• Title/Summary/Keyword: TEM/EDS

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Biological Synthesis of Au Core-Ag Shell Bimetallic Nanoparticles Using Magnolia kobus Leaf Extract (목련잎 추출액을 이용한 Au Core-Ag Shell 합금 나노입자의 생물학적 합성)

  • Song, Jae Yong;Kim, Beom Soo
    • Korean Chemical Engineering Research
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    • v.48 no.1
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    • pp.98-102
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    • 2010
  • Magnolia kobus leaf extract was used for the synthesis of bimetallic Au core-Ag shell nanoparticles. Gold seeds and silver shells were formed by first treating aqueous solution of $HAuCl_4$ and then $AgNO_3$ with the plant leaf extract as reducing agent. UV-visible spectroscopy was monitored as a function of reaction time to follow the formation of bimetallic nanoparticles. The synthesized bimetallic nanoparticles were characterized with transmission electron microscopy(TEM), energy dispersive X-ray spectroscopy(EDS), and X-ray photoelectron spectroscopy(XPS). TEM images showed that the bimetallic nanoparticles are a mixture of plate(triangles, pentagons, and hexagons) and spherical structures. The atomic Ag contents of the bimetallic Au/Ag nanoparticles determined from EDS and XPS analysis were 34 and 65 wt%, respectively, suggesting the formation of bimetallic Au core-Ag shell nanostructure. This core-shell type nanostructure is expected to have potential for application in surface enhanced Raman spectroscopy and in the sensitive detection of biomolecules.

Enhanced Electrochemical Properties of Surface Modified LiMn2O4 by Li-Fe Composites for Rechargeable Lithium Ion Batteries

  • Shi, Jin-Yi;Yi, Cheol-Woo;Liang, Lianhua;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.2
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    • pp.309-314
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    • 2010
  • The surface modified $LiMn_2O_4$ materials with Li-Fe composites were prepared by a sol-gel method to improve the electrochemical performance of $LiMn_2O_4$ and were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), and transmission electron microscopy (TEM)-EDS. XRD results indicate that all the samples (modified and pristine samples) have cubic spinel structures, and XRD, XPS, and TEM-EDS data reveal the formation of $Li(Li_xFe_xMn_{2-2x})O_4$ solid solution on the surface of particles. For the electrochemical properties, the modified material demonstrated dramatically enhanced reversibility and stability even at elevated temperature. These improvements are attributed to the formation of the solid solution, and thus-formed solid solution phase on the surface of $LiMn_2O_4$ particle reduces the dissolution of Mn ion and suppresses the Jahn-Teller effect.

Asbestos Analysis of China Sepiolite by Transmission Electron Microscopy (중국산 해포석 내 석면 함유 유무 분석)

  • Song, Se Wook;Chung, Yong Hyun;Han, Jeong Hee
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.23 no.3
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    • pp.205-211
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    • 2013
  • Objectives: 21 sepiolite substances produced in China were investigated for the presence of asbestos in their materials. Materials and methods: In order to identify asbestos in sepiolite substances, test materials were analyzed using a transmission electron microscope equipped with energy dispersive X-ray spectrometer (TEM-EDS) for confirming their shape and components (atomic %). Results: Five of 21 sepiolte substances were asbestos-containing materials. Two chrysotile containing sepiolite proved to be asbestoscontaining materials, as did two chrysotile mixed with tremolite containing sepiolite. 16 sepiolite substances did not contain asbestos materials. Conclusions: When importing sepiolite substances, they must be analyzed to determine if there is asbestos in their materials.

Vertically Distributed Aerosol Sampling and Analysis using Tethered Balloon Sampler System in Ansan (안산지역 내에서의 Tethered Balloon 탑재형 포집기를 이용한 연직 분포된 Aerosol 포집 및 분석)

  • Eun, Hee-Ram;Kim, Whan-Ki;Lee, Hong-Ku;Yoo, Dong-Hyun;Yook, Se-Jin;Ahn, Kang-Ho
    • Particle and aerosol research
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    • v.7 no.4
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    • pp.139-149
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    • 2011
  • It is very important to measure atmospheric particles and evaluate the characteristics of them since aerosol can influence atmospheric environment, climate, and health. Satellite, aircraft, radio sonde are usually used to measure the vertical distribution of particle properties, temperature, humidity, and pressure. Although the method of using an aircraft is favorable to collect the horizontal distribution of the particles, but unadaptable to measure the vertical distribution of the particles. However, all-in-one balloon particle sampler system can collect particles depending on each altitude controling the balloon by winch. In this research, we performed the air sampling on the TEM grids using house made light weight impactor at the altitude of 300m and 900m. The collected particles were analyzed using TEM/EDS.

EF-TEM을 이용한 직접가열 실험을 통한 Titanium의 고온에서의 상변화 연구

  • 김진규;이영부;김윤중
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.22-23
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    • 2002
  • Titanium은 높은 강도, 낮은 밀도, 부식에 대한 저항 등, 타 금속에 비해 월등히 뛰어난 성질을 가지고 있기 때문에 산업 전반에 거쳐 그 응용이 크게 증가하고 있으며, 특히 고온에서의 응용이 중요성을 띠게 됨에 따라 고온으로의 상전이 관계에 따른 구조적 규명이 필요하다. 순수한 titanium은 상온에서 조밀충진 육방정계의 α-상구조(a=2.953Å, c=4.683 Å, P6₃/mmc)를 이루고 있으나, 대략 880℃ 이상에서는 β-상의 체심입방정계 (a=3.320Å, Im3m)로 상전이가 되는 것으로 알려져 있다. 이에 대한 대부분의 연구가 kinetics와 thermodynamics에 관련되어 있으며, TEM을 이용한 직접가열실험은 거의 전무한 상태이다. 본 실험에서는 TEM 직접가열을 통하여 titanium의 고온에서의 상전이와 가열시 발생할 수 있는 산화층 형성을 연구하였다. TEM 시편은 순도 99.94%의 titanium foil(Alfa Aesar, #00360, 0.025mm thick)를 이용하였고, 분석 장비로는 에너지여과 기능이 있는 TEM(EM912 Omega, Carl Zeiss)과 Gatan사의 double-tilt heating holder를 사용하였다. Titanium의 상전이를 관찰하기 위해 900℃ 까지 분당 10℃ 의 속도로 가열을 하였다. 통계적 분석 오차를 줄이기 위해 서로 다른 4군데의 관찰영역을 선택하여, 상온 - 600℃ - 900℃ - 상온의 단계별로 회절패턴을 관찰 및 기록하였고, 발생 가능한 산화에 대해서는 동일한 장비를 사용하여 EDS 분석을 하였다. 상온에서의 서로 다른 영역의 회절패턴들은 결함의 존재에 상관없이, 온도가 증가함에 따라 그 결함수가 증가하게 된다. 특히 600℃ 에서는 쌍정과 관련된 회절점들이 본래의 회절점 주위에 형성되어있지만, 각 면들의 격자상수의 변화는 나타나지 않았다. 그러나 900℃ 에서는 쌍정에 의한 회절점의 수가 증가하며, 회절점 사이에 발달한 뚜렷한 막대모양의 강도분포와 격자상수의 변화를 관찰할 수 있었다. 다시 상온으로 냉각시킨 후 관찰한 각각의 회절패턴에서는 격자 상수의 감소와 함께 900℃에 보여진 막대 모양의 강도분포와 쌍정에 의한 회절점들이 여전히 남아있었다. EDS분석 결과 가열 실험을 통해 시편이 열적 산화가 되어 있음을 확인 할 수 있었다. 순수한 titanium의 α-상에서 β-상으로의 상전이를 파악할 수 있는 격자상수의 변화자체는 매우 작은 값이기 때문에 상온과 900℃ 에서 기록된 전자회절패턴 상에서의 면간거리와 면간각도의 측정만으로는 상전이 여부를 명확히 구별할 수 없었다. 그러나, 결함에 의한 상변화가 900℃ 에서 심하게 관찰되어지는 것은 상전이와 관계가 있는 것으로 볼 수 있다. 고온에서 상온으로의 가역적 반응을 관찰할 수 없었던 이유는 열적산화로 생긴 산화층의 산소원자들이 고온의 상전이 과정 중에 Ti 원자와 반응이 일어나 TiO/sub X/ 구조로 전이되었기 때문으로 추정하고 있다.

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Toxicity of Talc Containing Tremolite asbestos on Respiratory System in Sprague-Dawely Rats (랫드의 기도로 투여된 투각섬석함유활석이 호흡기계에 미치는 영향 연구)

  • Chung, Yong-Hyun;Han, Jeong-Hee;Kang, Min-Gu;Lee, Sung-Bae;Kim, Jong-Kyu;Kim, Hyeon-Yeong;Yang, Jung-Sun
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.20 no.2
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    • pp.119-130
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    • 2010
  • Pulmonary toxicity of talc containing tremolite asbestos (TCT) has been studied in term sequential in Sprague-Dawely rats. UICC chrysotile(average diameter 0.03${\mu}m$, average length 2.93${\mu}m$) was applied as the positive control. TCT was analyzed for its physicochemical properties by transmission electron microscope equipped with energy dispersive X-ray spectrometer(TEM-EDS). The effects of 2mg TCT(talc average diameter 9.7${\pm}$8.4${\mu}m$; tremolite average diameter 1.6${\pm}$1.6${\mu}m$, average length 10.8${\pm}$7.0${\mu}m$) on pathological changes were evaluated after 1, 8 weeks instilled into rat lungs. 2mg Chrysotile continuously affected lung pathological changes. Inflammation and granuloma response broke out from 1 week after instilled with chrysotile and the pathological examination further showed increased legions of lung after 8 weeks. But TCT did not showed lung pathological changes. The biopersistence of TCT and chrysotile was evaluated by TEM- EDS. Whereas chrysotile continuously have retained to 8 weeks instilled into rat lungs, talc of TCT showed statistically significant decrease of diameter from 1 weeks and statistically significant change in Si atomic % compositions at 8 weeks instilled into rat lungs. Physicochemical properties of tremolite of TCT were not affected until 8 weeks instilled into rat lungs. This study showed that the durability of TCT in the lungs is much weaker than chrysotile.

Confirmation of Long-term stability on THPP using thermodynamic and kinetic analysis (열역학적 및 속도론적 분석을 통한 THPP의 노화 안정성 확인)

  • Lee, Junwoo;Kim, Sangwon;Choi, Kyoungwon;Lee, Seung Bok;Ryu, Byungtae;Park, Taiho
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2017.05a
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    • pp.513-516
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    • 2017
  • When stored for long periods in a powder-based device (PMD), the explosive power in the device is aged and the explosive power is changed. Thus, The gunpowder used in the PMD must be chemically and physically stable for both internal and external factors. Since $BKNO_3$ and THPP are used as representative gunpowder, thermodynamic and kinetic analyzes were performed based on these gunpowders. Differential scanning calorimeter (DSC) was used to analyze the calorific value and reaction rate. As a result, there was no significant change in caloric value and reaction rate in THPP. In addition, XPS and TEM-EDS analyzes were performed to confirm the formation of oxide films directly related to aging, and no oxide films were observed as a result of thermal analysis. In addition, XPS and TEM-EDS analyzes were performed to confirm the formation of oxide films directly related to aging. As a results, no oxide films were observed. It can be concluded that THPP is the most famous gunpowder in terms of long-term stability.

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Transmission Electron Microscopy Specimen Preparation for Layer-area Graphene by a Direct Transfer Method

  • Cho, Youngji;Yang, Jun-Mo;Lam, Do Van;Lee, Seung-Mo;Kim, Jae-Hyun;Han, Kwan-Young;Chang, Jiho
    • Applied Microscopy
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    • v.44 no.4
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    • pp.133-137
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    • 2014
  • We suggest a facile transmission electron microscopy (TEM) specimen preparation method for the direct (polymer-free) transfer of layer-area graphene from Cu substrates to a TEM grid. The standard (polymer-based) method and direct transfer method were by TEM, high-resolution TEM, and energy dispersive X-ray spectroscopy (EDS). The folds and crystalline particles were formed in a graphene specimen by the standard method, while the graphene specimen by the direct method with a new etchant solution exhibited clean and full coverage of the graphene surface, which reduced several wet chemical steps and accompanying mechanical stresses and avoided formation of the oxide metal.

A Study of Titanium Phase Transition through In-situ EF-TEM Heating Experiments (EF-TEM 직접가열 실험을 통한 titanium의 고온 상전이 연구)

  • Kim, Jin-Gyu;Lee, Young-Bu;Kim, Youn-Joong
    • Applied Microscopy
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    • v.33 no.1
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    • pp.49-58
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    • 2003
  • The ${\alpha}-{\beta}$ phase transition of titanium was investigated through in-situ EF-TEM heating experiments. Three different areas of a titanium foil were observed to minimize statistical errors. Systematic recording of diffraction patterns and images was carried out from $RT{\rightarrow}600^{\circ}C{\rightarrow}900^{\circ}C{\rightarrow}RT$ on each area. The following results were obtained: (1) Transition of titanium takes place very rapidly at $900^{\circ}C$. Two phases of titanium, ${\alpha}\;and\;{\beta}$, coexist at this temperature. (2) The transited ${\beta}$-phase appears in the form of twinned plates which are arranged in rotation relationship one another. (3) Analyses of electron diffraction patterns and EDS data indicate that the thermal oxidation layer is gradually formed on the surface of titanium above $900^{\circ}C$, which hinders the reversible ${\beta}{\rightarrow}{\alpha}$ phase transition upon cooling.