• Title/Summary/Keyword: TEM microstructure

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Microstructure and Microdefects of Diamond Thin Films Deposited by MPECVD (마이크로웨이브 화학증착법에 의한 다이아몬드 박막의 미세구조오 미세결함)

  • Lee, Se-Hyeon;Lee, Yu-Gi;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.6 no.8
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    • pp.833-840
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    • 1996
  • Diamond thin films were deposited on p-type (100) Si wafers using MPECVD. Prior to deposition, ultrasonic striking was done to improve density of nucleation sites with dimond powder of 40~$60\mu$m size. Then diamond thin films were deposited at $^900{\circ}C$, 40Torr and 1000W microwave power using ${CH}_{4}$ and ${H}_{2}$ gases. The purity, the morphology and the microstructur'e and microdefects of diamond thin films were characterized by Raman spectroscopy, SEM and TEM, repectively. In Raman spectroscopy the peaks of non-diamond phase increased as ${CH}_{4}$, concentration increased. In SEM, the morphology of diamond thin films varied from crystalline to cauliflower as ${CH}_{4}$, concentration increased. As ${CH}_{4}$ con centration increased, the density of defects increased, with most defects being {III} twin. ${MTP}_{5}$, were formed with five (II]) planes. As these (Ill) Planes were twinned, ${MTP}_{5}$, represented five-fold symmetry. ]n the interfaces, defects in diamond thin films fanned out from small regions implying nucleation sites.

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Analysis of the microstructure of melting-pool in aluminum specimens fabricated by SLM technique (SLM 기법으로 제작한 알루미늄 시편 내부 멜팅풀 미세조직 분석)

  • Kim, Moo-Sun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.12
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    • pp.115-119
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    • 2020
  • Selective Laser Melting (SLM) technology is state-of-the-art additive manufacturing process technology that produces a three-dimensional structure by irradiating a laser on a fine metal powder to perform the fusion of a specific area and repeat this process. Owing to the characteristics of the additive manufacturing process, the melting phenomenon of the metal material by the laser has directionality depending on the process conditions, such as the irradiation direction of the laser and the build-up direction. For this reason, the composition of the metal material in the structure exhibits non-uniform characteristics. In this study, aluminum (AlSi10Mg) specimens were manufactured by applying SLM technology, and the material composition characteristics of the specimen were analyzed. The specimens were manufactured as cylinders by the build-up orientation of 0°, 45°, and 90°. The surface morphology of the specimen plane was analyzed optically. TEM analysis was performed on the core and the interface of the melting-pool inside the specimen generated by laser irradiation. The analysis results confirmed that there was a difference between the nano cell structure of the core and the interface of the melting-pool, and that the composition ratio of Si appeared higher at the interface than at the core of the cell.

The Effect of Stacking Fault on Thermoelectric Property for n-type SiC Semiconductor (N형 SiC 반도체의 열전 물성에 미치는 적층 결함의 영향)

  • Pai, Chul-Hoon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.3
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    • pp.13-19
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    • 2021
  • This study examined the effects of stacking faults on the thermoelectric properties for n-type SiC semiconductors. Porous SiC semiconductors with 30~42 % porosity were fabricated by the heat treatment of pressed ��-SiC powder compacts at 1600~2100 ℃ for 20~120 min in an N2 atmosphere. XRD was performed to examine the stacking faults, lattice strain, and precise lattice parameters of the specimens. The porosity and surface area were analyzed, and SEM, TEM, and HRTEM were carried out to examine the microstructure. The electrical conductivity and the Seebeck coefficient were measured at 550~900 ℃ in an Ar atmosphere. The electrical conductivity increased with increasing heat treatment temperature and time, which might be due to an increase in carrier concentration and improvement in grain-to-grain connectivity. The Seebeck coefficients were negative due to nitrogen behaving as a donor, and their absolute values also increased with increasing heat treatment temperature and time. This might be due to a decrease in stacking fault density, i.e., a decrease in stacking fault density accompanied by grain growth and crystallite growth must have increased the phonon mean free path, enhancing the phonon-drag effect, leading to a larger Seebeck coefficient.

Penetration behavior by carbon potential in laser-carburized TiZrN coatings (TiZrN 코팅의 레이저 침탄에서 탄소 포텐셜에 따른 침입 거동)

  • Lee, Byunghyun;Kim, Taewoo;Hong, Eunpyo;Kim, Seonghoon;Lee, Heesoo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.6
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    • pp.282-286
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    • 2021
  • Penetration depth and compressive residual stress of laser-carburized TiZrN coating by thickness of carbon paste were investigated in terms of carbon potential. The carbon paste was covered with a thickness of 1.1 mm using screen printing, and applied to a thickness of 0.4 mm using spin coating, and laser carburization was performed under the same conditions. As the thickness of carbon paste increased, the diffraction pattern of the laser-carburized TiZrN coating shifted to a lower angle, indicating solid solution strengthening and lattice distortion. For microstructure analysis using TEM, the defects and carbon concentration of the laser-carburized TiZrN coating increased as the carbon paste was thicker. It indicated that the variation of the carbon potential corresponds to the change in the paste thickness. In XPS depth profile analysis, high concentration of carbon and formation of carbide were observed in laser-carburized TiZrN coating with thick carbon paste. It revealed that the carbon concentration on the surface and carbon potential were changed by the thickness control of carbon paste. The compressive residual stress increased from 3.67 GPa to 4.58 GPa by the variation of carbon concentration.

A Study on the Physical Properties of a Compound Using the Crosslinking of Vinylized-mesoporous Silica and Regenerated Polyethylene (비닐화 실란이 도입된 메조포러스 실리카와 재생 폴리에틸렌의 가교결합을 이용한 컴파운드의 물성 연구)

  • Tae-Yoon Kim;Hyun-Ho Park;Chang-Seop Lee
    • Journal of the Korean Chemical Society
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    • v.67 no.6
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    • pp.420-428
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    • 2023
  • Crosslinking was introduced into vinylized-mesoporous silica and recycled polyethylene. By introducing a vinyl group into the mesoporous silica, it becomes a material capable of inducing cross-linking with non-polar polyethylene. By synthesizing vinylized-mesoporous silica and inducing crosslinking with recycled polyethylene, a recycled polyethylene composite with improved physical properties than existing recycled polyethylene was synthesized. In addition, even when a small amount is added according to the grade of recycled polyethylene using vinylized-mesoporous silica, the crosslinking reaction proceeds and all physical properties are improved. Four types of vinylized-mesoporous silica were synthesized, and the shape, microstructure, and functional groups were analyzed by TEM, BET, FT-IR, and XRD. Using vinylized-mesoporous silica, three types of compounds were blended by crosslinking reaction with recycled polyethylene. In order to confirm the presence or absence of crosslinking, analysis was performed using XPS and FT-IR, and physical properties such as tensile strength, elongation, flexural strength, and flexural modulus were confirmed using a universal testing machine. As a result, by applying vinylized-mesoporous silica to recycled polyethylene in various grades, the weak physical properties of existing recycled polyethylene were overcome. By applying the vinylized-mesoporous silica, recycled polyethylene composite material that overcomes the weak physical properties to the normal polyethylene, it shows the optimal physical property index that can be used commercially. Therefore, it is expected that it can potentially increase the use of recycled polyethylene and recycle resources.

Effect of Ti-Doped Al2O3 Coating Thickness and Annealed Condition on Microstructure and Electrochemical Properties of LiCoO2 Thin-Film Cathode (Ti 첨가 Al2O3 코팅층의 두께와 열처리 조건이 LiCoO2 양극 박막의 미세구조와 전기화학적 특성에 미치는 영향)

  • Choi, Ji-Ae;Lee, Seong-Rae;Cho, Won-Il;Cho, Byung-Won
    • Korean Journal of Materials Research
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    • v.17 no.8
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    • pp.447-451
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    • 2007
  • We investigated the dependence of the various annealing conditions and thickness ($6\sim45nm$) of the Ti-doped $Al_2O_3$ coating on the electrochemical properties and the capacity fading of Ti-doped $Al_2O_3$ coated $LiCoO_2$ films. The Ti-doped-$Al_2O_3$-coating layer and the cathode films were deposited on $Al_2O_3$ plate substrates by RF-magnetron sputter. Microstructural and electrochemical properties of Ti-doped-$Al_2O_3$-coated $LiCoO_2$ films were investigated by transmission electron microscopy (TEM) and a dc four-point probe method, respectively. The cycling performance of Ti-doped $Al_2O_3$ coated $LiCoO_2$ film was improved at higher cut-off voltage. But it has different electrochemical properties with various annealing conditions. They were related on the microstructure, surface morphology and the interface condition. Suppression of Li-ion migration is dominant at the coating thickness >24.nm during charge/discharge processes. It is due to the electrochemically passive nature of the Ti-doped $Al_2O_3$ films. The sample be made up of Ti-doped $Al_2O_3$ coated on annealed $LiCoO_2$ film with additional annealing at $400^{\circ}C$ had good adhesion between coating layer and cathode films. This sample showed the best capacity retention of $\sim92%$ with a charge cut off of 4.5 V after 50 cycles. The Ti-doped $Al_2O_3$ film was an amorphous phase and it has a higher electrical conductivity than that of the $Al_2O_3$ film. Therefore, the Ti-doped $Al_2O_3$ coated improved the cycle performance and the capacity retention at high voltage (4.5 V) of $LiCoO_2$ films.

The Effects of Nitrogen on Microstructure and Magnetic Properties of Nanocrystalline Fe-Nb-B-N Thin Films (나노결정구조 Fe-Nb-B-N 박막의 미세구조 및 자기적 특성)

  • 박진영;서수정;노태환;김광윤;김종열;김희중
    • Journal of the Korean Magnetics Society
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    • v.7 no.5
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    • pp.250-257
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    • 1997
  • The microstructure and magnetic properties of Fe-Nb-B-N thin film alloys, which produced by rf magnetron sputtering method in $Ar+N_2$ mixed gas atmosphere, were investigated. The $Fe_{70}Nb_{14}B_{11}N_5$ films, annealed at 59$0^{\circ}C$, exhibit soft magnetic properties: $4{\pi}M_s=16.5kG$ , $H_c=0.13Oe$ and ${\mu}_{eff}$ (1~10 MHz)=5, 000. The frequency stability of the Fe-Nb-B-N films has also been found to be good up to 10 MHz. The Fe-Nb-B-N thin film alloys annealed at 59$0^{\circ}C$ consist of three phase; fine crystalline $\alpha$-Fe phase with grain size of about 5~10 nm, Nb-B rich amorphous phase and Nb-nitride precipitates with the size of less than 3 nm. Annealed Fe-Nb-B films have two phases; $\alpha$-Fe grains with the size of about 10 nm and Nb-B rich amorphous phase. The addition of N decreased $\alpha$-Fe grain size due to the precipitation of NbN. The good magnetic properties of the Fe-Nb-B-N film alloys are due to fine $\alpha$-Fe grains resulting from the precipitation of NbN.

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Microstructure evolution and effect on deuterium retention in oxide dispersion strengthened tungsten during He+ irradiation

  • Ding, Xiao-Yu;Xu, Qiu;Zhu, Xiao-yong;Luo, Lai-Ma;Huang, Jian-Jun;Yu, Bin;Gao, Xiang;Li, Jian-Gang;Wu, Yu-Cheng
    • Nuclear Engineering and Technology
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    • v.52 no.12
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    • pp.2860-2866
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    • 2020
  • Oxide dispersion-strengthened materials W-1wt%Pr2O3 and W-1wt%La2O3 were synthesized by wet chemical method and spark plasma sintering. The field emission scanning electron microscopy (FE-SEM) analysis, XRD and Vickers microhardness measurements were conducted to characterize the samples. The irradiations were carried out with a 5 keV helium ion beam to fluences up to 5.0 × 1021 ions/m2 under 600 ℃ using the low-energy ion irradiation system. Transmission electron microscopy (TEM) study was performed to investigate the microstructural evolution in W-1wt%Pr2O3 and W-1wt%La2O3. At 1.0 × 1020 He+/m2, the average loops size of the W-1wt%Pr2O3 was 4.3 nm, much lower than W-1wt% La2O3 of 8.5 nm. However, helium bubbles were not observed throughout in both doped W materials. The effects of pre-irradiation with 1.0 × 1021 He+/m2 on trapping of injected deuterium in doped W was studied by thermal desorption spectrometry (TDS) technique using quadrupole mass spectrometer. Compared with the samples without He+ pre-irradiation, deuterium (D) retention of doped W materials increased after He+ irradiation, whose retention was unsaturated at the damage level of 1.0 × 1022D2+/m2. The present results implied that irradiation effect of He+ ions must be taken into account to evaluate the deuterium retention in fusion material applications.

Microstructural Characterization of Clad Interface in Welds of Ni-Cr-Mo High Strength Low Alloy Steel (Ni-Cr-Mo계 고강도 저합금강 용접클래드 계면의 미세조직 특성 평가)

  • Kim, Hong-Eun;Lee, Ki-Hyoung;Kim, Min-Chul;Lee, Ho-Jin;Kim, Keong-Ho;Lee, Chang-Hee
    • Korean Journal of Metals and Materials
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    • v.49 no.8
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    • pp.628-634
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    • 2011
  • SA508 Gr.4N Ni-Cr-Mo low alloy steel, in which Ni and Cr contents are higher than in commercial SA508 Gr.3 Mn-Mo-Ni low alloy steels, may be a candidate reactor pressure vessel (RPV) material with higher strength and toughness from its tempered martensitic microstructure. The inner surface of the RPV is weld-cladded with stainless steels to prevent corrosion. The goal of this study is to evaluate the microstructural properties of the clad interface between Ni-Cr-Mo low alloy steel and stainless weldment, and the effects of post weld heat treatment (PWHT) on the properties. The properties of the clad interface were compared with those of commercial Mn-Mo-Ni low alloy steel. Multi-layer welding of model alloys with ER308L and ER309L stainless steel by the SAW method was performed, and then PWHT was conducted at $610^{\circ}C$ for 30 h. The microstructural changes of the clad interface were analyzed using OM, SEM and TEM, and micro-Vickers hardness tests were performed. Before PWHT, the heat affected zone (HAZ) showed higher hardness than base and weld metals due to formation of martensite after welding in both steels. In addition, the hardness of the HAZ in Ni-Cr-Mo low alloy steel was higher than that in Mn-Mo-Ni low alloy steel due to a comparatively high martensite fraction. The hardness of the HAZ decreased after PWHT in both steels, but the dark region was formed near the fusion line in which the hardness was locally high. In the case of Mn-Mo-Ni low alloy steel, formation of fine Cr-carbides in the weld region near the fusion line by diffusion of C from the base metal resulted in locally high hardness in the dark region. However, the precipitates of the region in the Ni-Cr-Mo low alloy steel were similar to that in the base metal, and the hardness in the region was not greatly different from that in the base metal.

Decomposition Behavior of Secondary Solidification Phase During Heat Treatment of Squeeze Cast Al-Cu-Si-Mg (용탕단조 Al-Cu-Si-Mg합금의 열처리시 제2응고상의 분해거동)

  • Kim, Yu-Chan;Kim, Do-Hyang;Han, Yo-Sub;Lee, Ho-In
    • Journal of Korea Foundry Society
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    • v.17 no.6
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    • pp.560-568
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    • 1997
  • The dissolution behavior of secondary solidification phases in squeeze cast Al-3.9wt%Cu-1.5wt%Si-1.0wt%Mg has been studied using a combination of optical microscope, image analyzer, scanning electron microscope(SEM), energy dispersive spectrometer(EDS), X-ray diffractometer(XRD) and differential thermal analyzer (DTA). Special emphasis was placed on the investigation of the effects of the nonequilibrium heat treatment on the dissolution of the second solidification phases. Ascast microstructure consisted of primary solidification product of ${\alpha}-Al$ and secondary solidification products of $Al_2Cu$, $Mg_2Si$ and $Al_2CuMg$. Equilibrium and non-equilibrium solution treatments were carried out at the temperatures of $495^{\circ}C$, $502^{\circ}C$ and $515^{\circ}C$ for 3 to 5 hours. The amount of the dissolved secondary phases increased with increasing solution treatment temperature, for example, area fractions of $Al_2Cu$, $Mg_2Si$ and $Al_2CuMg$ were approximately 0%, 1.6% and 4.2% after solution treatment at $495^{\circ}C$ for 5hours, and were approximately 0%, 0.36% and 2% after solution treatment at $515^{\circ}C$ for 5hours. The best combination of tensile properties was obtained when the as-cast alloy was solution treated at $515^{\circ}C$ for 3hours followed by aging at $180^{\circ}C$ for 10 hours. Detailed DTA and TEM study showed that the strengthening behavior during aging was due to enhanced precipitation of the platelet type fine ${\theta}'$ phase.

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