• Title/Summary/Keyword: X-ray structure analysis

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A facile chemical synthesis of a novel photo catalyst: SWCNT/titania nanocomposite

  • Paul, Rima;Kumbhakar, Pathik;Mitra, Apurba K.
    • Advances in nano research
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    • v.1 no.2
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    • pp.71-82
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    • 2013
  • A simple chemical precipitation technique is reported for the synthesis of a hybrid nanostructure of single-wall carbon nanotubes (SWCNT) and titania ($TiO_2$) nanocrystals of average size 5 nm, which may be useful as a prominent photocatalytic material with improved functionality. The synthesized hybrid structure has been characterized by transmission electron microscopy (HRTEM), energy-dispersive X-ray analysis (EDAX), powder X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. It is clearly revealed that nearly monodispersed titania nanocrystals (anatase phase) of average size 5 nm decorate the surfaces of SWCNT bundles. The UV-vis absorption study shows a blue shift of 16 nm in the absorbance peak position of the composite material compared to the unmodified SWCNTs. The photoluminescence study shows a violet-blue emission in the range of 325-500 nm with a peak emission at 400 nm. The low temperature electrical transport property of the synthesized nanomaterial has been studied between 77-300 K. The DC conductivity shows semiconductor-like characteristics with conductivity increasing sharply with temperature in the range of 175-300 K. Such nanocomposites may find wide applications as improved photocatalyst due to transfer of photo-ejected electrons from $TiO_2$ to SWCNT, thus reducing recombination, with the SWCNT scaffold providing a firm and better positioning of the catalytic material.

Crystal Growth, Spectral, Magnetic, Antibacterial and Antifungal Studies of Co(II) and Ni(II) Complexes of 4-Nitrobenzoic Acid

  • Roy, Sunalya M.;Sudarsanakumar, M.R.;Dhanya, V.S.;Suma, S.;Kurup, M.R. Prathapachandra
    • Journal of the Korean Chemical Society
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    • v.58 no.3
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    • pp.258-266
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    • 2014
  • Single crystals of cobalt(II) and nickel(II) complexes of 4-nitrobenzoic acid have been successfully grown by gel diffusion technique. The grown crystals were characterized by elemental analysis, FT-IR and UV-Visible spectroscopy. The structure of the grown crystals was elucidated using single crystal X-ray diffraction studies. The title compounds $[Co(Pnba)_2(H_2O)_4]{\cdot}2H_2O$ 1 and $[Ni(Pnba)_2(H_2O)_4]{\cdot}2H_2O$ 2 where PnbaH=4-nitrobenzoic acid, crystallize in centrosymmetric triclinic space group P-1. Magnetic susceptibility measurements reveal that the compounds are paramagnetic in nature. The mechanical strength of the grown crystals was determined by Vicker's microhardness studies. The ligand (4-nitrobenzoic acid) and the complexes have been screened for their biological activity against various bacteria and fungi. The activity data show that the biological activity of the complexes is higher than that of the ligand.

Synthesis, Thermal Decomposition Pattern and Single Crystal X-Ray Studiesof Dimeric [Cu(dmae)(OCOCH3)(H2O)]2: A Precursor for the Aerosol Assisted Chemical Vapour Deposition of Copper Metal Thin Films

  • Mazhar, Muhammad;Hussain, S.M.;Rabbani, Faiz;Kociok-Kohn, Gabriele;Molloy, Kieran C.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.10
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    • pp.1572-1576
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    • 2006
  • A dimeric precursor, $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ for the CVD of copper metal films, (dmaeH = N,N-dimethylaminoethanol) was synthesized by the reaction of copper(II) acetate monohydrate ($Cu(OCOCH_3)_2{\cdot}H_2O$) and dmaeH in toluene. The product was characterized by m.p. determination, elemental analysis and X-ray crystallography. Molecular structure of $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ shows that a dimeric unit $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ is linked to another through hydrogen bond and it undergoes facile decomposition at 300 C to deposit granular copper metal film under nitrogen atmosphere. The decomposition temperature, thermal behaviour, kinetic parameters, evolved gas pattern of the complex, morphology, and the composition of the film were also investigated.

Analysis of Sputter-Deposited SnO thin Film with SnO/Sn Composite Target (SnO/Sn 혼합 타겟을 이용한 SnO 박막 제조 및 특성)

  • Kim, Cheol;Kim, Sungdong;Kim, Sarah Eunkyung
    • Korean Journal of Materials Research
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    • v.26 no.4
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    • pp.222-227
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    • 2016
  • Tin oxides have been studied for various applications such as gas detecting materials, transparent electrodes, transparent devices, and solar cells. p-type SnO is a promising transparent oxide semiconductor because of its high optical transparency and excellent electrical properties. In this study, we fabricated p-type SnO thin film using rf magnetron sputtering with an SnO/Sn composite target; we examined the effects of various oxygen flow rates on the SnO thin films. We fundamentally investigated the structural, optical, and electrical properties of the p-type SnO thin films utilizing X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV/Vis spectrometry, and Hall Effect measurement. A p-type SnO thin film of $P_{O2}=3%$ was obtained with > 80% transmittance, carrier concentration of $1.12{\times}10^{18}cm^{-3}$, and mobility of $1.18cm^2V^{-1}s^{-1}$. With increasing of the oxygen partial pressure, electrical conductivity transition from p-type to n-type was observed in the SnO crystal structure.

Structural evolution and kinetic study of high isotacticity poly(acrylonitrile) during isothermal pre-oxidation

  • Zhang, Li;Dai, Yongqiang;Kai, Yi;Jin, Ri-Guang
    • Carbon letters
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    • v.12 no.4
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    • pp.229-235
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    • 2011
  • Isotactic polyacrylonitrile (PAN) with triad isotacticity of 0.53, which was determined by $^{13}C$ NMR, using dialkylmagnesium as an initiator, was successfully synthesized. Isothermal treatment of iso-PAN was conducted in air at 200, 220, 250 and $280^{\circ}C$. Structural evolutions and chemical changes were studied with Fourier transformation infrared and wide-angle X-ray diffraction during stabilization. A new parameter $CNF={I_{2240cm}}^{-1}/ ({I_{1595cm}}^{-1}+f^*{I_{1595cm}}^{-1})$ was defined to evaluate residual nitrile groups. Crystallinity and crystal size were calculated with X-ray diffraction dates. The results indicated that the nitrile groups had partly converted into a ladder structure as stabilization proceeded. The rate of reaction increased with treatment temperature; crystallinity and crystal size decreased proportionally to pyrolysis temperature. The iso-conversional method coupled with the Kissinger and Flynn-Wall-Ozawa methods were used to determine kinetic parameters via differential scanning calorimetry analysis with different heating rates. The active energy of the reaction was 171.1 and 169.1 kJ/mol, calculated with the two methods respectively and implied the sensitivity of the reaction with temperature.

Effect of Heat-Treated Temperature on Surface Crystal Structure and Catalytic Activity of ACF/ZnO Composite under Ultraviolet Irradiation and Ultrasonication

  • Zhang, Kan;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.47 no.2
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    • pp.136-141
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    • 2010
  • ACF/ZnO photocatalyst was synthesized by a sol-gel method using activated carbon fiber (ACF) and Zn $(NO_3)_2$ as precursors. Samples were characterized by Brunauer-Emmett-Teller measurements (BET), scanning electron microscope (SEM), X-ray diffraction (XRD), and energy dispersive X-ray (EDX). The XRD results showed that ACF/ZnO composites only included a hexagonal phase by heat-treated temperature at $400^{\circ}C$, $500^{\circ}C$, $600^{\circ}C$, and $700^{\circ}C$. The SEM analysis revealed that the ACF/ZnO composites did not exhibit any morphological changes of the catalyst surface according to the different heat-treated temperatures. The photocatalytic activity of the samples was tested for degradation of methylene blue (MB) solutions under ultraviolet (UV) light and ultrasonication respectively. The results showed that the photocatalytic activity of ACF/ZnO composites heat-treated at $500^{\circ}C$ was higher than other samples, which is ascribed to the fine distribution of ZnO particles on the surface of the ACF. In addition, an ultrasound of low power (50 W) was used as an irradiation source to successfully induce ACF/ZnO composites to perform sonocatalytic degradation of MB. Results indicated that the sonocatalytic method in the presence of ACF/ZnO composites is an advisable choice for the treatments of organic dyes.

Characteristics of Plasma Damage and Recover in PZT Films by Dry Etching (건식식각에 의한 PZT 박막의 플라즈마 손상 및 회복특성)

  • 강명구;김경태;김동표;김창일
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07a
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    • pp.375-378
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    • 2002
  • We investigated the reduction of etching damage by additive O$_2$ in etching gas and recovery of etching damage by O$_2$ annealing. The PZT thin films were etched using additive Ar or O$_2$ into Cl$_2$/CF$_4$ gas mixing ratio of 8/2. In order to recover ferroelectric properties of PZT thin films after etching, the etched PZT thin films were annealed at 600 C in O$_2$ atmosphere for 10 min. The remanent polarization is decreased seriously and fatigue is accelerated in the PZT sample etched in Ar/(C1$_2$+CF$_4$) plasma, whereas these characteristics are improved in O$_2$/(Cl$_2$/CF$_4$). From x-ray photoelectron spectroscopy (XPS) analysis, the intensities of Pb-O, Zr-O and Ti-O peaks are changed and the etch byproducts such as metal chloride and metal fluoride are reduced by O$_2$ annealing. From electron probe micro analyzer (EPMA) and auger electron spectroscopy(AES), O$_2$ vacancy is observed after etching. In x-ray diffraction (XRD), the structure damage in the additive O$_2$ into C1$_2$/CF$_4$ is reduced and the improvement of ferroelectric behavioral annealed sample is consistent with the increase of the (100) and (200) PZT peaks.

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Characteristic study of mechanical properties of Structural rolled steel and Stainless steel for MIG welding (구조용 압연강재와 스테인리스 강재의 MIG 용접에 대한 기계적 특성연구)

  • Lim, J.Y.;Yoon, M.J.;Kim, S.Y.;Kim, T.G.
    • Journal of the Korean Society of Manufacturing Process Engineers
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    • v.13 no.1
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    • pp.100-106
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    • 2014
  • It is well known that fatigue failures occur on welded structures in industrial application due to repetitive load force. In order to decrease the incidence of fatigue failure, we analyzed the mechanical properties based on structural aspects in rolled steel(SS 400) welded onto stainless steel (STS 304) by the MIG welding method as well as the structure of rolled steel welded onto itself. We compared the hardness, tensile and fatigue properties with two types of samples which had no defects on the welding parts as observed by X-ray topographic analysis. It was found that the tensile and fatigue strength levels of SS 400 welded onto STS 304 by the MIG welding method were higher than those of STS 304 welded onto itself.

A Study of Recycle of Waste Wood After Cultivating Oak Mushroom (II) - On the Structure of Cellulose Crystal Transformation of the Waste Wood - (표고버섯골목의 재활용에 관한 연구 (II) - 폐골목 세포벽 중의 셀룰로오스 결정의 변태구조 -)

  • Kim, Nam-Hun;Lee, Won-Yang
    • Journal of the Korean Wood Science and Technology
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    • v.23 no.3
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    • pp.1-7
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    • 1995
  • The crystal transformation from cellulose I to cellulose II during alkaline swelling of waste wood, which has been used for cultivating oak mushroom(Cortinellus edodes (Berk.) Ito et Imai), was investigated and compared to that of normal wood by a series of X-ray diffraction analysis. When the sapwood of cultivated wood was treated with 20% NaOH solution for 2 hours, the cellulose I can be easily transformed into Na-cellulose I than normal wood or heartwood of cultivated wood. Certainly the formation of Na-cellulose in wood is proportional to alkali swelling duration, and the formation of cultivated sapwood was faster than that of the other woods. Cellulose I in the sapwood of cultivated wood was easily transformed into cellulose II during mercerization, but the sapwood of normal wood and the heartwood of cultivated wood hardly converted to cellulose II. Namely, most of Na-cellulose I in normal wood can be reconverted to cellulose I in the process of washing and drying. Therefore, it can be concluded from this study that in cell wall lignin and hemicellulose can prevent the alkaline swelling of cellulose in wood and the transformation from cellulose I to cellulose II as well.

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Physical Properties Change of Serpentine and Talc by Planetary Ball Mill (유성밀 분쇄에 의한 사문석과 활석의 물리적 특성변화)

  • Kim, Dong-Jin;Jeong, Heon-Saeng;Lee, Jae-Cheon;Lee, Ja-Hyeon
    • Korean Journal of Materials Research
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    • v.9 no.8
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    • pp.810-816
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    • 1999
  • The variations of crystalline structures and physical proerties of serpentine and talc mineral which was treated in a planetary ball mill, wre investigated by means of X-ray diffraction, FT-IR, DSC-TG, particle size analysis and SEM observation. The crystalline peaks of serpentine and talc in the XRD patterns were gradually reduced with the increase of grinding time and after 120 minutes turned into the amorphous phase, which is attributed to the disordering of the local structure around magnesium. The endothermic peaks for the ground serpentine and talc sample are observed at a considerably lower temperatures than that for the starting sample. A morphological change from the originally flat and irregular shape to spherically agglomerated particles was clearly observed.

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