• Title/Summary/Keyword: SEM and EDS

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Colloidal Synthesis of Octahedral Shaped PbSe Nanocrystals from Lead Oleate and Se : Temperature Effect

  • Gokarna, Anisha;Jun, Ki-Won;Khanna, P.K.;Baeg, Jin-Ook;Seok, Sang-Il
    • Bulletin of the Korean Chemical Society
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    • v.26 no.11
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    • pp.1803-1806
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    • 2005
  • Formation of octahedral shaped PbSe quantum dots at higher synthesis temperature is being reported in this paper. The synthesis includes the reaction between lead oleate and trioctylphosphine selenide under inert gas conditions to produce PbSe. TEM, SEM, XRD and EDS were used to characterize the samples. The SEM exhibited the formation of spherical shaped nanocrystals at temperature below 140 ${^{\circ}C}$ and octahedral shaped nanoparticles at higher temperatures. Moreover, the TEM also showed the well resolved (111) lattice fringes proving that the nanocrystals were crystalline in nature. Synthesis of highly pure PbSe nanocrystals was another interesting aspect of this research.

The Effects of Surface Pretreatments on Adhesion Strength of TiN Films by DC Magnetron Sputtering (표면전처리가 반응성 스퍼터링법으로 제조한 TiN 코팅층의 밀착력에 미치는 영향)

  • 김흥윤;백운승;권식철;김규호
    • Journal of the Korean institute of surface engineering
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    • v.26 no.5
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    • pp.225-234
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    • 1993
  • Titanium nitride coatings were deposited onto SUS304 stainless steel substrates pretreated by mechanical scrubbing, chemical etching at 50% HCl solution and Ar ion etching. Adhesion strength were measured by scratch tester and confirmed by SEM with EDS. Adhesion strength of Ar ion etched substrate was 10 to 15 times higher than that of mechanical scrubbed or chemical etched substrate. Ar ion etching brought about an uniform and fine spherical shaped surface, while chemical etching gave rise to a rough and irregular surface on SEM micrograph. It was suggested that higher adhesion strength might be caused by anchoring effect of Ar ion etched surface prior to TiN deposition.

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Evaluation of the effects of two novel irrigants on intraradicular dentine erosion, debris and smear layer removal

  • Gorduysus, Melahat;Kucukkaya, Selen;Bayramgil, Nursel Pekel;Gorduysus, Mehmet Omer
    • Restorative Dentistry and Endodontics
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    • v.40 no.3
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    • pp.216-222
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    • 2015
  • Objectives: To evaluate the effects of copolymer of acrylic acid and maleic acid (Poly[AA-co-MA]) and calcium hypochlorite ($Ca(OCl)_2$) on root canal dentin using scanning electron microscope (SEM). Materials and Methods: Twenty-four single-rooted teeth were instrumented and the apical and coronal thirds of each root were removed, leaving the 5 mm middle thirds, which were then separated into two pieces longitudinally. The specimens were randomly divided into six groups and subjected to each irrigant for 5 min as follows: G1, $Ca(OCl)_2$; G2, Poly(AA-co-MA); G3, $Ca(OCl)_2$ + Poly(AA-co-MA); G4, sodium hypochlorite (NaOCl); G5, ethylenediaminetetraacetic acid (EDTA); G6, NaOCl+EDTA. The specimens were prepared for SEM evaluation. Smear layer, debris and erosion scores were recorded by two blinded examiners. One image from G3 was analyzed with energy dispersive spectroscopy (EDS) on suspicion of precipitate formation. Data were analyzed using the Kruskal-Wallis and Dunn tests. Results: G1 and G4 showed the presence of debris and smear layer and they were statistically different from G2, G3, G5 and G6 where debris and smear layer were totally removed (p < 0.05). In G1 and G4, erosion evaluation could not be done because of debris and smear layer. G2, G3 and G5 showed no erosion, and there was no significant difference between them. G6 showed severe erosion and was statistically different from G2, G3 and G5 (p < 0.05). EDS microanalysis showed the presence of Na, P, and Ca elements on the surface. Conclusions: Poly(AA-co-MA) is effective in removing the smear layer and debris without causing erosion either alone or with $Ca(OCl)_2$.

Effect of barium silicate filler content on mechanical properties of resin nanoceramics for additive manufacturing

  • Won, Sun;Ko, Kyung-Ho;Park, Chan-Jin;Cho, Lee-Ra;Huh, Yoon-Hyuk
    • The Journal of Advanced Prosthodontics
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    • v.14 no.5
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    • pp.315-323
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    • 2022
  • PURPOSE. The purpose of this study was to investigate the effect of barium silicate filler contents on mechanical properties of resin nanoceramics (RNCs) for additive manufacturing (AM). MATERIALS AND METHODS. Additively manufactured RNC specimens were divided into 4 groups depending on the content of ceramic fillers and polymers: 0% barium silicate and 100% polymer (B0/P10, control group); 50% barium silicate and 50% polymer (B5/P5); 60% barium silicate and 40% polymer (B6/P4); 67% barium silicate and 33% polymer (B6.7/P3.3). The compressive strength (n = 15) and fracture toughness (n = 12) of the specimens were measured, and scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) analyses were performed. Independent sample Kruskal-Wallis tests were performed on the compressive strength and fracture toughness test results, and the significance of each group was analyzed at the 95% confidence interval through post-tests using the Bonferroni's method. RESULTS. B6/P4 and B6.7/P3.3 exhibited much higher yield strength than B0/P10 and B5/P5 (P < .05). Compared to the control group (B0/P10), the other three groups exhibited higher ultimate strength (P < .05). The fracture toughness of B6/P4 and B6.7/P3.3 were similar (P > .05). The content of barium silicate and fracture toughness showed a positive correlation coefficient (R = 0.582). SEM and EDS analyses revealed the presence of an oval-shaped ceramic aggregate in B6/P4 specimens, whereas the ceramic filler and polymer substrate were homogeneously mixed in B6.7/P3.3. CONCLUSION. Increasing the ceramic filler content improves the mechanical properties, but it can be accompanied by a decrease in the flowability and the homogeneity of the slurry.

Effect of accelerators with waste material on the properties of cement paste and mortar

  • Devi, Kiran;Saini, Babita;Aggarwal, Paratibha
    • Computers and Concrete
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    • v.22 no.2
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    • pp.153-159
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    • 2018
  • Accelerators are used to speed up the construction by accelerating the setting time which helps in early removal of formwork thus leading to faster construction rate. Admixtures are used in mortar and concrete during or after mixing to improve certain properties of material which cannot be achieved in conventional cement mortar and concrete. The various industrial by products make nuisance and are hazardous to ecosystem as well. These wastes can be used in the construction industries to reduce the consumption of cement/aggregates, cost; and save the energy and environment by utilising waste and eliminate their disposal problem as well. The effect of calcium nitrate and triethanolamine (TEA) as accelerators and marble powder (MP) as waste material on the various properties of cement paste and mortar has been studied in the present work. The replacement ratio of MP was 0-10% @ 2.5% by weight of cement. The addition of calcium nitrate was 0% and 1%; and variation of addition of TEA was 0-0.1@ 0.025% and 0.1-1.0@ 0.1% by weight of cement. On the basis of setting time, some mix proportions were selected and further investigated. Setting time and soundness of cement paste; compressive strength and microstructure of mortar mix of selected mix proportions were studied experimentally at 3, 7 and 28 days aging. Results showed that use of MP, calcium nitrate, TEA and their combination reduced setting time of cement paste for all the mixes. Addition of calcium nitrate increased the compressive strength at all curing ages while MP and TEA decreased the compressive strength. The mechanism of additives was discussed through scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS) analysis of the specimens.

Energy-dispersive X-ray spectroscopic investigation of a fractured non-submerged dental implant associated with abutment fracture

  • Truc Thi Hoang Nguyen;Mi Young Eo;Kezia Rachellea Mustakim;Mi Hyun Seo;Hoon Myoung;Soung Min Kim
    • Journal of the Korean Association of Oral and Maxillofacial Surgeons
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    • v.49 no.1
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    • pp.43-48
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    • 2023
  • The biocompatibility and durability of implant fixtures are major concerns for dentists and patients. Mechanical complications of the implant include abutment screw loosening, screw fracture, loss of implant prostheses, and implant fracture. This case report aims to describe management of a case of fixture damage that occurred after screw fracture in a tissue level, internal connection implant and microscopic evaluation of the fractured fixture. A trephine bur was used to remove the fixture, and the socket was grafted using allogeneic bone material. The failed implant was examined by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS), which revealed a fractured fixture with both normal and irregular bone patterns. The SEM and EDS results give an enlightenment of the failed fixture surface micromorphology with microfracture and contaminated chemical compositions. Noticeably, the significantly high level of gold (Au) on the implant surface and the trace amounts of Au and titanium (Ti) in the bone tissue were recorded, which might have resulted from instability and micro-movement of the implant-abutment connection over an extended period of time. Further study with larger number of patient and different types of implants is needed for further conclusion.

Hydrothermal Pressure Effect over Preparation of MoS2: Catalyst Characterization and Direct Methanation (수열 압력 제조 조건이 MoS2 촉매 특성과 직접 메탄화 반응에 미치는 영향)

  • PARK, JEONGHWAN;KIM, SEONGSOO;KIM, JINGUL
    • Transactions of the Korean hydrogen and new energy society
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    • v.29 no.2
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    • pp.170-180
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    • 2018
  • After $MoS_2$ catalyst was prepared at 1, 30, and 70 atm, the hydrothermal pressure effect over preparation of $MoS_2$ was investigated in terms of catalyst characterization and direct methanation. Multifaceted characterization techniques such as XRD, BET, SEM, TPR, EDS, and XPS were used to analyze and investigate the effect of high pressure over the preparation of surface and bulk $MoS_2$ catalyst. Result from XRD, SEM, and BET demonstrated that $MoS_2$ was more dispersed as preparation pressure was increased, which resulted finer $MoS_2$ crystal size and higher surface area. EDS result confirmed that bulk composition was $MoS_2$ and XPS result showed that S/Mo mole ratio of surface was about 1.3. TPR showed that $MoS_2$ prepared at 30 atm possessed higher active surface sites than $MoS_2$ prepared at 1 atm and these sites could contribute to higher CO yield during methanation. Direct methanation was used to evaluate the CO conversion of the both catalysts prepared at 1 atm and 30 atm and reaction condition was at feed mole ratio of $H_2/CO=1$, GHSV=4800, 30 atm, temperature($^{\circ}C$) of 300, 350, 400, and 450. $MoS_2$ prepared at 30 atm showed more stable and higher CO conversion than $MoS_2$ prepared at 1 atm. Faster deactivation was occurred over $MoS_2$ prepared at 1 atm, which indicated that preparation pressure of $MoS_2$ catalyst was the dominant factor to improve the yield of direct methanation.

Analysis of Polymeric Insulators Exposed to In-service Conditions (실 포설 환경에 노출된 송전용 고분자애자의 평가)

  • Lee, Sang-Jin;Youn, Bok-Hee;Bai, Kyoung-Moo;Jeon, Seung-Ik
    • Proceedings of the KIEE Conference
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    • 2004.11a
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    • pp.248-250
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    • 2004
  • We have investigated the surface state of 154kV polymeric insulators exposed to in-service conditions for about five years. In order to evaluate surface aging of silicone rubber exposed to real field environments, we used various analytic methods such as contact angle, ATR-FTIR, SEM-EDS. Although contaminants were accumulated on weathershed surface, polymeric insulator has retained its intrinsic surface hydrophocity. In addition, ATR-FTIR confirmed the diffusion layer of a low molecular weight silicone fluid on surface layer and no surface cracking and chalking were Indicated by SEM. Polymeric insulators have still retained their improved pollution performance over porcelain insulators. That will lead to very low frequency of flashovers throughout their useful life, often under contaminated conditions.

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Effects of Electron Beam Irradiation on Tribological and Physico-chemical Properties of Polyoxymethylene (POM-C) copolymer

  • Rahman, Md. Shahinur;Yang, Jong-Keun;Shaislamov, Ulugbek;Lyakhov, Konstantin;Kim, Min-Seok;Lee, Heon-Ju
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.153-153
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    • 2016
  • Polyoxymethylene copolymer (POM-C) is an attractive and widely used engineering thermoplastic across many industrial sectors owing to outstanding physical, mechanical, self-lubricating and chemical properties. In this research work, the POM-C blocks were irradiated with 1 MeV electron beam energy in five doses (100, 200, 300, 500 and 700 KGy) in vacuum condition at room temperature. The tribological and physico-chemical properties of electron beam irradiated POM-C blocks have been analyzed using Pin on disk tribometer, Raman spectroscopy, SEM-EDS, Optical microscopy, 3D Nano surface profiler system and Contact angle analyzer. Electron beam irradiation at a dose of 100 kGy resulted in a decrease of the friction coefficient and wear loss of POM-C block due to well suited cross-linking, carbonization, free radicals formation and energetic electrons-atoms collisions (physical interaction). It also shows lowest surface roughness and highest water contact angle among all unirradiated and irradiated POM-C blocks. The irradiation doses at 200, 300, 500 and 700 kGy resulted in increase of the friction coefficient as compared to unirradiated POM-C block due to severe chain scission, chemical and physical structural degradation. The electron beam irradiation transferred the wear of unirradiated POM-C block from the abrasive wear, adhesive wear and scraping to mild scraping for the 1 MeV, 100 kGy irradiated POM-C block which is concluded from SEM-EDS and Optical microscopic observations. The degree of improvement for tribological attribute relies on the electron beam irradiation condition (energy and dose rate).

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Rotated Bending Fatigue Strength in Aged 1Cr-1Mo-0.25V Steel at Elevated Temperature (시효열화시킨 1Cr-1Mo-0.25V 강의 고온화의 회전굽힘 피로강도에 관한 연구)

  • Suh, Chang-Min;Huh, Jeong-Hoon;Namh, Seung-Hoon
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.20 no.9
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    • pp.2819-2832
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    • 1996
  • The estimation of the remaining life for the aged components in power plant as well as chemical and petroleum plants has been recently concerned. The raw materials used in this study are the 1Cr-1Mo-0.25V steel which intensified P and S compositions along with the nominal compositions of ASTM A 470 standard. Five kinds of specimens with the different degradation levels were prepared by isothermal aging heat treatment at 630.deg.C. The mechanical properties and rotated bending fatigue strength of virgin and aged 1Cr-1Mo-0.25V steel have been investigated through the hardness, tensile, fatigue test, SEM fractograph and EDS analysis at 538.deg.C and room temperature, respectively. Thus the data of aged specimens were compared with those of virgin specimen to evaluate the aging effects. The main results obtained in this study are as follows ; The decrease of the yield and tensile strength due to degradation was distinguished until 50, 000hrs simulated service time. And it was confirmed that the considerable amount of P, Mn, Cr and S was precipitated at the grain boundary of aged material through the SEM and EDS analysis. The rotated bendingd fatigue strength at 538.deg.C of virgin, 25, 000, 50, 000, 75, 000 and 100, 000 hrs aged material was decreased 44.6 %, 49.6 %, 51.5 %, 52.4% and 53.8% than that of virgin material at 10$_{7}$cycles of room temperature, respectively. The major cracks of virgin and aged materials mainly initiated at the inclusions including Si, P and Mn compositions which were located at the outer periphery of the specimen.n.