• Title/Summary/Keyword: TEM Journal

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Properties and particles dispersion of biodegradable resin/clay nanocomposites

  • Okada, Kenji;Mitsunaga, Takashi;Nagase, Youichi
    • Korea-Australia Rheology Journal
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    • v.15 no.1
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    • pp.43-50
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    • 2003
  • In this study, two types of biodegradable resins-based clay nanocomposites, in which organic montmorillonite clay was filled, were prepared by the direct melt blending method. In order to characterize the nanocomposite structure, wide-angle X-ray diffraction (WAXD) and TEM observation were performed. Characterization of the nanocomposites shows that intercalated and partially exfoliated structures were generated by the melt blending method. Mechanical and rheological properties of the nanocomposites were measured respectively. For the mechanical properties, there were improvements in tensile strength and Young's modulus of the nanocomposites due to the reinforcement of nanoparticles. The rheological behaviors of the nanocomposites were significantly affected by the degree of the dispersion of the organoclay. The storage modulus of the nanocomposites was measured and the degree of the dispersion of the organoclay was evaluated from the value of the terminal slope of the storage modulus. In addition, the quantity of the shear necessary for making the nanocomposite for melt intercalation method was estimated from the relationship between the value of the terminal slope of the storage modulus and the applied shear.

A Study on the Cracking Behavior in the Welds of Ni-Cr-Fe and Ni-Fe-Cr-Mo Alloys Part I : Solidification Cracking in the Fusion Zone (Ni-Cr-Fe 및 Ni-Fe-Cr-Mo계 합금의 용접부 균열특성에 관한 연구 Part I : 용착금속의 응고균열)

  • 김희봉;이창희
    • Journal of Welding and Joining
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    • v.15 no.4
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    • pp.78-89
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    • 1997
  • This study has evaluated the weld metal solidification cracking behavior of several Ni base superalloys (Incoloy 825, Inconel 718 and Inconel 600). Austenitic stainless steels(304, 310S) were also included for comparison. In addition, a possible mechanism of solidification cracking in the fusion zone was suggested based on the extensive microstructural examinations with SEM, EDAX, TEM, SADP and AEM. The solidification cracking resistance of Ni base superalloys was found to be far inferior to that of austenitic stainless steels. The solidification cracking of Incoloy 825 and Inconel 718 was believel to be closely related with the Laves-austenite (Ti rich in 825 and Nb rich in 718) and MC-austenite eutectic phases formed along the grain boundaries during solidification. Cracking in Inconel 600 was always found along the grain boundaries which were enriched with Ti and P. Further, solidifidcation cracking resistance was dependent not only upon the type of love melting phases but also on the amount of the phases along the solidification grain boundaries.

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A Study on the Strength Characteristics of $L1_{2}-Ni_{3}Al$ Intermetallic Compound ($L1_{2}-Ni_{3}Al$ 금속간화합물의 강도특성에 관한 연구)

  • Han, Chang-Suk;Chun, Chang-Hwan;Han, Seung-Oh
    • Journal of the Korean Society for Heat Treatment
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    • v.22 no.1
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    • pp.8-15
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    • 2009
  • Structural studies have been performed on precipitation hardening found in $Ni_{3}Al$ based ordered alloys using transmission electron microscopy (TEM). Tilt experiments by the weak-beam method were made to obtain some information concerning the cross slip mechanism of the superlattice dislocation. The strength of ${\gamma}'-Ni_3$(Al,Ti) increases over the temperature range of experiment by the precipitation of fine $\gamma$ particles. The peak temperature where a maximum strength was obtained shifted to higher temperature. Over the whole temperature range, the interaction between dislocation and $\gamma$ precipitates is attractive. On the temperature range of 773 K to 973 K, the dislocations in ${\gamma}'$ matrix move on (111) primary slip plane. When the applied stress is removed, the dislocations make cross slip into (010) plane, while those in $\gamma$ precipitates remain on the (111) primary slip plane. The increase of high temperature strength in ${\gamma}'-Ni_3$(Al,Ti) containing $\gamma$ precipitates is due to the restraint of cross slip of dislocations from (111) to (010) by the dispersion of disordered $\gamma$ particles.

Effect of cooling rate on the microstructure and impact toughness of Cu-bearing HSLA steels (Cu를 함유한 HSLA강의 미세 조직과 인성에 미치는 냉각 속도의 영향)

  • 박태원;심인옥;김영우;강정윤;박화순
    • Journal of Welding and Joining
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    • v.13 no.2
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    • pp.122-131
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    • 1995
  • The effects of cooling rate on the microstructures, precipitation of Cu-cluster, .epsilon.-Cu and impact toughness of high strength low alloy(HSLA) steel were studied using hardness tester, impact tester, DSC(differential scanning calorimetry), AES(auger electron spectroscopy) and TEM(transmission electron microscopy). Not only the Cu-precipitates but also the segregation of Cu, As, Sb, P, S, N, Sn along grain boundary were not observed at the specimens heat treated from 800.deg. C to 300.deg. C with the cooling time of 12-125 sec. The Cu-cluster, .epsilon.-Cu are formed by introducing ageing after cooling and the effect of precipitates on hardening increase after cooling was the same in all cooling rate. The peak hardness was obtained at an ageing of 500.deg. C in all cooling conditions. The impact energy become higher as the cooling time increases. This fact can be explained to be due to the tempering effect applied on the cooling stage since the present alloy has a relatively high Ms temperature and the local high concentration of the retained austenite.

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Characteristics of Silicon Oxide Films Grown by Rapid Thermal Oxidation (급속일산화법에 의한 실리콘 산화막의 특성)

  • 이귀연;양두영;이재용
    • Journal of the Korean Institute of Telematics and Electronics A
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    • v.28A no.12
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    • pp.59-64
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    • 1991
  • Thin (25-103$\AA$) SiO$_2$ films are grown using the rapid thermal oxidation processing at temperatures of 105$0^{\circ}C$-115$0^{\circ}C$ for 5-30 sec, in order to investigate the characteristics of ultra thin oxide. For measuring the thickness of oxide TEM, ellipsometry, and C-V method which is taken in the condition of small surface band bending are used and compared. When neglecting the small deviation affected by both interface state and moisture charge effect, those three methods described above give similar results. In order to examine the effect of rapid thermal annealing, part of samples are annealed in N$_2$ ambient. MOS capacitors are fabricated and the characteristics of I-V and C-V are measured. Measurements show that the activation energy of initial thickness of oxide grown during the ramp-up time is of 1.125eV and the activation energy of the oxidation rate is of 0.98eV. As oxidation temperature is increased, dielectric breakdown field E$_{BD}$ is decreased due to the increase of fixed charge density N$_f$ However, E$_{BD}$ is shown to be decreased as increasing the thickness of oxide. The increase of N$_f$ in the early stage of thermal annealing results in the decrease of E$_{BD}$.

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A Study on Formation of Ni-Tl-P deposits by Electroless Plating (무전해도금에 의한 Ni-Tl-P 피막형성에 관한 연구)

  • 류일광;추현식
    • Journal of Surface Science and Engineering
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    • v.33 no.2
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    • pp.126-134
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    • 2000
  • This study investigated the bath compositions and plating conditions and crystal structure used for achieving nickel-thallium-phosphorus deposits by means electroless plating. The electroless nickel-thallium-phosphorus deposits were achieved with a bath using sodium hypophosphite as the reducing agent and sodium citrate as the complexing agent. The depositing rate was 10.5mg.$cm^{2-1}$ .$hr^{-1 }$ from the optimistic bath composition, 0.1M nickel sulfate, 0.005M thallium sulfate, 0.2M sodium hypophosphite, and 0.05M sodium citrat and the recommended plating conditions, pH 5.5 and $90^{\circ}C$. The composition of alloy deposits determined by X-ray analysis (EDS) that the Thallium was increased with major increasing concentration of complexing agent and thallium ion in bath solution, it decreased according to the increasing concentrations of reduction agent in the bath solution, Bit Phosphorus showed a contrary to the thallium. It was observed from X-ray diffraction analysis, Scanning Electron Microscopy and Transmission Electron Microscopy. The crystalline structure of deposits was amorphous at the first deposited state but it was changed $Ni-T1-Ni_{5}$ $P_2$ polycrystalline when subjected to 1 hour heat treatment of more than $350^{\circ}C$. TEM observation demonstrated that the microstructure was identical to the result of the XRD at as deposited but it became $Ni-Tl-Ni_{5}$ $P_2$ polycrystalline when heated. And grain size was 10-50nm.

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Homogeneous Mixing of Si3N4 with Sintering Additives by Coprecipitation Method (질화규소의 소결첨가제의 공침법에 의한 균일혼합)

  • 김지순
    • Journal of the Korean Ceramic Society
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    • v.30 no.10
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    • pp.829-837
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    • 1993
  • Chemically and geometrically homogeneous mixing of Si3N4 powders with sintering additives(YAG, 3Y2O3$.$5Al2O3) was attempted via coprecipitation method. X-ray dot maps for the additive elements(Al and Y) showed that the additives are evenly distributed in the powder mixture prepared by coprecipitation method(CP). TEM observation of the coprecipittion-treated Si3N4 powders revealed that they are covered with extremely fine crystallites of additive. The shift in isoelectric point(IEP) of Si3N4 powders from pH 6.7 to pH 7.9 after coprecipitation mixing gave another evidence for coating of Si3N4 powders with YAG additives. SIMS analysis for composition on the surface and in the matrix of mixed powders showed that the YAG additives are highly enriched on the surface of coprecipitation-treated Si3N4 powders. Especially when a small amount of additive was used, the effect of homogeneous additive distribution on densification was preceptible: After pressureless-sintering of powder compacts containing 5 mol% YAG at 1800$^{\circ}C$ for 0.5h, a sintered density of 96.5% theoretical was obtained from the specimens prepared bycoprecipitation in comparison with 93.8% from the mechanically-mixed one.

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Preparation and Characteristics of Nanometer-sized ZnO Powder by Solution Combustion Process for Photocatalyst Applications (용액 연소법에 의한 광촉매용 나노크기의 ZnO 분말의 제조 및 특성)

  • Lee, Kang-Ryeol;Kim, Whung-Whoe;Park, Sung
    • Journal of the Korean Ceramic Society
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    • v.38 no.8
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    • pp.765-770
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    • 2001
  • 광촉매용 ZnO 나노크기의 분말은 시작원료와 연료의 종류에 따라 용액연소법에 의해 제조되었다. 결정상은 XRD로부터 확인할 수 있었으며 분말의 하소온도는 TG 분석으로부터 결정되었다. 분말의 비표면적은 BET 법에 의해 측정되었으며 평균입자크기와 형태를 SEM과 TEM으로부터 조사하였다. 또한 분말의 순도를 조사하기 위해 적외선 흡수스펙트럼을 측정하였으며 광촉매 효율로서 은이 첨가된 사진현상액을 이용하여 은의 수거율을 측정하였다. 용액연소법으로 제조한 경우 시작원료와 연료에 관계없이 단상의 ZnO 분말을 쉽게 얻을 수 있었다. 그러나 합성된 ZnO 분말의 입자크기와 형태는 연료의 종류에 따라 서로 다르게 보였다. 특히, 연료로 glycine을 사용한 경우, ZnO 분말의 입자 형태는 균일한 나노 크기의 구형이었으나 carbohydrazide을 사용한 경우에는 판상과 같은 형태를 보였다. 이러한 결과를 기초로 하여 시작원료와 연료로 Zn(OH)$_2$와 glycine을 사용하여 합성된 ZnO 분말이 우수한 분말 특성을 보였으며 75nm의 입자크기와 94$m^2$/g의 비표면적을 보였다. 또한 사진현상액에 존재하는 은이 3분 이내에 완전히 제거되는 우수한 광촉매 성질을 보였다.

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Effects of Thermal Annealing on Dielectric and Piezoelectric Properties of Pb(Zn, Mg)1/3Nb2/3O3-PbTiO3 System in the Vicinity of Morphotropic Phase Boundary

  • Hyun M. Jang;Lee, Kyu-Mann
    • The Korean Journal of Ceramics
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    • v.1 no.1
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    • pp.13-20
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    • 1995
  • Effects of thermal annealing on the dielectric/piezoelectric properties of $Pb(Zn, Mg)_{1/3}Nb_{2/3}O_3-PbTiO_3$ ceramics (PZMNPT) with Zn/Mg=6/4) were examined across the rhombohedral/tetragonal morphotropic phase boundary (MPB). Both the relative dielectric permittivity ($\varepsilon$r)and the piezoelectric constant($d_33$)/electromechanical coupling constant ($k_p$)were increased by thermal annealing ($800^{\circ}$~$900^{\circ}C$) after sintering at $1150^{\circ}C$ for 1 hr. Based on the dielectric analysis using the series mixing model and the concept of a random distribution of the local Curie points, the observed improvements in the dielectric and piezoelectric properties of PZMN-PT were interpreted in terms of the elimination of PbO-rich amorphous intergranular layers(~1nm) induced by thermal annealing. A concrete evidence of the presence of amorphous grain-boundary layers in the unannealed (as-sintered) specimen was obtained by examining the structure of intergranular region using a TEM.

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Effect of $\alpha-Al_2O_3$ Seeds and Alumina Sol on $\alpha$-Alumina Powder Derived from $\gamma-Al_2O_3$ ($\gamma$-알루미나부터 $\alpha$-알루미나 분말 제조에 있어 Seeding과 알루미나 졸이 미치는 영향)

  • 임경란;장진욱;임창섭;홍국선
    • Journal of the Korean Ceramic Society
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    • v.32 no.4
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    • pp.482-488
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    • 1995
  • The phase transformation temperature from $\theta$- to $\alpha$-alumina was lowered from 1214$^{\circ}C$ to 114$0^{\circ}C$ in DSC by treating ${\gamma}$-alumina obtained by calcination of boehmite at $700^{\circ}C$ for 2hrswith $\alpha$-Al2O3 seeds (d50=0.36${\mu}{\textrm}{m}$) and 3wt% of the alumina sol. $\alpha$-Al2O3 seeds seemed to lower to the transformation temperature and the alumina sol suppressed the high temperature agglormeration. The effect was increased as the amount of the sol was increased, which was supported by TEM and particle size distribution. For an example, spherical ${\gamma}$-alumina powder with d50=0.54${\mu}{\textrm}{m}$ was prepared by treating the ${\gamma}$-alumina with 9 wt% of the alumina sol and 3wt% of the $\alpha$-Al2O3. It sintered to 99% of the theoretical density at 150$0^{\circ}C$ for 2hrs. and it had relatively homogeneous microstructure with 2~3${\mu}{\textrm}{m}$ sized grains.

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