by varying oxidation time from 80 sec to 360 sec, and measured resistances and magnetoresistance(MR) ratios of TMR devices. We used a high resolution transmission electron microscope(HRTEM) to investigate microstructural evolution of insulating layer. The average resistance of devices increased from 16.38 $\Omega$ to 1018 $\Omega$ while MR ratio decreased from 30.31 %(25.18 %) to 15.01 %(14.97 %) as oxidation time increased from 80 sec to 360 sec. The values in brackets are calculated values considering geometry effect. By comparing cross-sectional TEM images of 220 sec and 360 sec-oxidation time, we found that insulating layer of 360 sec-oxidized was 30 % and 40% greater than that of 150 sec-oxidized in thickness and thickness variation, respectively. Therefore, we assumed that increase of thickness variation with oxidation time is major reason of MR decrease. The resistance of 80 sec-oxidized specimen was 160 k$\Omega$$\mu\textrm{m}^2$ which is appropriate for industrial needs of magnetic random access memory(MRAM) application.

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Low-temperture Synthesis of CdTe/Te Core-shell Hetero-nanostructures by Vapor-solid Process

  • Song, Gwan-U;Kim, Tae-Hun;Bae, Ji-Hwan;Lee, Jae-Uk;Park, Min-Ho;Yang, Cheol-Ung
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.580-580
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    • 2012
  • Heterostructures has unique and important properties, which may be helpful for finding many potential applications in the field of electronic, thermoelectric, and optoelectronic devices. We synthesized CdTe/Te core-shell heterostructures by vapor-solid process at low temperatures using a quartz tube furnace. Two step vapor-solid processes were employed. First, various tellurium structures such as nanowires, nanorods, nanoneedles, microtubes and microrods were synthesized under various deposition conditions. These tellurium nanostructures were then used as substrates in the second step to synthesize the CdTe/Te core-shell heterostructures. Using this method, various sizes, shapes and types of CdTe/Te core-shell structures were fabricated under a range of conditions. These structures were analysed by scanning electron microscopy, high resolution transmission electron microscopy, and energy dispersive x-ray spectroscopy. The vapor phase process at low temperatures appears to be an efficient method for producing a variety of Cd/Te hetero-nanostructures. In addition, the hetero-nanostructures can be tailored to the needs of specific applications by deliberately controlling the synthetic parameters.

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Preparation of binder-free IrO2-RuO2/TiO2 nanotube electrode for DSA application. (DSA 활용을 위한 바인더를 사용하지 않은 IrO2-RuO2/TiO2 나노튜브 전극 제조)

  • Yu, Hyeon-Seok;Choe, Jin-Seop
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.28-28
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    • 2018
  • 수전해(electrochemical water splitting)는 연료전지의 가역적 역반응을 이용하여 물로부터 수소와 산소를 발생시키는 기술이다. 산소는 음극에서 발생하는데, 이 때 음극 표면은 고농도의 산소 음이온 및 라디칼에 장시간 노출된다. 때문에 기계적, 화학적 내구성이 우수한 전극재를 사용할 필요가 있다. 불용성 전극 (dimensionally stable anode, DSA)은 이러한 기술적 요구사항을 잘 만족하는 상용화 된 전극이다. 티타늄이나 티타늄 합금 표면에 촉매를 미량 반복 살포하여 산화물 형태의 매우 견고한 표면을 형성함으로서 내구성을 확보한다. 그러나, 보통 DSA 제조 기법의 특징에 따라 다공성 표면 구조를 사용하지는 않기 때문에 생산 과정이 복잡하고 비용이 많이 발생하는 문제를 여전히 나타내고 있다. 본 연구는 상기 문제를 개선하기 위한 수전해용 음극 제조 기술에 관한 연구이다. 티타늄과 티타늄 합금은 동일한 양극산화 기술 적용이 가능하다는 점을 이용하여 티타늄 기판으로부터 다공성 구조를 형성함으로써 바인더의 사용을 배제하였다. 단일공정양극산화기법 (single-step anodization)을 이용하여 $IrO_2$$RuO_2$를 도핑함으로써 TiO2에 촉매능을 부여하였다. 제조된 나노튜브들의 구조적 특징을 HR-TEM (High-resolution transmission electron microscope)과 FE-SEM (Field-emission scanning electron microscope)으로 분석하고 SAED (selective area electron diffraction) 패턴을 분석하여 전극재의 결정성을 확인하였다. 알칼라인 분위기에서 일으킨 산소발생반응 (oxygen evolution reaction, OER)의 LSV (linear sweep voltammetry) 결과를 XPS (X-ray photoelectron microscoscopy) 결과와 연관지어 촉매 표면 구조와 과전압의 관계를 해석하였다. LSV 결과로부터 Tafel 분석을 연달아 수행함으로써 전극의 속도결정단계를 정의하였다. 최종적으로 사이클 테스트 통하여 DSA로써의 성능을 평가하였다.

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Microstructure and Giant Magnetoresistance of AgCo Nano-granular Alloy Films (Ag-Co합금박막의 두께에 따르는 미세구조 변화 및 자기저항 거동)

  • 이성래;김세휘
    • Journal of the Korean Magnetics Society
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    • v.8 no.3
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    • pp.131-137
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    • 1998
  • The thickness dependence of the microstructure and the giant magnetoresistance behavior of co-evaporated Co-Ag granular alloy films were investigated. The maximum magnetoresistance ratio of 24% was observed in the the as-deposited state of the 40 at. % Co alloy having 200 nm thickness. The surface scattering contributed about 20% to the total resistivity in the 20 nm thick films. The MR ratio dropped sharply when the film thickness was below 50 nm. The reduction in the Co particle size and the increase in solid solubility of Ag in fcc Co when the film thickness decreased were observed using a high resolution TEM. The aspect ratio of the Co particles was also affected by the film thickness. Those microstructural changes as well as the surface induced spin flipping play a significant role in the $\Delta$p change.

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High quality topological insulator Bi2Se3 grown on h-BN using molecular beam epitaxy

  • Park, Joon Young;Lee, Gil-Ho;Jo, Janghyun;Cheng, Austin K.;Yoon, Hosang;Watanabe, Kenji;Taniguchi, Takashi;Kim, Miyoung;Kim, Philip;Yi, Gyu-Chul
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.284-284
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    • 2016
  • Topological insulator (TI) is a bulk-insulating material with topologically protected Dirac surface states in the band gap. In particular, $Bi_2Se_3$ attracted great attention as a model three-dimensional TI due to its simple electronic structure of the surface states in a relatively large band gap (~0.3 eV). However, experimental efforts using $Bi_2Se_3$ have been difficult due to the abundance of structural defects, which frequently results in the bulk conduction being dominant over the surface conduction in transport due to the bulk doping effects of the defect sites. One promising approach in avoiding this problem is to reduce the structural defects by heteroepitaxially grow $Bi_2Se_3$ on a substrate with a compatible lattice structure, while also preventing surface degradation by encapsulating the pristine interface between $Bi_2Se_3$ and the substrate in a clean growth environment. A particularly promising choice of substrate for the heteroepitaxial growth is hexagonal boron nitride (h-BN), which has the same two-dimensional (2D) van der Waals (vdW) layered structure and hexagonal lattice symmetry as $Bi_2Se_3$. Moreover, since h-BN is a dielectric insulator with a large bandgap energy of 5.97 eV and chemically inert surfaces, it is well suited as a substrate for high mobility electronic transport studies of vdW material systems. Here we report the heteroepitaxial growth and characterization of high quality topological insulator $Bi_2Se_3$ thin films prepared on h-BN layers. Especially, we used molecular beam epitaxy to achieve high quality TI thin films with extremely low defect concentrations and an ideal interface between the films and substrates. To optimize the morphology and microstructural quality of the films, a two-step growth was performed on h-BN layers transferred on transmission electron microscopy (TEM) compatible substrates. The resulting $Bi_2Se_3$ thin films were highly crystalline with atomically smooth terraces over a large area, and the $Bi_2Se_3$ and h-BN exhibited a clear heteroepitaxial relationship with an atomically abrupt and clean interface, as examined by high-resolution TEM. Magnetotransport characterizations revealed that this interface supports a high quality topological surface state devoid of bulk contribution, as evidenced by Hall, Shubnikov-de Haas, and weak anti-localization measurements. We believe that the experimental scheme demonstrated in this talk can serve as a promising method for the preparation of high quality TI thin films as well as many other heterostructures based on 2D vdW layered materials.

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Applications of the Scanning Electron Microscope (주사형(走査型) 전자현미경(電子顯微鏡)의 응용분야(應用分野))

  • Kim, Yong-Nak
    • Applied Microscopy
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    • v.2 no.1
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    • pp.39-46
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    • 1972
  • There are many kinds of microscopes suitable for general studies; optical microscopes(OM), conventional transmission electron microscopes (TEM), and scanning electron microscopes(SEM). The optical microscopes and the conventional transmission electron microscopes are very familiar. The images of these microscopes are directly formed on an image plane with one or more image forming lenses. On the other hand, the image of the scanning electron microscope is formed on a fluorescent screen of a cathode ray tube using a scanning system similar to television technique. In this paper, the features and some applications of the scanning electron microscope will be discussed briefly. The recently available scanning electron microscope, combining a resolution of about $200{\AA}$ with great depth of field, is favorable when compared to the replica technique. It avoids the problem of specimen damage and the introduction of artifacts. In addition, it permits the examination of many samples that can not be replicated, and provides a broader range of information. The scanning electron microscope has found application in diverse fields of study including biology, chemistry, materials science, semiconductor technology, and many others. In scanning electron microscopy, the secondary electron method. the backscattererd electron method, and the electromotive force method are most widely used, and the transmitted electron method will become more useful. Change-over of magnification can be easily done by controlling the scanning width of the electron probe. It is possible. to continuously vary the magnification over the range from 100 times to 1.00,000 times without readjustment of focusing. Conclusion: With the development of a scanning. electron microscope, it is now possible to observe almost all-information produced through interactions between substances and electrons in the form of image. When the probe is properly focused on the specimen, changing magnification of specimen orientation does not require any change in focus. This is quite different from the conventional transmission electron microscope. It is worthwhile to note that the typical probe currents of $10^{-10}$ to $10^{-12}\;{\AA}$ are for below the $10^{-5}$ to $10^{-7}\;{\AA}$ of a conventional. transmission microscope. This reduces specimen contamination and specimen damage due to heatings. Outstanding features of the scanning electron microscope include the 'stereoscopic observation of a bulky or fiber specimen in high resolution' and 'observation of potential distribution and electromotive force in semiconductor devices'.

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High Alloying Degree of Carbon Supported Pt-Ru Alloy Nanoparticles Applying Anhydrous Ethanol as a Solvent

  • Choi, Kwang-Hyun;Lee, Kug-Seung;Jeon, Tae-Yeol;Park, Hee-Young;Jung, Nam-Gee;Chung, Young-Hoon;Sung, Yung-Eun
    • Journal of Electrochemical Science and Technology
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    • v.1 no.1
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    • pp.19-24
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    • 2010
  • Alloying degree is an important structural factor of PtRu catalysts for direct methanol fuel cells (DMFC). In this work, carbon supported PtRu catalysts were synthesized by reduction method using anhydrous ethanol as a solvent and $NaBH_4$ as a reducing agent. Using anhydrous ethanol as a solvent resulted in high alloying degree and good dispersion. The morphological structure and crystallanity of synthesized catalysts were characterized by X-ray diffraction (XRD), high resolution transmission electron microscope (HR-TEM). CO stripping and methanol oxidation reaction were measured. Due to high alloying degree catalyst prepared in anhydrous ethanol, exhibited low onset potential for methanol oxidation and negative peak shift of CO oxidation than commercial sample. Consequently, samples, applying ethanol as a solvent, exhibited not only enhanced CO oxidation, but also increased methanol oxidation reaction (MOR) activity compared with commercial PtRu/C (40 wt%, E-tek) and 40 wt% PtRu/C prepared in water solution.

Property of Nickel Silicides with Hydrogenated Amorphous Silicon Thickness Prepared by Low Temperature Process (나노급 수소화된 비정질 실리콘층 두께에 따른 저온형성 니켈실리사이드의 물성 연구)

  • Kim, Jongryul;Choi, Youngyoun;Park, Jongsung;Song, Ohsung
    • Korean Journal of Metals and Materials
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    • v.46 no.11
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    • pp.762-769
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    • 2008
  • Hydrogenated amorphous silicon(a-Si : H) layers, 120 nm and 50 nm in thickness, were deposited on 200 $nm-SiO_2$/single-Si substrates by inductively coupled plasma chemical vapor deposition(ICP-CVD). Subsequently, 30 nm-Ni layers were deposited by E-beam evaporation. Finally, 30 nm-Ni/120 nm a-Si : H/200 $nm-SiO_2$/single-Si and 30 nm-Ni/50 nm a-Si:H/200 $nm-SiO_2$/single-Si were prepared. The prepared samples were annealed by rapid thermal annealing(RTA) from $200^{\circ}C$ to $500^{\circ}C$ in $50^{\circ}C$ increments for 30 minute. A four-point tester, high resolution X-ray diffraction(HRXRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and scanning probe microscopy(SPM) were used to examine the sheet resistance, phase transformation, in-plane microstructure, cross-sectional microstructure, and surface roughness, respectively. The nickel silicide on the 120 nm a-Si:H substrate showed high sheet resistance($470{\Omega}/{\Box}$) at T(temperature) < $450^{\circ}C$ and low sheet resistance ($70{\Omega}/{\Box}$) at T > $450^{\circ}C$. The high and low resistive regions contained ${\zeta}-Ni_2Si$ and NiSi, respectively. In case of microstructure showed mixed phase of nickel silicide and a-Si:H on the residual a-Si:H layer at T < $450^{\circ}C$ but no mixed phase and a residual a-Si:H layer at T > $450^{\circ}C$. The surface roughness matched the phase transformation according to the silicidation temperature. The nickel silicide on the 50 nm a-Si:H substrate had high sheet resistance(${\sim}1k{\Omega}/{\Box}$) at T < $400^{\circ}C$ and low sheet resistance ($100{\Omega}/{\Box}$) at T > $400^{\circ}C$. This was attributed to the formation of ${\delta}-Ni_2Si$ at T > $400^{\circ}C$ regardless of the siliciation temperature. An examination of the microstructure showed a region of nickel silicide at T < $400^{\circ}C$ that consisted of a mixed phase of nickel silicide and a-Si:H without a residual a-Si:H layer. The region at T > $400^{\circ}C$ showed crystalline nickel silicide without a mixed phase. The surface roughness remained constant regardless of the silicidation temperature. Our results suggest that a 50 nm a-Si:H nickel silicide layer is advantageous of the active layer of a thin film transistor(TFT) when applying a nano-thick layer with a constant sheet resistance, surface roughness, and ${\delta}-Ni_2Si$ temperatures > $400^{\circ}C$.