• 제목/요약/키워드: Electron diffraction data

검색결과 158건 처리시간 0.027초

Synthesis, spectral, thermal, structural study and theoretical treatment of new complexes of mannich base with Ni(II) and study of cytotoxicity effect on (Hepa-2) cell line and antimicrobial activity

  • Omar H. Al-Obaidi
    • 분석과학
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    • 제36권2호
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    • pp.70-79
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    • 2023
  • The synthesis of the Mannich base as a ligand (L) N-(morpholino (phenyl) methyl) acetamide is the subject of this study. Elemental analyses, FT-IR spectra, UV-vis, 1H-NMR, and magnetic measurements were used to confirm the synthesis of the [Ni(L)2]Cl2 complex, thermal analysis (TG/DTG), atomic absorption, and scanning, and structurally explained as electron microscopy (SEM), and X-ray powder diffraction (XRD) methods. The melting point of the complex and its molar conductivity were also measured. The suggested geometries of the complexes formed have a tetrahedral structure, according to the data acquired using various techniques. Theoretical approaches to the complex formation have been investigated. For molecular mechanics and semi-empirical calculations, the HYPERCHEM6 program had been used. The effect of the novel Ni(II) complex on the cancer cell Hepa-2 (human hepatocellular ademocarcinoma), that is the human laryngeal cancer, was studied. It has been found that these ligand and complex have potent effects on the cancer cell. The antibacterial activity of the free ligand and its complex was evaluated against two kinds of human pathogenic bacteria. The first category is Gram-positive (Staphylococcus aureas, epiderimids), whereas the second group is Gram-negative (Psedamonas aeruginosa, Escherichia coli) (from the diffusion method). Finally, it was discovered that various chemicals had varied growth-inhibiting effects on bacteria.

Effectiveness of Ni-based and Fe-based cladding alloys in delaying hydrogen generation for small modular reactors with increased accident tolerance

  • Alan Matias Avelar;Fabio de Camargo;Vanessa Sanches Pereira da Silva;Claudia Giovedi;Alfredo Abe;Marcelo Breda Mourao
    • Nuclear Engineering and Technology
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    • 제55권1호
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    • pp.156-168
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    • 2023
  • This study investigates the high temperature oxidation behaviour of a Ni-20Cr-1.2Si (wt.%) alloy in steam from 1200 ℃ to 1350 ℃ by Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD). The results demonstrate that exposed Ni-based alloy developed a thin oxide scale, consisted mainly of Cr2O3. The oxidation kinetics obtained from the experimental results was applied to evaluate the hydrogen generation considering a simplified reactor core model with different cladding alloys following an unmitigated Loss-Of-Coolant Accident (LOCA) scenario in a hypothetical Small Modular Reactor (SMR). Overall, experimental data and simulations results show that both Fe-based and Ni-based alloys may enhance cladding survivability, delaying its melting, as well as reducing hydrogen generation under accident conditions compared to Zr-based alloys. However, a substantial neutron absorption occurs when Ni-based alloys are used as cladding for current uranium-dioxide fuel systems, even when compared to Fe-based alloys.

칼륨-흑연 섬유층간화합물의 구조와 전자 에너지 상태의 분석 (The Analysis of Structure and Electron Energy State of Potassium-Graphite Fiber Intercalation Compounds)

  • 오원춘;김명건;고영신
    • 분석과학
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    • 제6권5호
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    • pp.479-487
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    • 1993
  • 구조가 잘 발달된 피치계 흑연섬유로부터 변형된 two-bulbs법를 사용하여 흑연섬유의 반응 온도 변화($T_g$ : $450^{\circ}C$, $400^{\circ}C$, $350^{\circ}C$, $300^{\circ}C$, $250^{\circ}C$)에 따라 칼륨 흑연 섬유층간 화합물을 합성하였다. K-GFIC의 stage 전이과정을 X-선 회절법을 이용하여 연구하였고, 이때 1 stage와 2 stage에 있어서 특징적인 (001) 회절선의 d값은 $5.40{\AA}$$8.78({\pm}0.01){\AA}$으로 나타났다. K-GFIC의 stage를 가진 K-GFIC의 반사율의 최소값이 원래 흑연 섬유보다 높은 에너지쪽에서 나타났음을 알 수 있었다. Stage의 혼재 때문에 높은 반응온도($400^{\circ}C$, $450^{\circ}C$)에서는 가시광선 영역에서 뚜렷한 반사율의 최소값을 찾을 수가 없었다. X-선 회절법과 UV/VIS 분광법 데이터는 낮은 stage를 가진 K-GFIC는 흑연 섬유층의 탄소원자들 사이에 전하 운반자가 존재하고 있음을 제시하고 있다. 또한 이러한 결과들은 K-GFIC의 전기적 성질과 물리적 성질에 대한 정보를 제공하여 주고 있다.

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X선 회절법에 의한 전남지역 천일염의 결정학적 특성 (Crystallographical Characteristics of Solar Salts Produced from Jeonnam Area by X-Ray Diffraction Technique)

  • 정병조;김용;김창대;현승철;함경식
    • 한국식품영양과학회지
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    • 제38권9호
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    • pp.1284-1288
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    • 2009
  • 본 연구는 천일염 결정 내에 함유된 무기물들의 화합물 결정 상태를 비파괴적인 방법인 XRD 방법으로 규명할 수 있는지를 조사하기 위하여, 전남 서남해안의 12개 지역 염전에서 채취한 12종의 천일염들에 대하여 X선 회절선을 측정하고, 이 X선 회절선 스펙트럼을 EDX 측정 결과와 JCPDS 데이터와의 비교 분석을 통하여 천일염 결정 내에 함유된 무기물들의 화합물 결정 상태를 처음으로 확인하였다. 특히 아직까지 알려져 있지 않았던 무기질 화합물 결정들이 천일염에 함유되어 있음을 밝혀냈는데, 신안 증도와 신의의 천일염에서 $Na_2S$, 신안 비금의 천일염에서 $KMgCl_3$, 신안 도초에서 $Ca(ClO_3)_2$, 해남 송지에서 $CaAl_4O_7$, 고흥에서 $CaSiO_3$, $CaCl_2$, 해남 토판 소금에서 NaKCl 등이 관측되었다. 또한 XRD 측정 결과는 천일염의 결정구조가 소금의 입방구조인 NaCl구조를 그대로 유지함을 보였으며, 격자상수도 정제염이나 시약염에 비해 거의 변화가 없는 비슷한 값을 보였다. 그러나 FE-SEM으로부터 조사한 천일염의 외형적 결정 구조는 정제염과 시약염에서 보이는 소금 NaCl의 결정구조인 정육면체의 결정 형태와는 달리 이들이 적층되어 이루어진 결정 형태의 특징을 보였다. 또한 결정 입자의 크기에 있어서도 정제염이나 시약염보다 수백 배에 이르는 특징을 보였다.

포항-울산간의 점토자원의 지질과 그 물리화학적 특성에 관한 연구 (A Study on Geology of Clay Mineral Deposits of Pohang-Ulsan Area and their Physico-Chemical Properties)

  • 김옥준;이하영;김서운;김수진
    • 자원환경지질
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    • 제4권4호
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    • pp.167-215
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    • 1971
  • I. Purpose and Importance of the Study The purpose of the present study is to clarify to geological, mineralogical, and physico-chemical properties of the clay minerals deposits imbedded in the Tertiary sediments in the areas between. Pohang and Ulsan along southeastern coastal region of Korea. These clays are being mined and utilized for filter and insecticide after activation or simple pulverizing, nontheless activated clays are short coming as chemical industry in Korea has been rapidly grown in recent years. In spite of such increase in clay demand, no goological investigation on clay deposits nor physico-chemical properties of the clays have been carried out up to date. Consequently activated clays produced in Korea is not only of low grade but also of shortage in supply, so that Korea has to import activated clays of better grade. The importance of the present study lies, therefore, on that guiding principle could be laid down by knowing stratigraphical horizons, of clay deposits and fundamental data of improving grade of activated clays might be derived from the results of physico-chemical examinations. II. Contents and Scope of the study The contents of the study are pinpointed down in the following two subjects: 1) General geological investigation of Tertiary formations distributed in the areas between Pohang and UIsan, and detail geological study of the bentonitic clay deposits imbedded in them. 2) To clarifty physico-chemical characteristics of the clays by means of chemical analysis, X-ray diffraction and electron microscope. The scope of the study involves the following there points: i) Regional geological investigation-This investigation has been carried out in order to find out the distribution of Tertiary sediments and exact location of clay mineral deposits in the areas between Pohang and UIsan. ii) Detail geological investigation-This has been concentrated in and around the clay deposits which. had been found out by the regional investigation. iii) Laboratory researchs include i) age determination and correlation of Tertiary sediments by paleontological study, and ii) Chemical analysis, X-ray diffraction, and electron microscopic studies on clays, samples taken from various clay deposits. III. Research Results and Suggestions 1) The geology of the area investigated is composed mainly of Janggi and Beomgokri groups of Miocene age in ascending order rested on the upper Silla system, Balkuksa granite and volcanic rocks of upper Cretaceous age as base. 2) Janggi group is composed in ascending order of Janggi conglomerate, Nultaeri rhyolitic tuff, Keumkwangdong shale, two beds of lignite-bearing formations which consist of alternation of conglomerate, sandstone and mudstone, and andesitic, rhyolitic, and basaltic tuff beds. 3) Beomgokri group is mainly composed of andesitic to rhyolitic tuff interlayered by conglomerate and tuffaceous sandstone. In the areas around boundary between North-and South Kyeongsang-do is distributed Haseori farmation which is composed of conglomerate, sandstone, mudstone and andesitic to rhyolitic tuff, and which is correlated to Eoilri formation of Janggi group. 4) Clay deposits of the area are interbedded in Eoilri, Haseori, Nultaeri tuff, Keumkwangdong shale, upper and lower horizon of the lower lignite-bearing seam, and Keumori rhyolitic tuff formations of Janggi group; and are genetically classi.fied into four categories, that is, i) those derived from volcanic ash beds(Haseori and Daeanri deposits), ii) those of secondary residual type from rhyolitic tuff beds(Seokupri deposits), iii) Clay beds above and beneath the lignite seams, (Janggi and Keumkwangdong deposits), and iv) those derived from rhyolitic tuff beds(Sangjeong and Tonghae deposits). 5) Mineral constituents of clay deposits are, according to X-ray diffraction, montmorillonite accompanied in different degree by cristobalite, plagioclase, quartz, stilbite, and halloysite in rare occasion. The clays are grouped according to mineral composition into four types; i) those consist mostly of montmorillonite, ii) those composed of montmorillonite and cristobalite, iii) those composed of montmorillonite and plagioclase, and iv) those composed of montmorillonite, plagioclase and quartz. 6) Clays interbedded in Haseori formation and vicinity of lignite seams belong to the first type, are of good quality and derived either from volcanic ash bed, or primary clay beds near lignite seams. Clays belonged to other types are derived from weathering of rhyolitic tuff formations and their quality varies depending upon original composition and degree of weathering. Few clays in secondary residual type contain small amount of halloysite. 7) Judging from analytical data, content of silica($SiO_2$) varies proportionally with content of cristobalite, and alumina($Al_2O_3$) content does not vary with that of plagioclase, but increases in the sedimentary bedded type of deposits. 8) It is unknown whether or not these days could be upgraded by beneficiation since no grain size of these impurities nor beneficiation test had been studied. 9) Clay beds derived from valcanic ash layers or sedimentary layers at the vicinity of lignite seams are thin in thickness and of small, discontinueous lenticular shape, although they are of good quality; and those derived from rhyolitic tuff formations or residual type from tuff are irregular in both occurrence and quality. It is, therefore, not only very difficult but also meaningless to calculate its reserve, and reserve estimation, even if done, will greatly be deviated from practically minable one. Consequently, way of discovery and exploitation of clay deposits in the area under consideration is to check the geologically favorable areas whenever needed.

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옥천대의 석류석데 변성암에서 산출되는 백운모, 녹니석 및 흑운모의 Intergrowth와 Interlayering (Intergrowth and Interlayering of Muscovite, Chlorite, and Biotite in a Garnet Zone Metamorphic Rock of the Ogcheon Belt, South Korea)

  • Yeong Boo Lee;Jung Hoo Lee;Chang Whan Oh
    • 한국광물학회지
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    • 제15권2호
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    • pp.122-131
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    • 2002
  • 옥천대 변성 이질암에 분포하는 백운모, 녹니석 및 흑운모는 각기 다른 크기에서 intergrowth와 interlayer 된 것을 전자현미분석(EPMA) 배면 산란 전자상(BEI) 관찰 및 투과 전자현미경(TEM)을 이용한 lattice fringe 상 관찰을 통한 연구에서 밝혔다. 이들 세 광물은 편광현미경 관찰에서도 intergrow된 것이 관찰되며 EPMA 분해능 이하의 크기에서는 interlayer된 것으로 보인다. 다시 말하면, EPMA 분석 자료는 흔히 백운모/녹니석(M/C), 흑운모/녹니 석(B/C), 백운모/파이로필라이트/녹니석(M/Py/C), 흑운모/파이로필라이트/녹니석(B/Py/C) 또는 흑운모/백운모/녹니석(B/M/C)과 같이 두 개 이상의 phyllosilicate 광물의 혼합 형태로 나타난다. BEI 관찰에서는 세 광물(백운모, 녹니석 및 흑운모)이 하나의 입자 안에서 다양한 크기로 섞여 있는 것으로 나타나며, TEM lattice fringe 상 관찰과 제한 시야 전자 회절상 관찰에 의하면 이들 세 광물 사이의 interlayering은 석류석대 변성암에서까지 관찰된다. TEM 관찰 결과 녹니석대 변성암에서는 M/C와 함께 7-$\AA$ layer(사문석, 녹니석의 전신)가 -$10\AA$ layer(백운모) 내에 100~200 $\AA$ 크기로 inter-layer된 것이 밝혀졌다. 흑운모대 변성암으로 가면 7-$\AA$ layer는 크기와 발견 횟수가 감소하고 10-$\AA$ layer는 녹니석(14 $\AA$)과 개별 layer 수준에서 interlayer된다. 석류석대 변성암에서는 7-$\AA$ layer는 더 이상 관찰되지 않으며 10-$\AA$ layer(흑운모)가 녹니석과 50~100 $\AA$ 크기로 interlayer된다.(BEI, TEM). 석류석대 변성암에서는 비교적 큰 크기(1000~2000 $\AA$)의 intergrowth가 흔히 관찰된다. 그러나 세 개의 변성대 암석은 모두 TEM 관찰에서 7-, 10-, 또는 14-$\AA$ layer들이 몇 개의 layer 단위에서 서로 interlayer된 것을 보여준다. 이와 같은 결과는 백운모, 녹니석 및 흑운모와 같은 변성 광물들이 비평형 광물 반응으로 만들어 졌으며 그 결과 불균질한 광물로 되었다는 것을 암시한다.

가용화 조성물을 함유한 PVP형 고체분산체의 제조 및 특성 (Preparation and Dissolution of Polyvinylpyrrolidone(PVP)-Based Solid Dispersion Systems Containing Solubilizers)

  • 조청일;김태완;최춘영;권경애;이범진
    • Journal of Pharmaceutical Investigation
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    • 제33권1호
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    • pp.7-14
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    • 2003
  • The PVP-based solid dispersion systems (SDs) containing lovastatin (LOS) and solubilizers (sodium lauryl sulfate, tween 80 and oleic acid) were prepared to enhance dissolution rate of practically water insoluble LOS using solvent evaporation method. Two different organic cosolvents either acetone/ethanol or acetonitrile/ethanol were used for the preparation of SDs. The LOS contents were highly decreased when acetone/ethanol cosolvents were used. The decrease of LOS contents was not caused by acetonitrile or acetone, based on HPLC data. The surface morphology as investigated by scanning electron microscope (SEM) and angle of repose as an index of flowability of SDs were highly dependent on the type and amount of solubilizers used. Based on differential scanning calorimetry (DSC) and X-ray powder diffraction data, the SDs made crystalline LOS into amorphous structure or partially eutectic mixtures. The simultaneous use of the solubilizers in SDs was also useful to increase dissolution rate of LOS in gastric or intestinal fluid. The SDs containing solubilizers reached 76% and 60% in gastric and intestinal fluid, respectively but the commercial tablet gave only less than 4%. These solubilizers in SDs could be also applicable for enhancing dissolution and bioavailability of poorly water-soluble drugs.

TiO2 분말 합성을 위한 Ammonium Hexafluofide Titanate의 열적 거동 연구 (Study on thermal behavior of Ammonium Hexafluofide Titanate for Synthesis of TiO2 Powders)

  • 이덕희;박재량;이찬기;박경수;김현모
    • 한국분말재료학회지
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    • 제23권5호
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    • pp.353-357
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    • 2016
  • In this study, $TiO_2$ powders are synthesized from ammonium hexafluoride titanate (AHFT, $(NH_4)_2TiF_6$) as a precursor by heat treatment. First, we evaluate the physical properties of AHFT using X-ray diffraction (XRD), particle size analysis (PSA), thermogravimetric analysis (TGA), and field-emission scanning electron microscopy (FE-SEM). Then, to prepare the $TiO_2$ powders, is heat-treated at $300-1300^{\circ}C$ for 1 h. The ratio of anatase to rutile phase in $TiO_2$ is estimated by XRD. The anatase phase forms at $500^{\circ}C$ and phase transformation to the rutile phase occurs at $1200^{\circ}C$. Increase in the particle size is observed upon increasing the reaction temperature, and the phase ratio of the rutile phase is determined from a comparison with the calculated XRD data. Thus, we show that anatase and rutile $TiO_2$ powders could be synthesized using AHFT as a raw material, and the obtained data are utilized for developing a new process for producing high-quality $TiO_2$ powder.

Surface Transition by Solvent Washing Effects and Biological Properties of Metal Treated Activated Carbons

  • Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • 제25권5호
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    • pp.639-646
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    • 2004
  • Metal treated activated carbons are prepared using various metals. Adsorption behaviors, morphologies, as well as antibacterial effects of metal treated samples are compared before and after solvent washing. Adsorption isotherms are used to characterize the porous structure of metal treated activated carbons before and after the solvent washing with acetone or ethyl alcohol. From these data, it is noticed that the changes in physicochemical properties of metal treated activated carbons depend on the solvents employed. Similar results are observed from BET data obtained from nitrogen adsorption isotherms. From scanning electron microscopy (SEM) studies, the changes in shape and size of metal particles are observed after the samples are washed with solvents. These changes result in different blocking effects, which, in turn, affect the adsorption behavior of metal treated activated carbons. X-ray diffraction (XRD) patterns of the samples treated with different metals are different each other. High intense sharp peaks attributed to metals are observed from silver treated samples, while the peaks are not observed from copper treated samples. To compare thermodynamic behavior of metal treated activated carbons washed with different type of solvents, differential scanning calorimetric (DSC) analysis is carried out. The analysis shows similar endothermic curves for all of the samples. Finally, antibacterial effects of metal treated activated carbon against Escherichia coli are discussed. Comparing the effects among the metals employed, highest effects are obtained from Cd, while lowest effects are obtained from Cu. Antibacterial activity becomes higher with the increase of the amount of metals treated, Optimum concentrations of metals to treat activated carbons, obtained from a shake flask test, are known to be 0.4, 0.1, and 0.6 moles for Ag, Cd, and Cu, respectively.

Growth and Characterization of Conducting ZnO Thin Films by Atomic Layer Deposition

  • Min, Yo-Sep;An, Cheng-Jin;Kim, Seong-Keun;Song, Jae-Won;Hwang, Cheol-Seong
    • Bulletin of the Korean Chemical Society
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    • 제31권9호
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    • pp.2503-2508
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    • 2010
  • ZnO thin films were grown on Si or $SiO_2$/Si substrates, at growth temperatures ranging from 150 to $400^{\circ}C$, by atomic layer deposition (ALD) using diethylzinc and water. Despite the large band gap of 3.3 eV, the ALD ZnO films show high n-type conductivity, i.e. low resistivity in the order of $10^{-3}\;{\Omega}cm$. In order to understand the high conductivity of ALD ZnO films, the films were characterized with X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, elastic recoil detection, Rutherford backscattering, Photoluminescence, and Raman spectroscopy. In addition, the various analytical data of the ZnO films were compared with those of ZnO single crystal. According to our analytical data, metallic zinc plays an important role for the high conductivity in ALD ZnO films. Therefore when the metallic zinc was additionally oxidized with ozone by a modified ALD sequence, the resistivity of ZnO films could be adjusted in a range of $3.8{\times}10^{-3}\;{\sim}\;19.0\;{\Omega}cm$ depending on the exposure time of ozone.