• Title/Summary/Keyword: Thermal microscopy

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An in Depth Study of Crystallinity, Crystallite Size and Orientation Measurements of a Selection of Poly(Ethylene Terephthalate) Fibers

  • Karacan Ismail
    • Fibers and Polymers
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    • v.6 no.3
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    • pp.186-199
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    • 2005
  • A selection of commercially available poly(ethy1ene terephtha1ate) fibers with different degrees of molecular alignment and crystallinity have been investigated utilizing a wide range of techniques including optical microscopy, infrared spectroscopy together with thermal and wide-angle X-ray diffraction techniques. Annealing experiments showed increased molecular alignment and crystallinity as shown by the increased values of birefringence and melting enthalpies. Crystallinity values determined from thermal analysis, density, unpolarized infrared spectroscopy and X-ray diffraction are compared and discussed in terms of the inherent capabilities and limitations of each measurement technique. The birefringence and refractive index values obtained from optical microscopy are found to decrease with increasing wavelength of light used in the experiments. The wide-angle X-ray diffraction analysis shows that the samples with relatively low orientation possess oriented non-crystalline array of chains whereas those with high molecular orientation possess well defined and oriented crystalline array of chains along the fiber axis direction. X-ray analysis showed increasing crystallite size trend with increasing molecular orientation. SEM images showed micro-cracks on low oriented fiber surfaces becoming smooth on highly oriented fiber surfaces. Excellent bending characteristics were observed with knotted fibers implying relatively easy fabric formation.

Effect of Ammonia on Alignment of Carbon Nanotubes in Thermal Chemical Vapor Deposition (촉매 금속을 이용한 열화학 기상 증착법에서 탄소 나노튜브의 수직배향 합성에 대한 암모니아의 역할)

  • Hong, Sang-Yeong;Jo, Yu-Seok;Choe, Gyu-Seok;Kim, Do-Jin;Kim, Hyo-Jin
    • Korean Journal of Materials Research
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    • v.11 no.8
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    • pp.697-702
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    • 2001
  • Effects of ammonia treatment on the morphologies of the catalytic metal films and carbon nanotubes subsequently synthesized via a thermal chemical vapor deposition method were investigated. An optimally controlled thermo-chemical process of ammonia treatment gave rise to a morphology of a dense distribution of vertically aligned carbon nanotubes. $NH_3$ treatment is a crucial key process to obtain vertically aligned carbon nanotubes. However, it was realized by a simple $NH_3$ treatment during synthesis at temperatures of $800-900^{\circ}C$ without any extra process. The structure and morphology of carbon nanotubes were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy.

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Growth characteristics of 4H-SiC homoepitaxial layers grown by thermal CVD (화학기상증착법으로 성장시킨 4H-SiC 동종박막의 성장 특성)

  • Jang, Seong-Joo;Jeong, Moon-Taeg;Seol, Woon-Hag;Park, Ju-Hoon
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1999.06a
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    • pp.271-284
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    • 1999
  • As a semiconductor material for electronic devices operated under extreme environmental conditions, silicon carbides (SiCs) have been intensively studied because of their excellent electrical, thermal and other physical properties. The growth characteristics of single-crystalline 4H-SiC homoepitaxial layers grown by a thermal chemical vapor deposition (CVD) were investigated. Especially, the successful growth condition of 4H-SiC homoepitaxial layers using a SiC-uncoated graphite susceptor that utilized Mo-plates was obtained. The CVD growth was performed in an RF-induction heated atmospheric pressure chamber and carried out using off-oriented substrates prepared by a modified Lely method. In order to investigate the crystallinity of grown epilayers, Nomarski optical microscopy, Raman spectroscopy, photoluminescence(PL), scanning electron microscopy (SEM) and other techniques were utilized. The best quality of 4H-SiC homoepitaxial layers was observed in conditions of growth temperature 1500$^{\circ}C$ and C/Si flow ratio 2.0 of C3H3 0.2sccm & SiH4 0.3sccm. The growth rate of epilayers was about 1.0$\mu\textrm{m}$/h in the above growth condition.

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Effect of Contact Stiffness on Lateral Force Calibration of Atomic Force Microscopy Cantilever (원자 현미경 탐침의 수평방향 힘 교정에 미치는 접촉 강성의 영향)

  • Tran, Da Khoa;Jeon, Ki-Joon;Chung, Koo-Hyun
    • Tribology and Lubricants
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    • v.28 no.6
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    • pp.289-296
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    • 2012
  • Atomic force microscopy (AFM) has been used for imaging surfaces and measuring surface forces at the nano-scale. Force calibration is important for the quantitative measurement of forces at the nano-scale using AFM. Normal force calibration is relatively straightforward, whereas the lateral force calibration is more complicated since the lateral stiffness of the cantilever is often comparable to the contact stiffness. In this work, the lateral force calibrations of the rectangular cantilever were performed using torsional Sader's method, thermal noise method, and wedge calibration method. The lateral optical lever sensitivity for the thermal noise method was determined from the friction loop under various normal forces as well. Experimental results showed that the discrepancies among the results of the different methods were as large as 30% due to the effect of the contact stiffness on the lateral force calibration of the cantilever used in this work. After correction for the effect of contact stiffness, all the calibration results agreed with each other, within experimental uncertainties.

Synthesis of TiO2 Nanowires by Thermal Oxidation of Titanium Alloy Powder (타이타늄 합금 분말의 열적산화를 통한 TiO2 나노와이어의 합성)

  • Kim, Yoo-Young;Cho, Kwon-Koo
    • Journal of Powder Materials
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    • v.25 no.1
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    • pp.48-53
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    • 2018
  • One-dimensional rutile $TiO_2$ is an important inorganic compound with applicability in sensors, solar cells, and Li-based batteries. However, conventional synthesis methods for $TiO_2$ nanowires are complicated and entail risks of environmental contamination. In this work, we report the growth of $TiO_2$ nanowires on a Ti alloy powder (Ti-6wt%Al-4wt%V, Ti64) using simple thermal oxidation under a limited supply of $O_2$. The optimum condition for $TiO_2$ nanowire synthesis is studied for variables including temperature, time, and pressure. $TiO_2$ nanowires of ${\sim}5{\mu}m$ in length and 100 nm in thickness are richly synthesized under the optimum condition with single-crystalline rutile phases. The formation of $TiO_2$ nanowires is greatly influenced by synthesis temperature and pressure. The synthesized $TiO_2$ nanowires are characterized using field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HR-TEM).

Growth characteristics of 4H-SiC homoepitaxial layers grown by thermal CVD

  • Jang, Seong-Joo;Jeong, Moon-Taeg;Seol, Woon-Hag;Park, Ju-Hoon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.3
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    • pp.303-308
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    • 1999
  • As a semiconductor material for electronic devices operated under extreme environmental conditions, silicon carbides(SiCs) have been intensively studied because of their excellent electrical, thermal and other physical properties. The growth characteristics of single-crystalline 4H-SiC homoepitaxial layers grown by a thermal chemical vapor deposition (CVD) were investigated. Especially, the successful growth condition of 4H-SiC homoepitaxial layers using a SiC-uncoated atmospheric pressure chamber and carried out using off-oriented substrates prepared by a modified Lely method. In order to investigate the crystallinity of grown epilayers, Nomarski optical microscopy, Raman spectroscopy, photoluninescence(PL), scanning electron microscopy(SEM) and other techniques were utilized. The best quality of 4H-SiC homoepitaxial layers was observed in conditions of growth temperature $1500^{\circ}C$ and C/Si flow ratio 2.0 of $C_{3}H_{8}\;0.2\;sccm\;&\;SiH_{4}\;0.3\;sccm$. The growth rate of epilayers was about $1.0\mu\textrm{m}/h$ in the above growth condition.

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γ-ray Radiation Induced Synthesis and Characterization of α-Cobalt Hydroxide Nanoparticles

  • Kim, Sang-Wook;Kwon, Bob-Jin;Park, Jeong-Hoon;Hur, Min-Goo;Yang, Seung-Dae;Jung, Hyun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.910-914
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    • 2010
  • A novel synthetic route has been developed to prepare $\alpha$-cobalt hydroxide with intercalated nitrate anions. It was successfully synthesized by $\gamma$-ray irradiation under simple conditions, i.e., air atmosphere, without base. Under $\gamma$-ray irradiation, it leads to the formation of layered cobalt hydroxynitrate compounds which have small crystalline size and have the role of a generator of hydroxyl anion. Structural and morphological characterizations were performed by using power X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high resolution transmission electron microscopy (HR-TEM). The component and thermal stability of the sample were respectively measured by Fourier transform infrared (FT-IR) spectroscopy, elemental analysis, and thermal analyses, including thermogravimetry (TG) and differential thermal analysis (DTA).

Effects of rapid thermal annealing and bias sputtering on the structure and properties of ZnO:Al films deposited by DC magnetron sputtering (Bias를 인가한 DC magnetron sputtering 법으로 증착된 ZnO:Al 박막의 구조적 특성과 RTP의 annealing에 따른 영향)

  • Park, Kyeong-Seok;Lee, Kyu-Seok;Lee, Sung-Wook;Park, Min-Woo;Kwak, Dong-Joo;Lim, Dong-Gun
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2005.07a
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    • pp.500-501
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    • 2005
  • Aluminum doped zinc oxide films (ZnO:Al) were deposited on glass substrate by DC magnetron sputtering from a ZnO target mixed with 2 wt% $Al_2O_3$. The effects of substrate bias on the electrical properties and film structure were studied. Films deposited with positive bias have been annealed at $600^{\circ}C$ using rapid thermal anneal (RTA) process. The effects of RTA on the evolution of film microstructure are to be also studied using X-ray diffraction, transmission electron microscopy, and atomic force microscopy. Positive bias sputtering may induce lattice defects caused by electron bombardments during deposition. The as-deposited film microstructure evolves from the film with high defect density to more stable film condition. The electrical properties of the films after RTA process were also studied and the results were correlated with the evolution of film microstructures.

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Types and Yields of Carbon Nanotubes Synthesized Depending on Catalyst Pretreatment

  • Go, Jae-Seong;Lee, Nae-Seong
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.17.2-17.2
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    • 2011
  • Double-walled carbon nanotubes (DWCNTs) were grown with vertical alignment on a Si wafer by using catalytic thermal chemical vapor deposition. This study investigated the effect of pre-annealing time of catalyst on the types of CNTs grown on the substrate. The catalyst layer is usually evolved into discretely distributed nanoparticles during the annealing and initial growth of CNTs. The 0.5-nm-thick Fe served as a catalyst, underneath which Al was coated as a catalyst support as well as a diffusion barrier on the Si substrate. Both the catalyst and support layers were coated by using thermal evaporation. CNTs were synthesized for 10 min by flowing 60 sccm of Ar and 60 sccm of H2 as a carrier gas and 20 sccm of C2H2 as a feedstock at 95 torr and $750^{\circ}C$. In this study, the catalyst and support layers were subject to annealing for 0~420 sec. As-grown CNTs were characterized by using field emission scanning electron microscopy, high resolution transmission electron microscopy, Raman spectroscopy, and atomic force microscopy. The annealing for 90~300 sec caused the growth of DWCNTs as high as ~670 ${\mu}m$ for 10 min while below 90 sec and over 420 sec 300~830 ${\mu}m$-thick triple and multiwalled CNTs occurred, respectively. Several radial breathing mode (RBM) peaks in the Raman spectra were observed at the Raman shifts of 112~191 cm-1, implying the presence of DWCNTs, TWCNTs, MWCNTs with the tube diameters 3.4, 4.0, 6.5 nm, respectively. The maximum ratio of DWCNTs was observed to be ~85% at the annealing time of 180 sec. The Raman spectra of the as-grown DWCNTs showed low G/D peak intensity ratios, indicating their low defect concentrations. As increasing the annealing time, the catalyst layer seemed to be granulated, and then grown to particles with larger sizes but fewer numbers by Ostwald ripening.

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Response of Metastatic Cancer Cells to Thermal Changes in vitro (배양온도 변화에 대한 전이성 암세포의 반응)

  • Ahn, San-Gil;Kwon, Young-Ee;Choi, Ho-Soon;Kwon, Jung-Kyun;Yoo, Jin-Young;Kim, Jong-Ryong;Kim, Won-Kyu
    • Applied Microscopy
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    • v.37 no.4
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    • pp.239-248
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    • 2007
  • Alteration of temperature is one of cancer therapies. In general, severe hyperthermia(around $43^{\circ}C$) and hypothermia(around $18^{\circ}C$) trigger apoptosis through mitochondria, though the specific mechanism is still unknown. CC-t6 and GB-d1 cell lines, which were originally derived from human cholangiocarcinoma and gall bladder cancer, were established from a metastatic lymph node. To investigate the mechanism of metastatic cancer cell response to thermal stresses, hyperthermia($37^{\circ}C{\rightarrow}43^{\circ}C$) and hypothermia($37^{\circ}C{\rightarrow}17.4^{\circ}C$) were designed. Thermal stresses did not induce apoptosis but necrotic cell death. Any alterations of caspase-3, -9, cytochrome c, Bax, and Bcl-2 were not found in both hyperthermia and hypothermia exposed fells using western blot analysis. In the transmission electron microscopy, typical necrotic, but not apoptotic, changes were observed. These results suggest that temperature changes induce cell death through necrotic pathway in metastatic cancer in vitro, and it can be one of effective anticancer methods.