• Title/Summary/Keyword: X-ray diffractometer (XRD)

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A SCANNING ELECTRON MICROSCOPIC STUDY OF BONDING ASPECTS TO THE SCLEROTIC DENTIN (경화된 상아질의 접합 양상에 관한 주사전자현미경적 연구)

  • Lee, Rin;Lee, Hyeong-Il;Lee, Kwang-Won;Son, Ho-Hyun
    • Restorative Dentistry and Endodontics
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    • v.22 no.1
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    • pp.228-243
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    • 1997
  • The changes of microstructures, morphology of sclerotic dentin and bonding aspects generated by an adhesive resin was investigated. Incisors and premolars showing natural cervical abrasions were collected and conditioned with 10 % phosphoric acid or 10 % maleic acid. The sclerotic dentin specimens were then rinsed and blot-dried and applied with dentin adhesive (All Bond 2) to the conditioned dentin surface. To examine the morphologic change of the sclerotic dentin specimen after etching and bonding procedure, the treated specimens were examined by SEM. To analyze the chemical composition of sclerotic dentin and crystals occluding dentinal tubules, the sclerotic dentin specimen was powdered and examined with X-ray Diffractometer. To investigate the Ca/P weight percent ratio within the dentinal tubules, the sclerotic dentin specimen was fractured perpendicularly to the long axis of the tooth from the center of cervical abrasion lesion and then examined with EDX(Energy Dispersive X-ray) microanalyzer. The results were as follows : 1. The increased width of peritubular dentin and the depositions of the irregular amorphous materials within the dentinal tubules were showed in the sclerotic dentin specimens. 2. After the treatment of sclerotic dentin specimen with 10 % phosphoric acid or 10 % maleic acid, the lateral side of tubules rather than cross-sectional tubule openings was showed exclusively at the incisal and gingival incline of the specimens. 3. After the treatment of sclerotic dentin specimen with 10 % phosphoric acid or 10 % maleic acid, the hybrid layer was not formed evidently and the resin tag was not formed or shortly penetrated into the tubules with the thinner diameter. 4. According to the results of XRD analysis of the sclerotic dentin specimen, Hydroxyapatite and Octacalcium phosphate were predominent, however, Whitlockite crystals were rare. 5. The mean Ca/P weight percent ratio analysed from 5 fractured sclerotic dentin specimens was $2.322{\pm}0.170$ at the intertubular dentin, $1.826{\pm}0.051$ within the dentinal tubule.

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Evaluation of Raw and Calcined Eggshell for Removal of Cd2+ from Aqueous Solution

  • Kim, Youngjung;Yoo, Yerim;Kim, Min Gyeong;Choi, Jong-Ha;Ryoo, Keon Sang
    • Journal of the Korean Chemical Society
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    • v.64 no.5
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    • pp.249-258
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    • 2020
  • The potential use of egg shell and calcined egg shell as adsorbent was evaluated and compared to remove Cd2+ from aqueous solution. The samples were characterized using Thermogravimetry and Differential Thermal Analysis (TG/DTA), Scanning Electron Microscope (SEM), X-ray Diffractometer (XRD), Energy Dispersive X-ray Spectrometer (EDX) and BET Surface Analyzer. The batch-type adsorption experiment was conducted by varying diverse variables such as contact time, pH, initial Cd2+ concentrations and adsorbent dosage. The results showed that, under the initial Cd2+ concentrations ranged from 25 to 200 mg g-1, the removal efficiencies of Cd2+ by egg shell powder (ESP) were decreased steadily from 96.72% to 22.89% with increase in the initial Cd2+ concentration at 2.5 g of dosage and 8 h of contact time. However, on the contrary to this, calcined egg shell powder (CESP) showed removal efficiencies above 99% regardless of initial Cd2+ concentration. The difference in the adsorption behavior of Cd2+ may be explained due to the different pH values of ESP and CESP in solution. Cd2+ seems to be efficiently removed from aqueous solution by using the CESP with a basicity nature of around pH 12. It was also observed that an optimum dosage of ESP and CESP for nearly complete removal of Cd2+ from aqueous solution is approximately 5.0 g and 1.0 g, respectively. Consequently, Cd2+ is more favorably adsorbed on CESP than ESP in the studied conditions. Adsorption data were applied by the pseudo-first-order and pseudo-second-order kinetics models and Freundlich and Langmuir isotherm models, respectively. With regard to adsorption kinetics tests, the pseudo-second-order kinetics was more suitable for ESP and CESP. The adsorption pattern of Cd2+ by ESP was better fitted to Langmuir isotherm model. However, by contrast with ESP, CESP was described by Freundlich isotherm model well.

Effect of Alkali and Heat Treatments of Ti-6Al-4V Alloy on the Precipitation of Calcium Phosphate (Ti-6Al-4V 합금의 알칼리 및 열처리가 인산칼슘 침착에 미치는 영향)

  • Park, Jae-Han;Lim, Ki-Jung;Kim, Sang-Mok;Kim, Byung-Ock;Han, Kyung-Yoon
    • Journal of Periodontal and Implant Science
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    • v.30 no.1
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    • pp.187-203
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    • 2000
  • The precipitation of calcium phosphate on implant surface has been known to accelerate osseointegration and to enhance osseous adaptation. The present study was performed to examine whether the precipitation of calcium phosphate on Ti-6Al-4V alloy could be affected by the immersion in NaOH solution and heat treatment. Ti-6Al-4V alloy plates of $15{\times}3.5{\times}1mm$ in dimension were polished sequentially from #240 to #2,000 emery paper and one surface of each specimen was additionally polished with $0.1{\mu}m$ alumina paste. Polished specimens were soaked in various concentrations of NaOH solution(0.1, 1.0, 3.0, 5.0, 7.0, 10.0 M) at $60^{\circ}C$ for 24 hours for alkali treatment, and 5.0 M NaOH treated specimens were heated for 1 hour at each temperature of 400, 500, 600, 700, $800^{\circ}C$. After the alkali and heat treatments, specimens were soaked in the Hank's solution with pH 7.4 at $36.5^{\circ}C$ for 30days.The surface ingredient change of Ti-6Al-4V alloy was evaluated by thin-film X-ray diffractometer(TF-XRD) and the surface microstructure was observed by scanning electron microscope(SEM), and the elements of surface were analyzed by X-ray photoelectron spectroscopy(XPS). The results were obtained as follows ; 1. The precipitation of calcium phosphate on Ti-6Al-4V alloy was accelerated by the immersion in NaOH solution and heat treatment. 2. In Alkali treatment for the precipitation of calcium phosphate on Ti-6Al-4V alloy, the optimal concentration of NaOH solution was 5.0 M. 3. In heat treatment after alkali treatment in 5.0 M NaOH solution, the crystal formation on alloy surface was enhanced by increasing temperature. In heat treated alloys at $600^{\circ}C$, latticed structure and prominences of calcium phosphate layer were most dense. On heat treated alloy surface at the higher temperature(${\geq}700^{\circ}C$), main crystal form was titanium oxide rather than apatite. The above results suggested that the precipitation of calcium phosphate on the surface of Ti-6Al-4V alloy could be induced by alkali treatment in 5.0 M-NaOH solution and by heat treatment at $600^{\circ}C$.

Gas Permeability through Mixed Matrix Membrane of Poly(dimethylsiloxane) with Aluminosilicate Hollow Nanoparticles (알루미노규산염 나노입자를 이용한 Poly(dimethylsiloxane) 복합매질 분리막의 기체투과 특성)

  • Fang, Xiaoyi;Jung, Bumsuk
    • Membrane Journal
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    • v.29 no.1
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    • pp.51-60
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    • 2019
  • In order to improve gas separation properties of polymeric membranes which have been widely applied in the industry field, aluminosilicate hollow nanoparticles named as allophanes were synthesized by sol-gel method and formulated in Poly(dimethylsiloxane) (PDMS) matrix to investigate the gas separation properties of PDMS membrane. Transmission electron microscope (TEM), Energy dispersive X-ray analysis (EDX), X-ray diffractometer (XRD), Surface area and pore size analyzer (BET) and Fourier transform infrared spectrophotometer (FTIR) were carried out to characterize the synthetic allophanes. Then the PDMS mixed matrix membranes were prepared by adding different volume fraction of allophanes. To examine the effect of allophanes addition in PDMS matrix using unmodified allophane and modified ones, the gas permeation experiments were performed using oxygen, nitrogen, methane and carbon dioxide. As the volume fraction of modified allophane increased up to 4.05 Vol% the permeability of four test gases through PDMS mixed matrix membranes increased. Also, the selectivity of $O_2/N_2$ and $CO_2/CH_4$ increased with the contents of the modified allophane. Further improvement of gas separation properties of PDMS mixed matrix membranes containing higher volume percent of allophanes can be expected as long as well dispersion of allophanes in PDMS matrix can be achieved for better PDMS membranes.

The Development of an Electroconductive SiC-ZrB2 Ceramic Heater through Spark Plasma Sintering

  • Ju, Jin-Young;Kim, Cheol-Ho;Kim, Jae-Jin;Lee, Jung-Hoon;Lee, Hee-Seung;Shin, Yong-Deok
    • Journal of Electrical Engineering and Technology
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    • v.4 no.4
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    • pp.538-545
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    • 2009
  • The SiC-$ZrB_2$ composites were fabricated by combining 30, 35, 40 and 45vol.% of Zirconium Diboride (hereafter, $ZrB_2$) powders with Silicon Carbide (hereafter, SiC) matrix. The SiC-$ZrB_2$ composites, the sintered compacts, were produced through Spark Plasma Sintering (hereafter, SPS), and its physical, electrical, and mechanical properties were examined. Also, the thermal image analysis of the SiC-$ZrB_2$ composites was examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed via X-Ray Diffractometer (hereafter, XRD) analysis. The relative density of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$, and SiC+45vol.%$ZrB_2$ composites were 88.64%, 76.80%, 79.09% and 88.12%, respectively. The XRD phase analysis of the sintered compacts demonstrated high phase of SiC and $ZrB_2$ but low phase of $ZrO_2$. Among the SiC-$ZrB_2$ composites, the SiC+35vol.%$ZrB_2$ composite had the lowest flexural strength, 148.49MPa, and the SiC+40vol.%$ZrB_2$ composite had the highest flexural strength, 204.85MPa, at room temperature. The electrical resistivities of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$ and SiC+45vol.%$ZrB_2$ composites were $6.74\times10^{-4}$, $4.56\times10^{-3}$, $1.92\times10^{-3}$, and $4.95\times10^{-3}\Omega{\cdot}cm$ at room temperature, respectively. The electrical resistivities of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$ SiC+40vol.%$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ composites had Positive Temperature Coefficient Resistance (hereafter, PTCR) in the temperature range from $25^{\circ}C$ to $500^{\circ}C$. The V-I characteristics of the SiC+40vol.%$ZrB_2$ composite had a linear shape. Therefore, it is considered that the SiC+40vol.%$ZrB_2$ composite containing the most outstanding mechanical properties, high resistance temperature coefficient and PTCR characteristics among the sintered compacts can be used as an energy friendly ceramic heater or electrode material through SPS.

Structural and Solubility Characteristics of Coenzyme Q10 Complexes Including Cyclodextrin and Starch (사이클로덱스트린과 전분을 이용한 coenzyme Q10 복합체의 특성 연구)

  • Lee, Joon-Kyoung;Lee, Hyun-Joo;Lim, Jae-Kag
    • Korean Journal of Food Science and Technology
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    • v.46 no.2
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    • pp.180-188
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    • 2014
  • This study focused on assessing the solubility and structural characteristics of two types of coenzyme $Q_{10}$ ($CoQ_{10}$) complexes: the $CoQ_{10}$-starch and the $CoQ_{10}$-cyclodextrin complexes. The solubility of $CoQ_{10}$-starch complex increased significantly as the temperature was increased. However, the solubility of $CoQ_{10}$-cyclodextrin complex reached a peak at $37^{\circ}C$, and strong aggregation occurred at $50^{\circ}C$. When the temperature was raised to $80^{\circ}C$, the $CoQ_{10}$-cyclodextrin complex dissociated owing to the weakening of bonds, resulting in $CoQ_{10}$ emerging at the surface of water. Therefore, $CoQ_{10}$-cyclodextrin complexes have lower solubility, due to their reduced heat-stability, than do the $CoQ_{10}$-starch complexes. Structural differences between the two $CoQ_{10}$ complexes were confirmed by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffractometer (XRD), and differential scanning calorimeter (DSC). The $CoQ_{10}$-cyclodextrin complex included an isoprenoid chain of $CoQ_{10}$, while the $CoQ_{10}$-starch complex included both the benzoquinone ring and the isoprenoid chain of $CoQ_{10}$. These results suggest that $CoQ_{10}$-starch complexes possess higher heat-stability and solubility than do the $CoQ_{10}$-cyclodextrin complexes.

Studies of Crystallographic and Magnetic Properties in Fe0.9Zn0.1Cr2S4 (Fe0.9Zn0.1Cr2S4의 결정학적 및 자기적 성질에 관한 연구)

  • Bae, Sung-Hwan;Kim, Sam-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.34-37
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    • 2007
  • The crystallographic and magnetic properties of $Fe_{0.9}Zn_{0.1}Cr_2S_4$ have been studied by X-ray diffractometer(XRD), vibrating sample magnetometer(VSM) and $M\"{o}ssbauer$ spectroscopy measurement. The crystal structure was determined by the normal cubic spinel of space group Fd3m and the lattice constant was $a_0=9.9967\;{\AA}$. The specific phenomenon which looks like cusp pattern at 77 K was observed in magnetization corves(ZFC : Zero Field Cooling) under 100 Oe applied field. $N\acute{e}el$ temperature($T_N$) was determined to be 153 K by VSM and $M\"{o}ssbauer$ spectra. The asymmetric 8-line profile has been observed at 4.2 K, which was attributed by the colossal electric quadupole interaction(${\Delta}E_Q$), ${\Delta}E_Q$ has 2.22 mm/s at 4.2 K. The ${\Delta}E_Q$ abruptly decreases around 77 K and then it disappears above 77 K with diminishing of 8-line pattern. The isomer shift $\delta$ at room temperature is 0.48 mm/s relative to Fe metal, which means that the charge state of Fe ions is ferrous in character.

Photoeletrochemical Properties of α-Fe2O3 Film Deposited on ITO Prepared by Cathodic Electrodeposition (음극전착법을 이용한 α-Fe2O3 막의 광전기화학적특성)

  • 이은호;주오심;정광덕;최승철
    • Journal of the Korean Ceramic Society
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    • v.40 no.9
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    • pp.842-848
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    • 2003
  • Semiconducting $\alpha$-Fe$_2$O$_3$ film was prepared by the cathodic electrodeposition method on Indium Tin Oxide (ITO) substrate for photoelectrochemical cell application. After heat treatment at 50$0^{\circ}C$, the phase was changed from Fe to $\alpha$-Fe$_2$O$_3$. The phase, morphology, absorbance, and photocurrent density (A/$\textrm{cm}^2$) of the film depended on the preparation conditions: deposition time, applied voltage, and the duration of heat treatment. The $\alpha$-Fe$_2$O$_3$ film was characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscope (SEM), and UV -Visible Spectrophotometer. The stability of the $\alpha$-Fe$_2$O$_3$ film in aqueous solution was tested at zero bias potential under the white-light source of 100 mW/$\textrm{cm}^2$. The apparent grain size of the films formed at -2.0 V was larger than that grown at -2.5 V. The $\alpha$-Fe$_2$O$_3$ film deposited at -2.0 V for 180 s and heat-treated at 50$0^{\circ}C$ for 1 h showed the predominant photocurrent of 834$\mu$A/$\textrm{cm}^2$.

Characteristics and Preparation of Calcium Acetate from Butter Clam (Saxidomus purpuratus) Shell Powder by Response Surface Methodology (반응표면분석법을 이용한 개조개(Saxidomus purpuratus) 패각분말로부터 가용성 초산칼슘의 제조 및 특성)

  • Lee, Hyun Ji;Jung, Nam Young;Park, Sung Hwan;Song, Sang Mok;Kang, Sang In;Kim, Jin-Soo;Heu, Min Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.6
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    • pp.888-895
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    • 2015
  • For effective utilization of butter clam shell as a natural calcium resource, the optimal conditions for preparation of calcium acetate (BCCA) with high solubility were determined using response surface methodology (RSM). The polynomial models developed by RSM for pH, solubility, and yield were highly effective in describing the relationships between factors (P<0.05). Increased molar ratio of calcined powder (BCCP) from butter clam shell led to reduction of solubility, yield, color values, and overall quality. Critical values of multiple response optimization to independent variables were 2.70 M and 1.05 M for acetic acid and BCCP, respectively. The actual values (pH 7.04, 93.0% for solubility and 267.5% for yield) under optimization conditions were similar to predicted values. White indices of BCCAs were in the range of 89.7~93.3. Therefore, color value was improved by calcination and organic acid treatment. Buffering capacity of BCCAs was strong at pH 4.88 to 4.92 upon addition of ~2 mL of 1 N HCl. Calcium content and solubility of BCCAs were 20.7~22.8 g/100 g and 97.2~99.6%, respectively. The patterns of fourier transform infrared spectrometer and X-ray diffractometer analyses from BCCA were identified as calcium acetate monohydrate, and microstructure by field emission scanning electron microscope showed an irregular form.

On the Properties of TLCP/PBT Blends Prepared by In Situ Polymerization in PBT Solution (In situ 중합에 의해서 제조된 TLCP/PBT 블렌드의 특성 연구)

  • Choi, Jae-Kon;Park, Il-Soo;Kim, Sun;Choi, Yoo-Sung;Lee, Eung-Jae;Jo, Byung-Wook
    • Elastomers and Composites
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    • v.39 no.3
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    • pp.217-227
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    • 2004
  • A new thermotropic liquid crystalline polymer(TLCP) containing a triad aromatic ester type mesogenic unit and butylene terephthalate unit(BT) in the main chain was synthesized by polycondensation reaction. The TLCP synthesized showed nematic mesophasic behavior and its transition temperature from solid to mesophase was $260^{\circ}C$. The TLCP/PBT blends were prepared by in-situ polymerization in PBT solution and characterized by differential scanning calorimeter(DSC), thermogavimetric analyzer(TGA), scanning electron microscope(SEM), x-ray diffractometer(XRD), and dynamic mechanical thermal analyze, (DMTA). The blends showed well dispersed TLCP phases with domain sizes $0.05{\sim}0.2{\mu}m$ in the PBT matrix. As the increasing TLCP content from 5 to 20 wt%, ${\Delta}Hm$ values of pure PBT in the blend were increased because TLCP acts as a nucleating agent in the PBT matrix. The mechanical properties of the blends depended on the TLCP contents because the TLCP acted effectively as a reinforcing material in the PBT matrix. The blends showed good interfacial adhesion between the TLCP phase and PBT matrix.The blends prepared by in-situ polymerization showed higher mechanical properties and well dispersed TLCP domains than those of the blends prepared by melt blending.