• Title/Summary/Keyword: XRD analysis

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Polyaniline/SiO2 Catalyzed One-pot Mannich Reaction: An Efficient Synthesis of β-amino Carbonyl Compounds (Polyaniline/SiO2를 이용한 one-pot Mannich 반응: β-amino carbonyl 화합물의 효율적인 합성)

  • Yelwande, Ajeet A.;Arbad, Balasaheb R.;Lande, Machhindra K.
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.644-649
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    • 2011
  • Polyaniline/$SiO_2$ catalyzed one-pot mannich reaction of acetophenone, aromatic aldehydes and aromatic amines are carried out in ethanol to afford various ${\beta}$-amino ketones. The various wt% of polyaniline were supported on pure silica synthesized by using chemical oxidative method. The catalyst prepared has been characterized by means of thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) energy dispersive spectroscopy (EDS), and Fourier transform infrared spectroscopy (FT-IR). Solvent stability of catalyst was tested using UV-Visible spectroscopy. This protocol has several advantages such as high yield, simple work up procedure, non-toxic, clean, easy recovery and reusability of the catalyst.

Evaluation for Contents of Contaminants and Leaching Characteristics of Bottom Ash (바텀애쉬의 유해물질 함량 측정 및 용출특성 평가연구)

  • Koh, Taehoon;Lee, Sungjin;Shin, Minho;Kim, Byongsuk;Lee, Jeakeun;Lee, Taeyoon
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.6
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    • pp.77-83
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    • 2010
  • In this study, we tried to determine any detrimental effects on water quality when bottom ash obtained from a coal-fired power plant intended to be used as a fill material in construction sites. Physical-chemical properties of bottom ash were determined using proximate analysis, elemental analysis, XRD, and XRF. Classification of bottom ash as a waste material and soil contamination due to the use of bottom ash were performed by Korea waste standard leaching test and soil toxicity test, respectively. Results of leaching tests were compared to the regulations for water quality and groundwater quality and no harmful effects on water quality were found. Most of heavy metals in leachate were below detection limits but trace amount of $Cr^{6+}$ was found. However, concentration of $Cr^{6+}$ was below the regulation criteria. Column leaching tests indicated that concentrations of Pb and Zn were slightly higher than regulations but below regulations within 1 PVE, but concentrations of sulfate were 10 times higher than regulation and thus, the required time to reach regulation was almost 8 PVE.

Property of MgO with Different Sintering Temperatures under High Pressures (고압 환경에서 소결 온도에 따른 MgO 물성의 변화)

  • Song, Jeongho;Noh, Yunyoung;Song, Ohsung
    • Journal of the Korean Ceramic Society
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    • v.49 no.6
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    • pp.608-613
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    • 2012
  • We investigated the property changes of MgO powders sintered at temperatures ranging from $700^{\circ}C$ to $1900^{\circ}C$ for 5minutes at a pressure of 2.7 GPa for a high-pressure high-temperature(HPHT) diamond synthesis process. The physical properties of the sintered MgO powders were characterized by optical microscopy, field emission scanning electron microscopy (FE-SEM), Vickers hardness tests, and by the apparent density, and X-ray diffractometry. An optical micro-analysis showed that white MgO powders became black after sintering due to carbon contamination from the graphite heat source. FE-SEM revealed the growth in the grain size of the MgO powders from $0.3{\mu}m$ to $50{\mu}m$ after sintering at $1700^{\circ}C$. The hardness and apparent density increased to $1800^{\circ}C$ while the samples were dedensified at $1900^{\circ}C$ due to the growth of isolated pores. According to the XRD analysis, no phase transformation occurred in the MgO powders. These results suggest that HPHT-sintered MgO powders can show an accelerated sintering process characterized by grain neck growth, pore connections, isolated pore growth and dedensification in 5 minutes, while these processes with the conventional sintering process take at least 5 hours.

Deactivation of V2O5/TiO2 catalytic system on the sulfuric oxides (V2O5/TiO2 촉매시스템의 황산화물에 대한 비활성화 특성)

  • Jang, Hyun Tae;Cha, Wang Seog
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.16 no.11
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    • pp.7433-7438
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    • 2015
  • Deactivation characteristics of $V_2O_5/TiO_2$ catalysts were studied for selective catalytic reduction(SCR) of NOx with ammonia in the presence of $SO_2$. Performance of catalyst was investigated for $deNO_x$ activity while changing temperature, $SO_2$ concentration. The activity of catalyst was decreased with the increase of $SO_2$ concentration and reaction time. Also, degree of activity drop was largely decreased with the increase of reaction temperature in the range of $250{\sim}300^{\circ}C$. Physicochemical properties of deactivated catalysts were characterized by BET, XRD, SEM, TPD analysis. According to the analysis results, deactivation phenomena occur due to the relatively high formation of ammonium sulfate salts, which created by unreacted ammonia and water in the presence of $SO_2$. It was revealed that ammonium sulfate cause the pore plogging of support and deposition of active matter.

Effects of TiN/Ti Multilayer Coating on the Ti-30Ta-xZr Alloy Surface (Ti-30Ta-xZr 합금의 표면에 TiN/Ti 다층막코팅효과)

  • Kim, Y.U.;Jeong, Y.H.;Cho, J.Y.;Choe, H.C.;Vang, M.S.
    • Journal of Surface Science and Engineering
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    • v.42 no.4
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    • pp.161-168
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    • 2009
  • Effects of TiN/Ti multilayer coating on the Ti-30Ta-xZr alloy surface were studied by using various experiments. The Ti-30Ta containing Zr (5, 10 and 15 wt%) were melted 10 times to improve chemical homogeneity by using a vacuum furnace. And then samples were homogenized for 24 hrs at $1000^{\circ}C$. The specimens were prepared for TiN/Ti coating by cutting and polishing. The prepared specimens were coated with TiN/Ti multilayers by using DC magnetron sputtering method. The analyses of coated surface and coated layer were carried out by field emission scanning electron microscope(FE-SEM), EDX, and X-ray diffractometer(XRD). From the microstructure and XRD analysis of Ti-30Ta-xZr alloys, The equiaxed structure was changed to needle-like structure with increasing Zr content. And $\alpha$-peak and elastic modulus increased as Zr content increased. The $\alpha$ and $\beta$ phase predominantly were found in the specimen containing high Zr content. According to the analysis of TiN/Ti coating layer, the surface defects and structures of Ti-30Ta-xZr were covered with TiN/Ti coating layer and surface roughness decreased.

An Investigation of Lattice Parameter Measurement of Inorganic Crystals by Electron Diffraction Patterns (전자회절도형을 이용한 무기시료의 격자상수 측정법 연구)

  • Lee, Young-Boo;Kim, Youn-Joong
    • Applied Microscopy
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    • v.29 no.1
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    • pp.75-81
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    • 1999
  • Optimum conditions for making the Au and Al internal standards for TEM have been determined experimentally. The Au internal standard was produced by sputter coating at 9mA for 100 seconds in low vacuum $(\leq1\times10^{-3})$. The Al internal standard was produced by evaporation coating at 7kV for 10 minutes in high vacuum $(\leq1\times10^{-5})$. Measurements of the lattice parameters of andalusite and albite feldspars with this Au internal standard resulted in errors of (a) $ \leq1.2%$ in precion and $\leq0.3%$ in accuracy for andalusite: (b) $\leq0.5%$ in precision and $\leq1.1%$ in accuracy for albite feldspars. The most significant error occurred from the measuring processes of distances and angles of electron diffraction patterns. By employing systematic procedures of measurement with high precision devices, this lattice parameter determination method utilizing the internal standard should be a good alternative to the conventional powder XRD method or the sophisticated CBED method for special samples.

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Effect of $N_2$ and $O_2$ Properties of STS304 Stainless Steel Films Synthesized by Unbalanced Magnetron Sputtering Process (비대칭 마그네트론 스퍼터링법에 의해 합성된 STR304 스테인리스강 박막에서의 질소와 산소의 첨가 효가)

  • 김광석;이상율;김범석;한전건
    • Journal of Surface Science and Engineering
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    • v.34 no.2
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    • pp.89-96
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    • 2001
  • N- or O-doped STS304 stainless films were synthesized by an unbalanced magnetron sputtering process with various argon and reactive gas ($N_2$, $O_2$) mixtures. These films were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), Auger electron spectroscopy (AES) and Knoop microhardness tester. The Results from X-ray diffraction (XRD) analysis showed that a STS304 stainless steel film synthesized without reactive gas using a bulk STS304 stainless steel target had a ferrite bcc structure ($\alpha$ phase), while the N-doped STS304 stainless film was consisted of a nitrogen supersaturated fcc structure, which hsa a strong ${\gamma}$(200) phase. In the O-doped films, oxide Phases ($Fe_2$$O_3$ and $Cr_2$$O_3$) were observed from the films synthesized under an excess $O_2$ flow rate of 9sccm. AES analysis showed that nitrogen content in N-doped films increased as the nitrogen flow rate increased. Approximately 43 at.%N in the N-doped film was measured using a nitrogen flow rate of 8sccm. In O-doped film, approximately 15 at.%O was detected using a $O_2$ flow rate of 12sccm. the Knoop microhardness value of N-doped film using a nitrogen flow rate of 8 sccm was measured to be approximately $H_{ k}$ 1200 and this high value could be attributed to the fine grain size and increased residual stress in the N-doped film.

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Effect of Ca Ion on the SCR Reaction over VOx/TiO2 (Ca 이온이 VOx/TiO2 SCR 반응에 미치는 영향 연구)

  • Kim, Geo Jong;Hong, Sung Chang
    • Applied Chemistry for Engineering
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    • v.27 no.2
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    • pp.165-170
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    • 2016
  • In this study, we investigated the cause of the decrease in activities of $VO_x/TiO_2$ SCR catalyst used for the burner reactor at a scale of $150000Nm^3/hr$ using X-ray diffraction (XRD), brunauer-emmett-teller (BET), atomic emission spectroscopy inductively coupled plasma (AES ICP), $H_2$ temperature programmed reduction ($H_2$-TPR), and $NH_3$ temperature programmed desorption ($NH_3$-TPD) analysis. Since the crystallization of the $VO_x$ and phase transition of $TiO_2$ did not occur, it was concluded that the catalyst was not deactivated by the thermal effect. In addition, from the elemental analysis showing that a large quantity of calcium was detected but not sulfur, the deactivation process of the $VO_x/TiO_2$ SCR catalyst was mainly caused by Ca but not by $SO_2$. The calcium was also found to decrease the catalytic activity by means of reducing $NH_3$ adsorption.

A Study on Extinguishing Concentration of K2CO3-Zeolite Composites (K2CO3가 흡착된 합성제올라이트 구조체의 소화농도에 관한 연구)

  • Kim, Seung-Il;Shin, Chang-Sub
    • Fire Science and Engineering
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    • v.26 no.4
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    • pp.42-47
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    • 2012
  • In the study, fire extinguishing concentration of $K_2CO_3$-Zeolite composite was measured. Zeolite composite is a porous adsorbent which has small particle size, low density and anti-catalytic effect. Scanning Electron Microscopy, X-Ray diffraction and thermal analysis were also conducted to investigate the structural properties of composite. The result showed that despite of weight ratio, the extinguishing concentration of the composite was lower than pure $K_2CO_3$. The extinguishing concentration of $K_2CO_3$-Zeolite composite which has weight ratio of 7 : 3 was 5.72 times lower than that of pure $K_2CO_3$ and 1.1 times lower than that of ABC powder. The SEM and XRD patterns showed that $K_2CO_3$ was adsorbed on the Zeolite properly, and through the thermal analysis, it was founded that the composite is more effective extinguishing agent than pure $K_2CO_3$.

Flexural strength and microstructure of two lithium disilicate glass ceramics for CAD/CAM restoration in the dental clinic

  • Kang, Suk-Ho;Chang, Juhea;Son, Ho-Hyun
    • Restorative Dentistry and Endodontics
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    • v.38 no.3
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    • pp.134-140
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    • 2013
  • Objectives: There has been a growing interest in glass ceramic systems with good esthetics, high fracture resistance and bonding durability, and simplified fabrication techniques using CAD/CAM. The aim of this study is to compare flexural strength before and after heat treatment of two lithium disilicate CAD/CAM blocks, IPS e.max CAD (Ivoclar Vivadent) and Rosetta SM (Hass), and to observe their crystalline structures. Materials and Methods: Biaxial flexural strength was tested according to ISO 6872 with 20 disc form specimens sliced from each block before and after heat treatment. Also, the crystalline structures were observed using field-emission scanning microscopy (FE-SEM, Hitachi) and x-ray diffraction (XRD, Rigaku) analysis. The mean values of the biaxial flexural strength were analyzed by the Mann-Whitney U test at a significance level of p = 0.05. Results: There were no statistically significant differences in flexural strength between IPS e.max CAD and Rosetta SM either before heat treatment or after heat treatment. For both ceramics, the initial flexural strength greatly increased after heat treatment, with significant differences (p < 0.05). The FE-SEM images presented similar patterns of crystalline structure in the two ceramics. In the XRD analysis, they also had similar patterns, presenting high peak positions corresponding to the standard lithium metasilicate and lithium disilicate at each stage of heat treatment. Conclusions: IPS e.max CAD and Rosetta SM showed no significant differences in flexural strength. They had a similar crystalline pattern and molecular composition.