• Title/Summary/Keyword: X-ray Structure Analysis

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Thermal Stability of Ru-inserted Nickel Monosilicides (루테늄 삽입층에 의한 니켈모노실리사이드의 안정화)

  • Yoon, Kijeong;Song, Ohsung
    • Korean Journal of Metals and Materials
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    • v.46 no.3
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    • pp.159-168
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    • 2008
  • Thermally-evaporated 10 nm-Ni/1 nm-Ru/(30 nm or 70 nm-poly)Si structures were fabricated in order to investigate the thermal stability of Ru-inserted nickel monosilicide. The silicide samples underwent rapid thermal anne aling at $300{\sim}1,100^{\circ}C$ for 40 seconds. Silicides suitable for the salicide process were formed on the top of the single crystal and polycrystalline silicon substrates mimicking actives and gates. The sheet resistance was measured using a four-point probe. High resolution X-ray diffraction and Auger depth profiling were used for phase and chemical composition analysis, respectively. Transmission electron microscope and scanning probe microscope(SPM) were used to determine the cross-sectional structure and surface roughness. The silicide, which formed on single crystal silicon and 30 nm polysilicon substrate, could defer the transformation of $Ni_2Si $i and $NiSi_2 $, and was stable at temperatures up to $1,100^{\circ}C$ and $1,100^{\circ}C$, respectively. Regarding microstructure, the nano-size NiSi preferred phase was observed on single crystalline Si substrate, and agglomerate phase was shown on 30 nm-thick polycrystalline Si substrate, respectively. The silicide, formed on 70 nm polysilicon substrate, showed high resistance at temperatures >$700^{\circ}C$ caused by mixed microstructure. Through SPM analysis, we confirmed that the surface roughness increased abruptly on single crystal Si substrate while not changed on polycrystalline substrate. The Ru-inserted nickel monosilicide could maintain a low resistance in wide temperature range and is considered suitable for the nano-thick silicide process.

Synthesis and Characterization of Magnetic Core-shell ZnFe2O4@ZnO@SiO2 Nanoparticles (Magnetic Core-shell ZnFe2O4@ZnO@SiO2 Nanoparticle의 합성과 성질에 관한 연구)

  • Yoo, Jeong-Yeol;Lee, Young-Ki;Kim, Jong-Gyu
    • Journal of the Korean Chemical Society
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    • v.59 no.5
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    • pp.397-406
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    • 2015
  • ZnO, II-VI group inorganic compound semi-conductor, has been receiving much attention due to its wide applications in various fields. Since the ZnO has 3.37 eV of a wide band gap and 60 meV of big excitation binding energy, it is well-known material for various uses such the optical property, a semi-conductor, magnetism, antibiosis, photocatalyst, etc. When applied in the field of photocatalyst, many research studies have been actively conducted regarding magnetic materials and the core-shell structure to take on the need of recycling used materials. In this paper, magnetic core-shell ZnFe2O4@SiO2 nanoparticles (NPs) have been successfully synthesized through three steps. In order to analyze the structural characteristics of the synthesized substances, X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FT-IR) were used. The spinel structure of ZnFe2O4 and the wurtzite structure of ZnO were confirmed by XRD, and ZnO production rate was confirmed through the analysis of different concentrations of the precursors. The surface change of the synthesized materials was confirmed by SEM. The formation of SiO2 layer and the synthesis of ZnFe2O4@ZnO@SiO2 NPs were finally verified through the bond of Fe-O, Zn-O and Si-O-Si by FT-IR. The magnetic property of the synthesized materials was analyzed through the vibrating sample magnetometer (VSM). The increase and decrease in the magnetism were respectively confirmed by the results of the formed ZnO and SiO2 layer. The photocatalysis effect of the synthesized ZnFe2O4 @ZnO@SiO2 NPs was experimented in a black box (dark room) using methylene blue (MB) under UV irradiation.

Synthesis and Characterization of Aluminosilicate Prepared Using Structure Directing Agent Containing Piperidine Moiety (피페리딘형 구조유도분자를 이용한 알루미노실리케이트 제올라이트의 합성 및 특성 연구)

  • Kim, Su Hyun;Park, Sung Jun;Shin, Na Ra;Cho, Sung June
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.203-207
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    • 2013
  • Zeolites with different structures were synthesized from the hydrothermal synthesis condition employing simple structure directing agent (SDA) containing piperidine moiety. The gel containing $1.0SiO_2$:0.9SDA:$0.062NaAlO_2$:0.217NaOH:$20H_2O$ was subject to hydrothermal synthesis at 413~453 K for 7 days. FER type zeolite was obtained at 433 K when piperidine was employed as SDA, whereas TON and MFI type zeolites were also obtained at 433 K when 2,6-dimethylpiperidine and 2,2,6,6-tetramethylpiperidine were used, respectively. Further increase of hydrothermal synthesis temperature to 453 K resulted in the formation of TON type zeolite when 2-mtheylpiperidine was used. The structural analysis of powder X ray diffraction pattern over FER type zeolite suggested that the SDA, piperidine interacted intimately with the zeolite where it located close to the framework.

The surface kinetic properties of $ZrO_2$ Thin Films in dry etching by Inductively Coupled Plasma

  • Yang-Xue, Yang-Xue;Kim, Hwan-Jun;Kim, Dong-Pyo;Um, Doo-Seung;Woo, Jong-Chang;Kim, Chang-Il
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2009.06a
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    • pp.105-105
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    • 2009
  • $ZrO_2$ is one of the most attractive high dielectric constant (high-k) materials. As integrated circuit device dimensions continue to be scaled down, high-k materials have been studied more to resolve the problems for replacing the EY31conventional $SiO_2$. $ZrO_2$ has many favorable properties as a high dielectric constant (k= 20~25), wide band gap (5~7 eV) as well as a close thermal expansion coefficient with Si that results in good thermal stability of the $ZrO_2/Si$ structure. In order to get fine-line patterns, plasma etching has been studied more in the fabrication of ultra large-scale integrated circuits. The relation between the etch characteristics of high-k dielectric materials and plasma properties is required to be studied more to match standard processing procedure with low damaged removal process. Due to the easy control of ion energy and flux, low ownership and simple structure of the inductively coupled plasma (ICP), we chose it for high-density plasma in our study. And the $BCl_3$ included in the gas due to the effective extraction of oxygen in the form of $BCl_xO_y$ compound In this study, the surface kinetic properties of $ZrO_2$ thin film was investigated in function of Ch addition to $BCl_3/Ar$ gas mixture ratio, RF power and DC-bias power based on substrate temperature. The figure 1 showed the etch rate of $ZrO_2$ thin film as function of gas mixing ratio of $Cl_2/BCl_3/Ar$ dependent on temperature. The chemical state of film was investigated using x-ray photoelectron spectroscopy (XPS). The characteristics of the plasma were estimated using optical emission spectroscopy (OES). Auger electron spectroscopy (AES) was used for elemental analysis of etched surface.

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Synthesis and Properties of Polyurethane/Clay Nanocomposites Containing Siloxane Segment (실록산 세그먼트를 가진 폴리우레탄/점토 나노복합체의 제조 및 물성에 관한 연구)

  • Lee Jung Eun;Kim Hyung Joong
    • Polymer(Korea)
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    • v.29 no.2
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    • pp.177-182
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    • 2005
  • Montmorillonite (MMT) modified with siloxane diamine was reacted with a reactant obtained from 4,4'-diphenyl methane diisocyanate (MDI) and polyester type polyol, $Nippollan4010(\bar{M}_n2000)$. Finally, polyurethane (PU)/MMT composites were prepared by using 1,4-butane diol as a chain extender in $25\;wt\%$ solution of N,N-dimethyl acetamide (DMAc). It was expected that these nanocomposites had superior exfoliation property to that of MMT dispersed polyurethanes produced by simple mixing due to insertion of siloxane main chain to the silicate interlayer of MMT. Extent of reaction and formation of final products were analysed by using FT-IR spectroscopy. Dispersion into the PU and intercalation of MMT were identified by applying X-ray diffraction (XRD) and transmission electron microscopy (TEM). Tensile data were acquired by universal test machine (UTM). Thermal stability and variation of surface energy were characterized by thermal gravimetric analysis (TGA) method and measurement of contact angle on the synthesized composites, respectively. As the results the organo-MMT modified with siloxane diamine in the PU composites has an intercalated structure relatively well-expanded rather than a completely exfoliated structure. The tensile strengths and the moduli for the PU/organo-MMT composites were drastically enhanced in comparison to those of $PU/Na^+-MMT$ composites.

Chimie Douce Reaction to Layered High-$T_c$ Superconducting / Super-ionic Conducting Heterostructures

  • Kim, Young-Il;Hwang, Seong-Ju;Yoo, Han-Ill;Choy, Jin-Ho
    • The Korean Journal of Ceramics
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    • v.4 no.2
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    • pp.95-98
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    • 1998
  • We have developed new type of superconducting-superionic conducting nanohybrids, $Ag_xI_wBi_2Sr_2Ca_{n-1}Cu_nO_y$ (n=1 and 2) by applying the chimie douce reaction to the superconducting Bi-based cuprates. These nanohybrids can be achieved by the stepwise intercalation whereby the $Ag^+$ ion is thermally diffused into the pre-intercalated iodine sublattice of $IBi_2Sr_2Ca_{n-1}Cu_nO_y$. According to the X-ray diffraction analysis, the Ag-I intercalates are found to have an unique heterostructure in which the superionic conducting Ag-I layer and the superconducting $IBi_2Sr_2Ca_{n-1}Cu_nO_y$ layer are regularly interstratified with a remarkable basal increment of ~7.3$\AA$. The systematic XAS studies demonstrate that the intercalation of Ag-I accompanies the charge transfer between host and guest, giving rise to a change in hole concentration of $CuO_2$ layer and to a slight $T_c$ change. The Ag K-edge EXAFS result reveals that the intercalated Ag-I has a $\beta$-AgI-like local structure with distorted tetrahedral symmetry, suggesting a mobile environment for the intercalated $Ag^+$ ion. In fact, from ac impedance analyses, we have found that the Ag-I intercalates possess a fast ionic conductivity ($\sigma_i=10^{-1.4}\sim 10^{-2.6}\Omega^{-1}\textrm{cm}^{-1}\;at\;270^{\circ}C$ with an uniform activation energy ($\DeltaE_a=0.22\pm 0.02$ eV). More interesting finding is that these intercalates exhibit high electronic conducting as well as ionic ones ($t_i$=0.02~0.60) due to their interstratified structure consisting of superionic conducting and superconducting layers. In this respect, these new intercalates are expected to be useful as an electrode material in various electrochemical devices.

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General characteristics of Antheraea yamamai silkworm cocoon cultured in Korea (천잠 누에고치의 일반 성상)

  • Lee, Kwang-Gill;Chung, Da-Eun;Kim, Kee-Young;Jo, You-Young;Kim, Hyun-Bok;Kim, Sung-Kuk;Kweon, HaeYong
    • Journal of Sericultural and Entomological Science
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    • v.53 no.1
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    • pp.6-11
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    • 2015
  • Antheraea yamamai silkworm cocoon is considered as a natural biocompatible materials, but can not be used as medical resources due to its difficult processability. In this study, we examined the general characteristics including cocoon shell weight and structural and thermal properties of Antheraea yamamai silkworm cocoon. The cocoon shell weight and thickness of wild silkworm cocoon was 0.528 g and 0.424 mm, respectively. The cocoon has yellow-green color in outside cocoon but white in inner layer cocoon. Amino acid analysis showed that the main amino acid of Antheraea yamamai cocoon is alanine, glycine, serine, aspartic acid, tyrosine and arginine. X-ray diffractometry showed that strong diffraction peaks at $2{\theta}=16.8^{\circ}$, $20.4^{\circ}$, corresponded to ${\beta}$-sheet structure and sharp diffraction peaks at $2{\theta}=15.0^{\circ}$, $24.3^{\circ}$, $30.0^{\circ}$ due to the presence of calcium oxalate on cocoon surface. Antheraea yamamai cocoon was degraded at $370^{\circ}C$. These results might be used as basic information for development of non-textile materials using Anthereae yamamai silkworm cocoon.

The Crystal Structure of Nicotine Dihydroiodide (Nicotine Dihydroiodide의 結晶構造)

  • Koo, Chung-Hoe;Kim, Hoon-Sup
    • Journal of the Korean Chemical Society
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    • v.9 no.3
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    • pp.134-141
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    • 1965
  • Crystals of nicotine dihydroiodide, are orthorhombic with space group $p2_12_12_1$.The unit cell of dimensions a=7.61, b=11.01, e=17.27${\AA}$, contains four formula units. The structure has been determined by X-ray diffraction method and has been refined to give the R-index, ${\sum}{\mid}{\mid}F_{\circ}{\mid}-{\mid}F_c{\mid}{\mid}{\div}{\sum}{\mid}F_{\circ}{\mid}$, of 0.16 and 0.14 for $F_{okl}\;and\;F_{hol}$ respectively.The mean lengths of C-C and C-N bonds in pyridine ring are 1.40 and $1.35{\AA}$ and those in pyrolidine ring 1.56 and $1.48{\AA}$ respectively, though accurate measurement of bond length has not been attempted. The six atoms in the pyridine ring are coplanar and on the other hand $C_6,\;C_7,\;C_8$ and $N_2$ atoms in pyrrolidine ring form a plane within accuracy of the analysis, and $C_9$ atom is distant $0.22{\AA}$ out of the plane consist of $C_6,\;C_7,\;C_8$ and $N_2$ aoms. The normals to the two planes form an angle of $94^{\circ}$ with each other. Iodine atom is distant $3.55{\AA}$ from nitrogen atom in pyridine ring and the other iodine atom $3.58{\AA}$ from nitrogen atom in pyrrolidine ring, so that the nitrogen and iodine atoms are firmly linked.It seems that the only forces binding nicotine dihydroiodide molecules together in the crystal are Van der Waals forces.

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Fe-doped beta-tricalcium phosphate; crystal structure and biodegradable behavior with various heating temperature (Fe 이온 치환 beta-tricalcium phosphate의 하소 온도에 따른 미세구조 및 분해 특성)

  • Yoo, Kyung-Hyeon;Kim, Hyeonjin;Sun, Woo Gyeong;Yoon, Seog-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.30 no.6
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    • pp.244-250
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    • 2020
  • β-Tricalcium phosphate (β-TCP, Ca3(PO4)2) is a kind of biodegradable calcium phosphate ceramics with chemical and mineral compositions similar to those of bone. It is a potential candidate for bone repair surgery. To improve the bioactivity and osteoinductivity of β-TCP, various ions doped calcium phosphate have been studied. Among them, Iron is a trace element and its deficiency in the human body causes various problems. In this study, we investigated the effect of Fe ions on the structural variation, degradation behavior of β-TCP. Fe-doped β-TCP powders were synthesized by the coprecipitation method, and the heat treatment temperature was set at 925 and 1100℃. The structural analysis was carried out by Rietveld refinement using the X-ray diffraction results. Fe ions existed in a different state (Fe2+ or Fe3+) with different heat treatment temperatures, and the substitution sites (Ca-(4) and Ca-(5)) also changed with temperature. The degradation rate was fastest at Fe-doped β-TCP with heated at 1100℃. The cell viability behavior was also enhanced with the substitution of Fe ions. Therefore, the substitution of Fe ion has accelerated the degradation of β-TCP and improved the biocompatibility. It could be more utilized in biomedical devices.

Study on the Production Methods and Conservation Treatment of the Gold Earrings Excavated from the Ancient Tombs in Seokchon-dong in Seoul (석촌동 고분군 출토 금제이식의 제작기법 연구 및 보존처리)

  • Kim, Yeseung;Jeong, Seri;Lee, Dahye;Jang, Minkyeong;Kim, Naeun;Yang, Seokjin
    • Conservation Science in Museum
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    • v.26
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    • pp.143-160
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    • 2021
  • The Seoul Baekje Museum has been conducting excavations at the Ancient Tomb Complex in Seokchon-dong, Seoul (Historic Site No. 243), known to be tombs of the royal family and the ruling class during the Hanseong period of the Baekje Kingdom. In this study, gold earrings that were revealed during the excavation underwent scientific analysis and conservation treatment. Stereo microscopy, SEM, X-ray imaging, CT, and XRF were applied in the analysis, and the characteristics, internal structure, and composition of the earrings as well as their production method were investigated. The results confirmed that the main hoops of the gilt-bronze earrings were made of copper cores gilt using mercury amalgamation. The findings also revealed that the hexahedron in the middle pendant was made by connecting small rings using molten gold powder, and the pendant sphere at the end was formed by soldering two hemispheres. As for the two thin-hoop earrings, they showed similar surface compositions but were made using different methods, with one made from a copper core wrapped with a gold plate and the other made by bending a gold rod. The gold content varied depending on the item and the place of measurement, but overall the earrings showed a relatively high gold content of approximately 19 to 21K. The purity of the golden earrings and the sophisticated manufacturing techniques applied indicate the high status of the buried person and of the tomb complex in Seokchong-dong.