• Title/Summary/Keyword: Film cracks

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Characterization of the UV Oxidation of Raw Natural Rubber Thin Film Using Image and FT-IR Analysis

  • Kim, Ik-Sik;Lee, Bok-Won;Sohn, Kyung-Suk;Yoon, Joohoe;Lee, Jung-Hun
    • Elastomers and Composites
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    • v.51 no.1
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    • pp.1-9
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    • 2016
  • Characterization of the UV oxidation for raw natural rubber (NR) was investigated in controlled conditions through image and FT-IR analysis. The UV oxidation was performed on a thin film of natural rubber coated on a KBr window at 254 nm and room temperature to exclude the thermal oxidation. Before or after exposure to UV light, image of the NR thin film was observed at a right or tilted angle. FT-IR absorption spectra were measured in transmission mode with the UV irradiation time. The UV oxidation of NR was examined by the changes of absorption peaks at 3425, 1717, 1084, 1477, 1377, and $833cm^{-1}$ which were assigned to hydroxyl group (-OH), carbonyl group (-C=O), carbon-oxygen bond (-C-O), methylene group $(-CH_2-)$, methyl group $(-CH_3)$, and cis-methine group $(cis-CCH_3=CH-)$, respectively. During the initial exposure period, the results indicated that the appearance of carbonyl group was directly related to the reduction of cis-methine group containing carbon-carbon double bond (-C=C-). Most of aldehydes or ketones from carbon-carbon double bonds were formed very fast by chain scission. A lot of long wide cracks with one orientation at regular intervals which resulted in consecutive chain scission were observed by image analysis. During all exposure periods, on the other hand, it was considered that the continuous increment of hydroxyl and carbonyl group was closely related to the decrement of methylene and methyl group in the allylic position. Therefore, two possible mechanisms for the UV oxidation of NR were suggested.

Characterization on the Thermal Oxidation of Raw Natural Rubber Thin Film using Image and FT-IR Analysis

  • Kim, Ik-Sik;Cho, Hwanjeong;Sohn, Kyung-Suk;Choi, Hwa-Soon;Kim, Sung-Uk;Kim, Sinkon
    • Elastomers and Composites
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    • v.55 no.1
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    • pp.51-58
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    • 2020
  • In this study, the thermal oxidation of raw natural rubber (NR) was investigated under controlled conditions by optical image and fourier transform infrared (FT-IR) analysis. The thermal oxidation was performed on a transparent thin film of raw NR coated on a KBr window in a dark chamber at 80℃ under low humidity conditions to completely exclude moisture and restrict light oxidation. Images of the thin film of raw NR were obtained before and after thermal oxidation. FT-IR absorption spectra were measured in the transmission mode at different thermal exposure times. The thermal oxidation of NR was examined by the changes in the absorption peaks at 3449, 1736, 1447, 1377, 1242, 1072, and 833 cm-1, which corresponded to a hydroxyl group (-OH), a carbonyl group (-C=O) from an aldehyde and a ketone, a methylene group (-CH2-), a methyl group (-CH3), a carbon-oxygen single bond (-C-O) from an epoxide, a carbon-oxygen bond (-C-O) from an ether, an alcohol, a peroxide, or a cyclic peroxide, and a cis-methine group (cis-CCH3=CH-), respectively. In the initial stage of thermal oxidation, two different types of free radicals were produced quickly and randomly by the homolytic cleavage of a double bond and allylic hydrogen abstraction. Aldehydes and ketones were formed from chain scissions of the double bonds and alcohols were produced from allylic hydrogen abstraction at the methylene or methyl groups. Two reactions seemed to proceed competitively with each other. At a later stage, oxidative crosslinks seemed to dominate through the combination of free radicals such as an allyl radical (CH=CHCH2·), alkoxy radical (RO·), and peroxy radical (ROO·) and the reaction of a hydroperoxide (-ROOH) with a double bond. The image obtained after thermal oxidation showed hardening without cracks. Based on these observations, a plausible two-step mechanism was suggested for chain hardening caused by the thermal oxidation.

A STUDY ON THE RELATIONSHIP BETWEEN PLASMA CHARACTERISTICS AND FILM PROPERTIES FOR MgO BY PULSED DC MAGNETRON SPUTTERING

  • Nam, Kyung H.;Chung, Yun M.;Han, Jeon G.
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2001.11a
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    • pp.35-35
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    • 2001
  • agnesium Oxide (MgO) with a NaCI structure is well known to exhibit high secondary electron emission, excellent high temperature chemical stability, high thermal conductance and electrical insulating properties. For these reason MgO films have been widely used for a buffer layer of high $T_c$ superconducting and a protective layer for AC-plasma display panels to improve discharge characteristics and panel lifetime. Up to now MgO films have been synthesized by lE-beam evaporation, Molecular Beam Epitaxy (MBE) and Metalorganic Chemical Vapor Deposition (MOCVD), however there have been some limitations such as low film density and micro-cracks in films. Therefore magnetron sputtering process were emerged as predominant method to synthesis high density MgO films. In previous works, we designed and manufactured unbalanced magnetron source with high power density for the deposition of high quality MgO films. The magnetron discharges were sustained at the pressure of O.lmtorr with power density of $110W/\textrm{cm}^2$ and the maximum deposition rate was measured at $2.8\mu\textrm{m}/min$ for Cu films. In this study, the syntheses of MgO films were carried out by unbalanced magnetron sputtering with various $O_2$ partial pressure and specially target power densities, duty cycles and frequency using pulsed DC power supply. And also we investigated the plasma states with various $O_2$ partial pressure and pulsed DC conditions by Optical Emission Spectroscopy (OES). In order to confirm the relationships between plasma states and film properties such as microstructure and secondary electron emission coefficient were analyzed by X-Ray Diffraction(XRD), Transmission Electron Microscopy(TEM) and ${\gamma}-Focused$ Ion Beam (${\gamma}-FIB$).

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Effects of NaOH Concentration on the Structure of PEO Films Formed on AZ31 Mg Alloy in PO43- and SiO32- Containing Aqueous Solution (인산 및 규산 이온이 포함된 수용액에서 AZ31 마그네슘 합금의 플라즈마 전해산화 피막의 구조에 미치는 수산화나트륨 농도의 영향)

  • Kwon, Duyoung;Moon, Sungmo
    • Journal of the Korean institute of surface engineering
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    • v.49 no.1
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    • pp.46-53
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    • 2016
  • The structure of plasma electrolytic oxidation (PEO) coatings was investigated as a function of NaOH concentration in 0.06 M $Na_2SiO_3$ + 0.06 M $Na_3PO_4$ solution by using SEM and epoxy replica method. The PEO film was formed on AZ31 Mg alloy by the application of anodic pulse current with 0.2 ms width and its formation behavior was studied by voltage-time curves during the formation of PEO films. It was found that the addition of NaOH into $PO_4{^{3-}}$ and $SiO_3{^{2-}}$ containing aqueous solution causes a decrease in the PEO film formation voltage, suggesting that dielectric breakdown of the PEO becomes easier with increasing $OH^-$ ion concentration in the solution. With increasing $OH^-$ ion concentration, thickness of the PEO film increased and surface roughness decreased. The size of pores formed in the PEO layer became smaller and the number of cracks in the PEO layer increased with increasing $OH^-$ ion concentration. Based on the experimental results obtained in the work, it is suggested that $OH^-$ ions in the solution can contribute not only to the dielectric breakdown but also to the formation of PEO films in the presence of $PO_4{^{3-}}$ and $SiO_3{^{2-}}$ ions in the solution.

Fabrication and Characterization of Polycrystalline Mereuric Iodide Films using Particle-in-Binder Methods (Particle-in-Binder(PIB) 법을 이용한 다결정 $HgI_2$ 필름 제작 및 특성 연구)

  • Cha, Byung-Youl;Cho, Sung-Ho;Kim, So-Yeong;Woon, Min-Seuk;Nam, Sang-Hee
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.330-330
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    • 2007
  • Polycrystalline mercuric iodide $HgI_2$) films are being developed as a new detector technology for digital x-ray imaging. The $HgI_2$ is generally vacuum deposited by physical vapor deposition (PVD) process. But the PVD thick deposition has been caused any instability in the biasing due to any defects or cracks. In this work we present a new particle-in-binder (PIB) methodologies used for the $HgI_2$ thick films. These growth techniques can be easily extended to produce much larger film areas. This paper, for the first time, presents results and comparison of polycrystalline $HgI_2$ films derived by various PIB methods. We investigated the structural and morphological properties of the films using X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. The films were characterized with respect to their electrical properties and in response to x-ray photons. Physical and electrical results were also compared between conventional polycrystalline PVD and our detectors. Leakage current as low as $350\;pA/cm^2$ at the bias voltage of ~ 200 V has been observed. And high sensitivity and good linearity in the response to x-rays was obtained in the film derived by PIB sedimentation method. Our future efforts will concentrate on optimization of film growth techniques for uniform large area deposition on image readout arrays.

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Ce:YAG remote phosphor coating for white LED with silica sol binder (Silica sol 바인더를 적용한 백색 LED용 Ce:YAG remote 형광체 코팅)

  • Gim, Su Jin;Park, Ha Na;Choi, Jae Ho;Jung, Yoon Sung;Kim, Hyeong-Jun
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.5
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    • pp.212-217
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    • 2021
  • The applicability of the white LED from the blue LED of the coating film as a binder for surface and curved coatings were confirmed. The particle size of YAG is D50: 9~10 ㎛, and the crystal structure is garnet (Y3Al5O12), cubic. The coating film had no cracks, at the same time, the silica sol was uniformly coated with YAG phosphor, and the YAG content and thickness in the coating film showed a tendency to increase up to 40 ㎛ in proportion to the increase in the amount added. Furthermore, as the YAG content increased, the PL emission intensity increased and the color coordinate shift toward the end of the chromatic locus curve was confirmed.

Characterization on the Ozone Oxidation of Raw Natural Rubber Thin Film using Image and FT-IR Analysis

  • Kim, Ik-Sik;Lee, DooYoul;Sohn, Kyung-Suk;Lee, Jung-Hun;Bae, JoongWoo
    • Elastomers and Composites
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    • v.54 no.2
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    • pp.110-117
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    • 2019
  • The characterization of the ozone oxidation for raw natural rubber (NR) was investigated under controlled conditions through image and fourier transform infrared (FT-IR) analysis. The ozone oxidation was performed on a transparent thin film of raw NR coated on a KBr window in a dark chamber at $40^{\circ}C$ under low humidity conditions to completely exclude thermal, moisture, or light oxidation. The ozone concentration was set at 40 parts per hundred million (pphm). Before or after exposure to ozone, the image of the thin film for raw NR was observed at a right or tilted angle. FT-IR absorption spectra were measured in the transmission mode according to ozone exposure time. The ozone oxidation of NR was determined by the changes in the absorption peaks at 1736, 1715, 1697, and $833cm^{-1}$, which were assigned to an aldehyde group (-CHO), a ketone group (-COR), an inter-hydrogen bond between carbonyl group (-C=O) from an aldehyde or a ketone and an amide group (-CONH-) of protein, and a cis-methine group ($is-CCH_3=CH-$, respectively. During ozone exposure period, the results indicated that the formation of the carbonyl group of aldehyde or ketone was directly related to the decrement of the double bond of cis-1,4-polyisoprene. Only carbonyl compounds such as aldehydes or ketones seemed to be formed through chain scission by ozone. Long thin cracks with one orientation at regular intervals, which resulted in consecutive chain scission, were observed by image analysis. Therefore, one possible two-step mechanism for the formation of aldehyde and ketone was suggested.

Surface Engineering of GaN Photoelectrode by NH3 Treatment for Solar Water Oxidation

  • Soon Hyung Kang;Jun-Seok Ha
    • Journal of Electrochemical Science and Technology
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    • v.14 no.4
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    • pp.388-396
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    • 2023
  • Photoelectrochemical (PEC) water splitting is a vital source of clean and sustainable hydrogen energy. Moreover, the large-scale H2 production is currently necessary, while long-term stability and high PEC activity still remain important issues. In this study, a GaN-based photoelectrode was modified by an additional NH3 treatment (900℃ for 10 min) and its PEC behavior was monitored. The bare GaN exhibited a highly crystalline wurtzite structure with the (002) plane and the optical bandgap was approximately 3.2 eV. In comparison, the NH3-treated GaN film exhibited slightly reduced crystallinity and a small improvement in light absorption, resulting from the lattice stress or cracks induced by the excessive N supply. The minor surface nanotexturing created more surface area, providing electroactive reacting sites. From the surface XPS analysis, the formation of an N-Ga-O phase on the surface region of the GaN film was confirmed, which suppressed the charge recombination process and the positive shift of EFB. Therefore, these effects boosted the PEC activity of the NH3-treated GaN film, with J values of approximately 0.35 and 0.78 mA·cm-2 at 0.0 and 1.23 VRHE, respectively, and an onset potential (Von) of -0.24 VRHE. In addition, there was an approximate 50% improvement in the J value within the highly applied potential region with a positive shift of Von. This result could be explained by the increased nanotexturing on the surface structure, the newly formed defect/trap states correlated to the positive Von shift, and the formation of a GaOxN1-x phase, which partially blocked the charge recombination reaction.

Wear Characteristics of TiN Coating by Plasma Enhanced CVD (PECVD에 의한 TiN 코팅의 마모특성 연구)

  • Song, Kun;Ahn, Hyo-Sok
    • Tribology and Lubricants
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    • v.6 no.1
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    • pp.116-125
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    • 1990
  • An experimental programme was established to determine the wear behaviour of TiN coatings of thickness 1 $\mu$m and 3 $\mu$m. by PECVD with the variation of applied load, sliding velocity and sliding distance. It was shown that oxidation of transferred metal as sliding speed increased formed oxide film so that it contributed in decreasing the wear rate. With the roller-on-disc tribometer employed, the wear rate of the roller specimen was decreased with the increase in sliding distance due to the reduction in effective contact pressure. Finally, the severe cracks concentrated at the trailing edge of contact surface were explained in terms of high tensile stress prevailing at the trailing edge of the contact and were identified as a dominant wear mechanism as well as the strong local welding between coating layer and the counter surface, leading to the debonding of the coating layer.

The Behavior of TiN Thin Film Growth According to Substrate Surface Conditions in PECVD Process (모재표면오건에 따른 TiN 박막의 Morphology변화)

  • 노경준;이정일
    • Korean Journal of Crystallography
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    • v.3 no.1
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    • pp.53-66
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    • 1992
  • Extensive research has been perform성 on the property-microstructure-process condition relations of thin films. The various proposed models are mainly based on physical vapor deposition processes. Especially the study on the surface condition of substrates in Zone 1 with low surface mobility has not been sufficient. In this study, therefore, we discussed the mochological changes of TiN films deposited by plusma enhanced chemical vapor deposition process with substrates of different composition and micro-rorghness, and compared it with the Structure Zone Model. We could find out that the growth rate of films increased and micro-grain size decreased with the increase in micro-roughness, but it does not improve the mechanical properties because of many imperfections like voids, micro-cracks, stacking faults, etc. This means that, in these deposition conditions, the increase in shadowing diffect is more effective than the increase in nucleation sites on the growth of films due to the increase in substrate roughness.

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