• Title/Summary/Keyword: Crystal structure analysis

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A Study on the Characteristics of a Pt/TiO2 Catalyst Prepared by Liquid-Phase Ruduction for Formaldehyde Oxidation at Room Temperature (액상환원 기반 Pt/TiO2 촉매 제조를 이용한 포름알데히드 상온 산화 반응 특성 연구)

  • Jae Heon Kim;Younghee Jang;Geo Jong Kim;Sung Chul Kim;Sung Su Kim
    • Applied Chemistry for Engineering
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    • v.34 no.6
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    • pp.612-618
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    • 2023
  • Modern society spends more than 80% of its daily life indoors, emphasizing the need for attention to indoor air pollution due to the improvement in living standards. In this study, the performance and reaction characteristics of the Pt/TiO2 catalysts prepared by liquid-phase reduction for the removal of formaldehyde (HCHO), one of the indoor air pollutants, at room temperature without the need for additional light or heat were investigated. As a result, it showed that catalysts prepared by the same method showed approximately 40~80% various activities depending on the type of TiO2. XRD, BET, and XPS analyses were performed to investigate the particle size, crystal structure, specific surface area, and O/Ti molar ratio of the support material, and it revealed that the correlation between the properties and performance was insignificant. To explore the oxidation reaction pathway of formaldehyde (HCHO), in situ DRIFT analysis using carbon monoxide and H2-TPR was perfomed. The results revealed that the performance was demonstrated by the oxidation state of the active metal and the adsorption-desorption characteristics of the adsorbate species.

Fabrication and Electrochemical Characterization of Carbon Fluoride-based Lithium-Ion Primary Batteries with Improved Rate Performance Using Oxygen Plasma (산소 플라즈마를 이용하여 율속 성능이 개선된 불화탄소 기반 리튬 일차전지의 제조 및 전기 화학적 특성)

  • Seoyeong Cheon;Naeun Ha;Chaehun Lim;Seongjae Myeong;In Woo Lee;Young-Seak Lee
    • Applied Chemistry for Engineering
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    • v.34 no.5
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    • pp.534-540
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    • 2023
  • The high-rate performance is limited by several factors, such as polarization generation, low electrical conductivity, low surface energy, and low electrolyte permeability of CFX, which is widely used as a cathode active material in the lithium primary battery. Therefore, in this study, we aimed to improve the battery performance by using carbon fluoride modified by surface treatment using oxygen plasma as a cathode for lithium primary batteries. Through XPS and XRD analysis, changes in the surface chemical characteristics and crystal structure of CFX modified by oxygen plasma treatment were analyzed, and accordingly, the electrochemical characteristics of lithium-ion primary batteries were analyzed and discussed. As a result, the highest number of semi-ionic C-F bonds were formed under the oxygen plasma treatment condition (7.5 minutes) with the lowest fluorine to carbon (F/C) ratio. In addition, the primary cell prepared under this condition using carbon fluoride as the active material of the cathode showed the highest 3 F/C(3 C rate-performance) rate-performance and maintained a relatively high capacity (550 mAh/g) even at high rates. In this study, it was possible to produce lithium primary batteries with high-rate performance by adjusting the fluorine contents of carbon fluoride and the type of carbon-fluorine bonding through oxygen plasma treatment.

Cloning and Expression of Bacillus thuringiensis crylAa1 Type Gene. (Bacillus thuringiensis crylAa1 Type Gene의 클로닝과 발현)

  • 이형환;황성희;권혁한;안준호;김혜연;안성규;박수일
    • Microbiology and Biotechnology Letters
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    • v.32 no.2
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    • pp.110-116
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    • 2004
  • The over-expression in E. coli of the pHLN1-SO(+) and pHLN2-80(-) plasmids cloned an insecticidal crystal protein (ICP) gene (crylAal type) from Bacillus thuringiensis var. kurstaki HD 1 was investigated through in part, the deletion of -80 bp promoter and an alternative change of cloning vector system. Two recombinant plasmids were constructed in an attempt to analyze the over-expression of the ICP in relations to its gene structure possessing only -14 bp [Shine-Dalgarno (SD) sequence of -80 bp promoter]. Also, anther two recombinant plasmids similarly cloned the icp gene in a different vector system. The amounts of ICP produced from the recombinants were measured by SDS-PAGE and confirmed by Western blot analysis. One clone, pHLRBS1-14 clone in which only the SD sequence in the inverted orientation icp gene appeared, was more evident than the pHLRBS2-14 clone in which only the -14 bp SD sequence of the right orientated icp gene was shown to exist. The pHLN2-80(-) clone produced more ICP proteins than the pHLRBS1-14 clone. In the two clones, pHLNUC1-80 right-oriented icp gene and the pHLNUC2-80 clone inverted-orientation icp gene in a new different vector, the pHLNUC2-80 produced more ICP proteins in E. coli system. These results indicate that the P/ac promoter, the inverted icp gene insertion and -80 bp promoter (-66 bp part of the icp gene promoters), were concerned with the expression of the icp gene in the recombinant plasmids. In addition, the expression mechanism might result from the disruption of the transcription-suppressing regions in the promoter regions.

Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

Surface characteristics and stability of implants treated with alkali and heat (알칼리와 열처리에 의한 임플란트의 표면 특성 및 골유착 안정성에 관한 연구)

  • Song, Yun-Seok;Cho, In-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.46 no.5
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    • pp.490-499
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    • 2008
  • Statement of problem: Bioactive materials must have the ability to spontaneously form a bone like apatite layer on their surface and induce direct biochemical bonding to bone. A simple chemical treatment via alkali and heat has been revealed to induce bioactivity in titanium. Purpose: The purpose of this study was to evaluate the surface characteristics and stability of alkali and heat treated implants. Material and methods: Specimens were divided into three groups; group 1 was the control group with machined surface implants, groups 2 and 3 were treated with alkali solutions and heat treated in the atmosphere and vacuum conditions respectively. The surface characteristics were observed with FESEM, XPS, TF-XRD and AFM. Stability was evaluated with the resonance frequency analysis, periotest and removal torque values. One-way ANOVA and Duncan test were used for statistical analysis. Results: 1. Groups treated with alkali and heat showed similar characteristics. Groups 2 and 3 showed high compositions of Na ions on the surface with sub-micron sized pores compared to group 1. Group 2 showed mixed compositions of anatase and rutile with superior contents of rutile. 2. Resonance frequency analysis : The ISQ of group 2 showed significantly higher values than that of groups 1 and 3 at 12 weeks. The ISQ of groups 1 and 2 showed significant increase after 4 weeks, and the ISQ of group 3 increased significantly after 2 and 4 weeks respectively (P < .05). 3. Periotest: The PTV of groups 1 and 2 showed significant decrease after 4 weeks, and the PTV of group 3 showed significant decrease after 2 and 4 weeks respectively (P < .05). 4. Removal torque analysis: The removal torque value of group 2 was significantly higher than those of groups 1 and 3 at 2, 4 and 8 weeks. The removal torque values of groups 1 and 3 showed increase at 4 and 12 weeks, but the removal torque value of group 2 showed increase after 4 weeks (P < .05). Conclusion: An oxide layer with appropriate crystal structure and amorphous sodium titanate layer can be obtained on titanium implants through alkali and heat treatment in the atmosphere, and even alkali and heat treatment in vacuum conditions, provided a bioactive surface containing sodium. These surface layers can be considered to be effective for enhancement of osseointegration and reduction of healing period for implant treatment.

Synthesis and Electrochemical Properties of Carbon Coated Li4Ti5O12 using PVC (PVC를 원료로 탄소코팅한 Li4Ti5O12의 합성 및 전기화학적 특성)

  • Hyun, Si-Cheol;Na, Byung-Ki
    • Clean Technology
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    • v.24 no.1
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    • pp.77-84
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    • 2018
  • In this study, $Li_4Ti_5O_{12}$ anode materials for lithium ion battery were synthesized by dry ball-mill method. Polyvinyl chloride (PVC) as a carbon source was added to improve electrochemical properties. When the PVC was added after $Li_4Ti_5O_{12}$ formation, the spinel structure was well synthesized and it was confirmed by X-ray diffraction (XRD) experiments. When the carbon material was added before the synthesis and the heat treatment was performed, it was confirmed that a material having a different crystal structure was synthesized even when a small amount of carbon material was added. In the case of $Li_4Ti_5O_{12}$ without the carbon material, the electrical conductivity value was about $10{\mu}S\;m^{-1}$, which was very small and similar to that of the nonconductor. As the carbon was added, the electrical conductivity was greatly improved and increased up to 10,000 times. Electrochemical impedance spectroscopy (EIS) analysis showed that the size of semicircle corresponding to the resistance decreased with the carbon addition. This indicates that the resistance inside the electrode is reduced. According to the Cyclic voltammetry (CV) analysis, the potential difference between the oxidation peak and the reduction peak was reduced with carbon addition. This means that the rate of lithium ion insertion and deinsertion was increased. $Li_4Ti_5O_{12}$ with 9.5 wt% PVC added sample showed the best properties in rate capabilities of $180mA\;h\;g^{-1}$ at 0.2 C-rate, $165mA\;h\;g^{-1}$ at 0.5 C-rate, and $95.8mA\;h\;g^{-1}$ at 5 C-rate.

Removal of Fluoride Using Thermally Treated Activated Alumina (고온 처리된 활성알루미나를 이용한 불소 제거)

  • Park, Seong-Jik;Kim, Jae-Hyeon;Lee, Chang-Gu;Park, Jeong-Ann;Choi, Nag-Choul;Kim, Song-Bae
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.10
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    • pp.986-993
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    • 2010
  • In this study, sorption characteristics of thermally treated activated alumina (AA) for fluoride were investigated. Sorption experiments have been conducted in equilibrium and kinetic batch conditions. Also, effects of solution pH and anions on fluoride removal have been observed. The properties of thermally treated ( $700^{\circ}C$) activated alumina (AA700) and untreated activated alumina (UAA) were compared using field-emission scanning electron microscope, energy-dispersive spectrometry, X-ray diffractometer (XRD) analysis, and Brunauer-Emmett-Teller (BET) analysis. From the experiments using AA thermally treated at different temperatures (100, 300, 500, $700^{\circ}C$), it was found that at high fluoride concentrations (50, 100, 200 mg/L) the sorption capacity of thermally treated AA increased with increasing thermal treatment temperature. At an initial fluoride concentration of 200 mg/L, the sorption capacity of AA700 was 3.67 times greater than that of UAA. The BET analysis showed that the specific surface area of UAA was about 2 times larger than that of AA700. The XRD analysis indicated that UAA was composed of both boehmite (AlOOH) and bayerite ($Al(OH)_3$) while AA700 was $Al_2O_3$. The reason that fluoride sorption capacity of AA700 increased despite of decrease in specific surface area compared to UAA could be attributed to the change of crystal structure. The kinetic sorption test showed that fluoride sorption to AA700 arrived at equilibrium after 24 h. The equilibrium test demonstrated that the maximum sorption capacity of AA700 was 5.70 mg/g. Additional batch experiments indicated that fluoride sorption to AA700 was the highest at pH 7, decreasing at both acidic and basic solution pHs. Also, fluoride sorption to AA700 decreased in the presence of anions such as phosphate, nitrate, and carbonate. This study demonstrated that thermal treatment of AA at high temperature could increase its sorption capacity for fluoride.

An Experimental Study of Corrosion Characteristics and Compounds by Corrosion Factors in Iron Artifacts (철제유물 부식인자에 대한 부식양상 및 부식화합물 실험 연구)

  • Park, Hyung Ho;Lee, Jae Sung;Yu, Jae Eun
    • 보존과학연구
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    • s.33
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    • pp.33-43
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    • 2012
  • The corrosion phenomena of the iron artifacts was studied by morphology observation and instrumental analysis(EDS, XRD, Raman) with various corrosion factors in oder to verify to confirm the danger of corrosion factors. Corrosion compounds were collected by depositing pure Fe powder(99%) into a HCl, $HNO_3$, $H_2SO_4$, and $H_2O$ solution which contained the corrosion factors. Stereoscopic-microscope observations were then conducted determine the colors and shapes of the collected corrosion compounds, and SEM-EDS analysis was conducted to confirm the corrosion factors and the growth of these compounds. X-ray diffraction (XRD), Raman analyses were conducted to examine the crystal structure and compositions of the created corrosion compounds. The results of the experiment revealed that corrosion speed was faster in an acidic environment and corrosion of HCl and $H_2SO_4$ was greater than that of $HNO_3$. The corrosion compounds of HCl grew into a needle or chestnut-like shape after being affected by Cl- ion, and XRD and Raman analyses detected goethite and lepidocrocite. The corrosion compounds of $H_2SO_4$ was affected by S ion and grew into a slender-needle-like or cylindrical shape, and the XRD and Raman analyses detected goethite and lepidocrocite. The corrosion compounds of $HNO_3$ grew into a spherical or plate-like shape after being affected by O ion and the XRD and Raman analyses detected magnetite and lepidocrocite. Although the corrosion compounds of $H_2O$ grew into a spherical or plate-like shape after being affected by O ion, most of them were observed to have had spherical shapes, and the XRD and Raman analyses failed to detect corrosion compounds in them. It was found in the study that corrosion characteristics and compounds are diversely displayed according to the corrosion factor.

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A bilayer diffusion barrier of atomic layer deposited (ALD)-Ru/ALD-TaCN for direct plating of Cu

  • Kim, Soo-Hyun;Yim, Sung-Soo;Lee, Do-Joong;Kim, Ki-Su;Kim, Hyun-Mi;Kim, Ki-Bum;Sohn, Hyun-Chul
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.239-240
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    • 2008
  • As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

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Identification of Active Agents for Reductive Dechlorination Reactions in Cement/Fe (II) Systems by Using Cement Components (시멘트 구성성분을 이용한 시멘트/Fe(II)의 TCE 환원성 탈염소화 반응의 유효반응 성분 규명)

  • Jeong, Yu-Yeon;Kim, Hong-Seok;Hwang, In-Seong
    • Journal of Soil and Groundwater Environment
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    • v.13 no.1
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    • pp.92-100
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    • 2008
  • Experimental studies were conducted to identify the active agents for reductive dechlorination of TCE in cement/Fe(II) systems focusing on cement components such as CaO, $Fe_2O_3$, and $Al_2O_3$. A hematite that was used to simulate an $Fe_2O_3$ component in cement was found to have degradation efficiencies (k = 0.641 $day^{-1}$) equivalent to that of cement/Fe(II) systems in the presence of CaO/Fe(II), only when it contained an aluminum impurity$(Al_2O_3)$. When the effect of $Al_2O_3$ content of hematite/CaO/$Al_2O_3$/Fe(II) system was tested, the mole ratio of $Al_2O_3$ to CaO affected the rate of TCE degradation with an optimum ratio around 1 : 10 that resulted in a rate constant of 0.895 $day^{-1}$. In the SEM images of hematite/CaO/$Al_2O_3$/Fe(II) systems, acicular crystals were also found that were also observed in cement/Fe(II) systems. Thus it was suspected that these crystals were reactive reductants and that they might be goethite or ettringite that are known to have acicular structures. An EDS element map analysis revealed that these crystals were not goethite crystals. A subsequent experiment that tested reactivities of compounds formed during the ettringite synthesis showed that ettringite and minerals associated with ettringite formation are not reactive reductants. These observations conclude that a mineral containing CaO and $Al_2O_3$ with a acicular structure could be a major reactive reductant of cement/Fe(II) systems.