• Title/Summary/Keyword: powder X-ray diffraction

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Spectroscopic Identifications and Phase Equilibria of THF + 3-OH THF + CH4 Clathrate Hydrates (삼성분계 THF + 3-OH THF + CH4 크러스레이트 하이드레이트의 상평형 거동 해석 및 분광학적 분석)

  • Kim, Heejoong;Ahn, Yun-Ho;Moon, Seokyoon;Hong, Sujin;Park, Youngjune
    • Korean Chemical Engineering Research
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    • v.55 no.3
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    • pp.353-357
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    • 2017
  • In this study, the inclusion phenomena of tetrahydrofuran + 3-hydroxytetrahydrofuran + $CH_4$ clathrate hydrates were explored via thermodynamic and spectroscopic approaches. The phase equilibria of the double hydrates - THF + $CH_4$ and 3-OH THF + $CH_4$ clathrate hydrates - were determined by pressure-temperature trace during hydrate formation and dissociation, and the result revealed that the equilibrium pressures were shifted to lower pressure region compared to pure $CH_4$ hydrate. The powder X-ray diffraction patterns revealed that the double hydrates of THF + 3-OH THF formed structure II type clathrate hydrates with $CH_4$. The dispersive Raman spectra of the double clathrate hydrates also exhibited that $CH_4$ can be trapped in both $5^{12}6^4$ and $5^{12}$ cages whereas THF and 3-OH THF were encaged in $5^{12}6^4$ cage.

The Effects of Hydration Retarding of Portland Cement by $MgSiF_6.6H_2O$ (규불화마그네슘에 의한 포틀랜드 시멘트의 수화 지연효과)

  • 한상호;이경희;정성철;김남호
    • Journal of the Korean Ceramic Society
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    • v.34 no.2
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    • pp.163-170
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    • 1997
  • The retarding effects of MgSiF6.6H2O on the hydration of portland cement were studied. The setting time, flow value and compressive strength of mortar were measured and the mechanism of retardation was also studied by ion concentration in solution, SEM, BET, and X-ray diffraction. The results are as follows ; 1. Setting time was delayed by the addition of MgSiF6.6H2O. 2. The flow value of mortar decreases depending upon the amount of MgSiF6.6H2O. 3. The compressive strength was almost same or some increase on 28 days hydration. 4. The main retardation mechanism of MgSiF6 on the hydration of portland cement may be explained by the following hypothesis. MgSiF6 depressing the Ca++ and K+ ion concentration of cement paste solution be-cause of the recrystalization of K2SiF6 and CaF2 phase. The new products of K2SiF6 and CaF2 deposit on the surface of unhydrated cement powder and harzard the mass transfer through these layer. The low con-centration of Ca++, K+ ion in solution was decreasing the hydration rate of portland cement.

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Effect of Thermal Annealing for MgGa2Se4 Single Crystal Thin Film Grown by Hot Wall Epitaxy (뜨거운 곁쌓기 법에 의해 성장된 MgGa2Se4 단결정 박막의 열처리 효과)

  • Bang, Jinju;Kim, Hyejeong;Park, Hwangseuk;Kang, Jongwuk;Hong, Kwangjoon
    • Journal of Sensor Science and Technology
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    • v.23 no.1
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    • pp.51-57
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    • 2014
  • The evaporating materials for $MgGa_2Se_4$ single crystal thin films was prepared from horizontal electric furnace. To obtain the single crystal thin films, $MgGa_2Se_4$ compounded polycrystal powder was deposited on thoroughly etched semi-insulated GaAs(100) substrate by the hot wall epitaxy (HWE) method system. The source and substrate temperatures of optimized growth conditions, were $610^{\circ}C$ and $400^{\circ}C$, respectively.The source and substrate temperatures were $610^{\circ}C$ and $400^{\circ}C$, respectively. The crystalline structure of the single crystal thin films was investigated by double crystal X-ray diffraction (DCXD). The temperature dependence of the energy band gap of the $MgGa_2Se_4$ obtained from the absorption spectra was well described by the Varshni's relation, $E_g(T)=2.34\;eV-(8.81{\times}10^{-4}\;eV/K)T^2/(T+251\;K)$. After the as-grown $MgGa_2Se_4$ single crystal thin films was annealed in Mg-, Se-, and Ga-atmospheres, the origin of point defects of $MgGa_2Se_4$ single crystal thin films has been investigated by the photoluminescence (PL) at 10 K. The native defects of $V_{Mg}$, $V_{Se}$ obtained by PL measurements were classified as a donors or acceptors type. And we concluded that the heat-treatment in the Se-atmosphere converted $MgGa_2Se_4$ single crystal thin films to an optical n-type. Also, we confirmed that Ga in $MgGa_2Se_4$/GaAs did not form the native defects because Ga in $MgGa_2Se_4$ single crystal thin films existed in the form of stable bonds.

STUDY ON THE PROPERTIES OF GYPSUM-BONDED DENTAL INVESTMENTS (치과용 석고계 매몰재의 특성에 관한 연구)

  • Kim, Kyoung-Sun;Woo, Yi-Hyung;Choi, Boo-Byung
    • The Journal of Korean Academy of Prosthodontics
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    • v.28 no.1
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    • pp.137-163
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    • 1990
  • The properties of a investment material can be described by the consistency at the slurry state, the setting time, the compressive strength and the thermal expansion during the casting. In this study the effect of the production parameters which are included the ratio of quartz and cristobalite, the content of binder, the water powder ratio and the content and concentration of additives on the Properties of the gypsum-bonded investments has been investigated with help of the consistency test, the vicat needle test, the compressive strength test, the thermal expansion test, x-ray diffraction and DTA thermal differential test. The experimental results showed that the constitution of a investment with W/P ratio of 0.34, 30% of gypsum, 0.8% aluminium sulfate, 2% magnesium sulfate, 0.6% sodium phosphate was adapted for the properties of the KDA Spec. No. 13 type I investment. The important experimental results are summarized as follows. 1. The consistency of the investment decreased with increasing amount of aluminium sulfate and decreasing amount of sodium phosphate. An addition of magnesium sulfate up to 2% an increase of the consistency was shown. But 3% magnesium sulfate in investment showed a decrease of the consistency. The consistency did not vary significantly with a variation of the content of gypsum and cristobalite and the W/P ratio. 2. Aluminium sulfate and the magnesium sulfate promoted the hardening and the aluminium phosphate delayed the hardening. The setting time increased with amount of gypsum. The effect of the matrix on the setting time was insignificant. With the W/P ratio of 0.34 the setting time was 14 min. 3. The compressive strength decreased with the amount of aluminium sulfate up to 0.25% and increased with the amount of aluminium sulfate greater than 3%. The compressive strength decreased as decreasing the amount of magnesium sulfate and gypsum and as increasing the W/P ratio. The effect of the refractory on the compressive strength was also not significant. With the W/P ratio of 0.34 the compressive strength was $34Kg/mm^2$. 4. The 1st thermal expansion was found at the temperature near and the steady state or the contraction stage was found at the temperature between $250^{\circ}C$ and $500^{\circ}C$. After this stage the 2nd thermal expansion took place at the temperature near $500^{\circ}C$. The amount of thermal expansion increased with decreasing the content of magnesium sulfate, aluminium sulfate and gypsum and the W/P ratio. And the amount of thermal expansion increased as the content of sodium phosphate and cristobalite. With the W/P ratio of 0.34 the amount of total expansion was 1.2%.

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Calcium Aluminate Phosphor Supported $TiO_2$ Nanoparticles (산화(酸化)티탄 나노입자(粒子)가 담지(擔持)된 칼슘 알루미늄 형광체(螢光體))

  • Thube, Dilip R.;Kim, Jin-Hwan;Kang, Suk-Min;Ryu, Ho-Jin
    • Resources Recycling
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    • v.18 no.4
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    • pp.24-30
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    • 2009
  • Rare earth based calcium aluminate phosphor ($CaAl_2O_4:Eu^{2+}$, $Nd^{3+}$) supported $TiO_2$ nanoparticles are synthesized by using sol-gel method, which are further characterized using powder X-ray diffraction (XRD), fourier transform infrared (FT-IR), diffuse reflectance UV-Visible spectroscopy (DRS UV-Vis) and transmission electron microscopy (TEM). The XRD pattern of as-prepared and sintered phosphor supported $TiO_2$ does not show the tendency to change the crystal structure from anatase to rutile phase up to $600^{\circ}C$. This indicates that the phosphor support might inhibit the densification and crystallite growth by providing dissimilar boundaries. The diffuse reflectance spectral (DRS) measurements showed shift towards longer wavelength indicating reduction in the band-gap energy as compared to free $TiO_2$. The FT-IR spectra of phosphor supported $TiO_2$ nanoparticles show shift in the peak positions to lower wavelengths. This indicates that the $TiO_2$ nanoparticles are not free, but covalently bonded to the phosphor support. TEM micrographs show presence of crystalline and spherical $TiO_2$ nanoparticles (8 - 15 nm diameter) dispersed uniformly on the surface of phosphor.

Development and Characterization of Horse Bone-derived Natural Calcium Phosphate Powders

  • Jang, Kyoung-Je;Cho, Woo Jae;Seonwoo, Hoon;Kim, Jangho;Lim, Ki Taek;Chung, Pill-Hoon;Chung, Jong Hoon
    • Journal of Biosystems Engineering
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    • v.39 no.2
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    • pp.122-133
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    • 2014
  • Purpose: This study was to develop an effective process for fabricating biocompatible calcium phosphate powders (CPPs) using horse bones, and to investigate the characteristics of them. Methods: The characteristics of horse bone powders (HBPs) were investigated according to the different osseous tissue types (compact bone and cancellous bone), bone types (spine and tibia), pretreatment methods (cold water, $H_2O_2$, and hot water), sintering time (4, 8 and 12h), and sintering temperature (600, 900, 1100 and $1300^{\circ}C$). In addition, the grinding methods were compared based on the wet grinding (ball mill) and dry grinding (blade grinder) method to make it as powders. Finally, their cytotoxicity and cell viability were checked. Results: Regardless of the types of osseous tissues and bones, HBPs were well fabricated as biocompatible CPPs. It was also found that the pretreatment methods did not influence on the resultants, showing well-fabricated HBPs. Considering the processing time, the hot water method was the most suitable compared to other pretreatment methods. Further, 12h-sintering time was sufficient to remove residual organic compounds. The sintering temperatures greatly affected the properties of bone powders fabricated. The x-ray diffraction (XRD) peak of horse bone sintered at $600^{\circ}C$ was most closed to that of hydroxyapatite (HA). Our bioactivity study demonstrated that the HBPs fabricated by sintering horse bones at $1300^{\circ}C$ showed the best performance in terms of cell viability whereas the HBPs $1100^{\circ}C$ showed the cytotoxicity. Conclusions: Using various types of horse bone tissues, biocompatible CPPs were successfully developed. We conclude that the HBPs may have a great potential as biomaterials for various biological applications including bone tissue engineering.

A Study on the Luminescence Properties of LiGd9(SiO4)6O2:Ce3+ (LiGd9(SiO4)6O2:Ce3+ 형광 특성 연구)

  • Jin, Seongjin
    • Journal of the Korean Society of Radiology
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    • v.9 no.3
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    • pp.169-174
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    • 2015
  • $LiGd_9(SiO_4)_6O_2:Ce^{3+}$ phosphors were synthesized by solid-state reaction method. The structural characteristic was investigated by X-ray powder diffraction analysis. The emission and excitation spectra of the $Ce^{3+}$ ions doped $LiGd_9(SiO_4)_6O_2$ phosphors were obtained under the UV excitation. The emission spectra of $LiGd_9(SiO_4)_6O_2:Ce^{3+}$ shows the band at 410 nm corresponding to the $^2F_{5/2}$ and $^2F_{7/2}$ states of $Ce^{3+}$. The red shift of $Ce^{3+}$ emission is found as the $Ce^{3+}$ concentration increases, which could be explained by the change in crystal-field symmetry and strength with increasing $Ce^{3+}$ concentration. Fluorescence decay time of $Ce^{3+}$ was about 20 ns. When the concentration of $Ce^{3+}$ increases life time was slightly reduced.

Effect of Solubilizing and Microemulsifying Excipients in Polyethylene Glycol 6000 Solid Dispersion on Enhanced Dissolution and Bioavailability of Ketoconazole

  • Heo, Min-Young;Piao, Zong-Zhu;Kim, Tae-Wan;Cao, Qing-Ri;Kim, Ae-Ra;Lee, Beom-Jin
    • Archives of Pharmacal Research
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    • v.28 no.5
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    • pp.604-611
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    • 2005
  • Polyethylene glycol (PEG) 6000-based solid dispersions (SDs), by incorporating various pharmaceutical excipients or microemulsion systems, were prepared using a fusion method, t o compare the dissolution rates and bioavailabilities in rats. The amorphous structure of the drug in SDs was also characterized by powder X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). The ketoconazole (KT), as an antifungal agent, was selected as a model drug. The dissolution rate of KT increased when solubilizing excipients were incorporated into the PEG-based SDs. When hydrophilic and lipophilic excipients were combined and incorporated into PEG-based SDs, a remarkable enhancement of the dissolution rate was observed. The PEG-based SDs, incorporating a self microemulsifying drug delivery system (SMEDDS) or microemulsion (ME), were also useful at improving the dissolution rate by forming a microemulsion or dispersible particles within the aqueous medium. However, due to the limited solubilization capacity, these PEG-based SDs showed dissolution rates, below 50% in this study, under sink conditions. The PEG-based SD, with no pharmaceutical excipients incorporated, increased the maximum plasma concentration (C$_{max}$) and area under the plasma concentration curve (AUC$_{0-6h}$) two-fold compared to the drug only. The bioavailability was more pronounced in the cases of solubilizing and microemulsifying PEG-based SDs. The thermograms of the PEG-based SDs showed the characteristic peak of the carrier matrix around 60$^{\circ}C$, without a drug peak, indicating that the drug had changed into an amorphous structure. The diffraction pattern of the pure drug showed the drug to be highly crystalline in nature, as indicated by numerous distinctive peaks. The lack of the numerous distinctive peaks of the drug in the PEG-based SDs demonstrated that a high concentration of the drug molecules was dissolved in the solid-state carrier matrix of the amorphous structure. The utilization of oils, fatty acid and surfactant, or their mixtures, in PEG-based SD could be a useful tool to enhance the dissolution and bioavailability of poorly water-soluble drugs by forming solubilizing and microemulsifying systems when exposed to gastrointestinal fluid.

Preparation of nanoparticles CuInSe2 absorber layer by a non-vacuum process of low cost cryogenic milling (저가의 cryogenic milling 비진공법을 이용한 나노입자 CuInSe2 광흡수층 제조)

  • Kim, Ki-Hyun;Park, Byung-Ok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.2
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    • pp.108-113
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    • 2013
  • Chalcopyrite material $CuInSe_2$ (CIS) is known to be a very prominent absorber layer for high efficiency thin film solar cells. Current interest in the photovoltaic industry is to identify and develop more suitable materials and processes for the fabrication of efficient and cost-effective solar cells. Various processes have been being tried for making a low cost CIS absorber layer, this study obtained the CIS nanoparticles using commercial powder of 6 mm pieces for low cost CIS absorber layer by high frequency ball milling and cryogenic milling. And the CIS absorber layer was prepared by paste coating using milled-CIS nanoparticles in glove box under inert atmosphere. The chalcopyrite $CuInSe_2$ thin films were successfully made after selenization at the substrate temperature of $550^{\circ}C$ in 30 min, CIS solar cell of Al/ZnO/CdS/CIS/Mo structure prepared under various deposition process such as evaporation, sputtering and chemical vapor deposition respectively. Finally, we achieved CIS nanoparticles solar cell of electric efficient 1.74 % of Voc 29 mV, Jsc 35 $mA/cm^2$ FF 17.2 %. The CIS nanoparticles-based absorber layers were characterized by using EDS, XRD and HRSEM.

Optical properties of $Ag_2CdSnSe_4$ and $Ag_2CdSnSe_4:CO^{2+}$ single crystals ($Ag_2CdSnSe_4$$Ag_2CdSnSe_4:Co^{+2}$단결정의 광학적 특성)

  • 이충일
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.16-21
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    • 2001
  • Optical properties of $Ag_2CdSnSe_4$ and $Ag_2CdSnSe_4:Co^{+2}$ quaternary semiconductor single crystals grown by the chemical transport reaction method were investigated. The analysis of the X - ray powder diffraction measurements showed that these crystals have a wurtzite structure with lattice constants a = 4.357 $\AA$, c = 7.380 $\AA$, for $Ag_2CdSnSe_4$ and a = 4.885 $\AA$, c = 7.374 $\AA$, for $Ag_2CdSnSe_4:CO^{2+}$. The direct band gap at 298K, obtained from the optical absorption measurement, is found to be 1.21 eV for $Ag_2CdSnSe_4$ and 1.02 eV for $Ag_2CdSnSe_4:CO^{2+}$. The shrinkage of the band gap due to Co-doping is observed and is about 190 meV, We observed four absorption bands of $Co^{2+}$ ions in two near infrared regions of optical absorption spectra of $Ag_2CdSnSe_4$:$Co^{+2}$. These absorption bands were assigned as due to electronic transitions between the split energy levels of $Co^{2+}$ ions in $T_d$ crystal field under spin-orbit interactions.

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