• Journal of the Korean Crystal Growth and Crystal Technology
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• v.34 no.3
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• pp.79-85
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• 2024

We investigated the crystal structural property and chemical bonding nature of cellulose nanocrystal extracted directly from cotton cellulose using high-pressure homogenizer. The nanowire-like cellulose nanocrystals were randomly distributed in the form of a dense mesh. Based on calculating the interplanar distance of the Bragg-diffracted crystal plane observed through X-ray diffraction (XRD) analysis, it was found that the cellulose nanocrystals formed by high-pressure homogenizer had a monoclinc crystal structure, corresponding to the cellulose Iβ sub-polymorph. Solid-state nuclear magnetic resonance (NMR) analysis for the quantitatively evaluation of the amorphous region in cellulose nanocrystals revealed that the crystallinity index of cellulose nanocrystals was calculated to be 53.06 %. The O/C ratio of the surface of cellulose nanocrystal was estimated to be 0.82. Further analysis showed that chemical bonds of C-C bond or C-H bond, C-O bond, O-C-O bond or C=O bond, and O-C=O bond were the main chemical bonding states of the cellulose nanocrystal surface.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2002.11a
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• pp.97-117
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• 2002

A chemoinfometrical method for quantitative determination of crystal content of indomethacin (IMC) polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the conventional powder X-ray diffraction method was performed. Pure $\alpha$ and ${\gamma}$ forms of IMC were prepared using published methods. Powder X-ray diffraction profiles and NIR spectra were recorded for six kinds of standard materials with various content of ${\gamma}$ form IMC. The principal component regression (PCR) analyses were performed based on normalized NIR spectra sets of standard samples of known content of IMC ${\gamma}$ form. A calibration equation was determined to minimize the root mean square error of the prediction. The predicted ${\gamma}$ form content values were reproducible and had a relatively small standard deviation. The values of ${\gamma}$ form content predicted by two methods were in close agreement. The results were indicated that NIR spectroscopy provides for an accurate quantitative analysis of crystallinity in polymorphs compared with the results obtained by conventional powder X-ray diffractometry.

• Journal of the Korean Applied Science and Technology
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• v.31 no.3
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• pp.478-485
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• 2014

This study is to form the self assembly of cubic crystalline phase to penetrate into the skin epidermis. The various performance synthesized diglyceryl phytylacetate (DGPA) having hydroxyl group (-OH) and 4 methyl chains with phytyl group was carried out as an amphoteric lipid such as emulsifying power, self assembly. Emulsifying activity of DGPA was very stabilized on only 1% of small content, it could make a W/O emulsion containing high internal phase incorporated with water. Cubic liquid crystal structure with DGPA on three-phase diagram was formed, when mixed DGPA, dimethicone (2CS), and water. Through three-phase diagram forming the cubic liquid crystal area, hexagonal structure zone, and mixing water phase and hexagonal structure area, reversed micelle area were respectively certified. Its structure was proved by the SAXS (small angled x-ray scattering) analysis. As an application, formation of cubosome containing 10% of magnesium ascorbylphosphate and 5% of pyridoxine tris-hexyldecanoate was encapsulated. Occlusive effect of cubosome had above 1.7 times better than reversed micelle. From using poloxamer of dispersing agent, phase structure recovered from W/O emulsion to cubic liquid crystal phase when storage in $33^{\circ}C$ incubator. Therefore, our this study is expected to be as epidermal-dermal skin absorbers in skin care cosmetics and pharmaceuticals industries as raw materials to form a cubic crystal phase through a more in-depth research to DGPA having amphoteric lipid property.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.19 no.2
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• pp.84-89
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• 2009

The turbid/translucent, near colorless(milky) metamorphic sapphire samples from Sri Lanka have been characterized after the heat treatment in $N_2$ at $1650^{\circ}C$. As-received sapphire specimens became bluish-colored and exhibited more clarity after the heat treatment. It was found that the color change at inclusions zoning region is attributed by the dissolution. As received samples contain the micro/nano inclusions such as rutile($TiO_2$), ilmenite($FeTiO_3$), spinel($MgAl_{2}O_{4}$)/ulvospinel($Fe_{2}TiO_{4}$) and apatite($Ca_5(PO_4)_3$), which were dissolved by the heat treatment and form the blue color through $Fe^{2+}/Ti^{4+}$ charge transferring. The microstructures become different because as the dissolution of apatite($Ca_5(PO_4)_3(OH,F,Cl)$) in alumino silicates($Al_{2}SiO_{5}$) occurred, resulting in morphological change with the appearance of(Ca, Mg, Al) silicate on the surface. Both as-received and heat treated samples showed the rhombohedral crystal structure of $Al_{2}O_{3}$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.2
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• pp.216-223
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• 1997

By using aluminum iso - propoxide($Al(OC_3H_7)_3$, AIP), $Al_2O_3$thin films were deposited on (100) single crystal silicon wafer by MOCVD method. The compositions of deposited films were analysed by electron spectroscopy for chemical analyse(ESCA). The morphology and thickness of the deposited films were characterized by scanning electron microscopy. The refractive index and C-V propertied were studied by using ellipsometery and HP4192A, respectively. From the results of ESCA and SEM analysis at low pressure, more uniform and stable stoichiometric film can be obtained compared with that of atmospheric pressure. For optical film usage, required refractive index can be obtained by heat treatment of deposited film. To improve C -V characteristics in NMOS device, it is requred to control OH-which is mobile charge in oxide, to form $SiO_2$ layer between $Al_2O_3$ and Si by heat treatment.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.1
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• pp.29-35
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• 2012

Special attention in the role of convection in vapor crystal growth has been paid since some single crystals under high gravity acceleration of $10g_0$ appear considerably larger than those under normal gravity acceleration ($1g_0$). With increasing the gravity acceleration from $1g_0$ up to $10g_0$, the total molar flux for ${\Delta}T$ = 30 K increases by a factor of 4, while for ${\Delta}T$ = 90, by a factor of 3. The maximum molar fluxes for three different gravity levels of $1g_0$, $4g_0$ and $10g_0$, appear approximately in the neighborhood of y = 0.5 cm, and the molar fluxes show asymmetrical patterns, which indicate the occurrence of either one single or more than one convective cell. As the gravitational level is enhanced form $1g_0$ up to $10g_0$, the intensity of convection is increased significantly through the maximum molar fluxes for ${\Delta}T$ = 30 K and 90 K. At $10g_0$, the maximum total molar flux is nearly invariant for for ${\Delta}T$ = 30 K and 90 K. The total molar flux increases with increasing the gravity acceleration, for $1g_0{\leq}g_y{\leq}10g_0$, and decreases with increasing the partial pressure of component B, a noble gas called as Kr (Krypton), $P_B$. The ${{\mid}U{\mid}}_{max}$ is directly proportional to the gravity acceleration for 20 Torr $P_B{\leq}300$ Torr. As the partial pressure of $P_B$ (Torr) decreases from 300 Torr to 20 Torr, the slopes of the ${{\mid}U{\mid}}_{max}s$ versus the gravity accelerations increase from 0.29 sec to 0.54 sec, i.e. by a factor of 2. The total molar flux of $Hg_2Cl_2$ is first order exponentially decayed with increasing the partial pressure of component B, $P_B$ (Torr) from 20 Torr up to 300 Torr.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.6
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• pp.232-237
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• 2016

Cocrystallization of active pharmaceutical ingredients has been widely recognized as a versatile tool to regulate the physical properties of pharmaceutical compounds through designed crystal structures. Grinding or milling has been especially useful to screen the feasibility of cocrystal formation, and the addition of a small amount of liquid is routinely necessary. In the present study, the effect of temperature was studied for the milling cocrystallization of ibuprofen and nicotinamide to establish a liquid-free method. The milling-induced cocrystallization was more effective with liquid nitrogen cooling than at room temperature, which was confirmed by XRD and DSC analyses. This behavior was attributed to the limited molecular mobility below the glass transition temperatures of the cocrystal components, which made it effective to destruct the crystals of raw materials and consequently form the ibuprofen/nicotinamide cocrystal. Further studies would be necessary to establish the utility of the current conclusion to the field of pharmaceutical crystallization.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.20 no.4
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• pp.159-163
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• 2010

Co-(0.5 mol%) and Ce-(0~0.3 mol%) doped cubic zirconia ($ZrO_2:Y_2O_3$=64:36 mol%) single crystals grown by a skull melting method were heat-treated in $N_2$ at $1200^{\circ}C$ for 3 hrs. The brown-colored as-grown single crystals were changed into either green or blue color after the heat treatment. Before and after the heat treatment, the YSZ (yttriastabilized zirconia) single crystals were cut for wafer form (${\phi}7mm{\times}t2mm$) and round brilliant cut ($\phi$ 12 mm). The optical and structural properties were examined by UV-VIS spectrophotometer and X-ray diffraction. Absorption by $Ce^{3+}(^2F_{5/2},\;_{7/2}(4f){\rightarrow}^2T_g(5d^1)),\;Co^{2+}(^4A_2(^4F){\rightarrow}^4T_1(^4F)$ or $^4T_1(^4P))$ and $Co^{3+}$, change of ionization energy and lattice parameter were confirmed.

• Bulletin of the Korean Chemical Society
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• v.27 no.11
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• pp.1809-1814
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• 2006

The L-Valinate anion coordinating zinc complex, [$Zn(val)_2(H-2O)$], was isolated and structurally characterized by single crystal X-ray crystallography. The crystal possess orthorhombic symmetry with a space group $P2_12_12_1$, Z = 4, and a = 7.4279(2)$\AA$, b = 9.4342(2)$\AA$, c =20.5862(7)$\AA$ respectively. The compound features a penta-coordinate zinc ion in which the two valine anion molecules are directly coordinating the central zinc metal ion via their N (amine) and O (carboxylate) atoms, and an additional coordination to zinc is made by water molecule (solvent) to form a distorted square pyramidal structure. In addition, further synthesis of the valine capped ZnS:Mn nanocrystal from the reaction of [$Zn(val)_2(H-2O)$] precursor with $Na_2S$ and 1.95 weight % of $Mn^{2+}$ dopant is described. Obtained valine capped nanocrystal was water dispersible and was optically characterized by UV-vis and solution PL spectroscopy. The solution PL spectrum for the valine capped ZnS:Mn nanocrystal showed an excitation peak at 280 nm and a very narrow emission peak at 558 nm respectively. The measured and calculated PL efficiency of the nanocrystal in water was 15.8%. The obtained powders were characterized by XRD, HR-TEM, and EDXS analyses. The particle size of the nanocrystal was also measured via a TEM image. The measured average particle size was 3.3 nm.

• Korean Journal of Materials Research
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• v.6 no.8
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• pp.768-778
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• 1996

Iron oxide (hematite, $\alpha$-${Fe}_{2}{O}_{3}$) particles were prepared directly from aqueous solution using a crystal growth controller. Paticles properties and reaction mechanisum of products as a function of basicity, formation process and mechanism of needle-lkie hematite were investigated. hexagonal hermatite particles were formed in teh range below pH 9.0, ellipsoidal or rectangular hematite particles in the range of pH 10.75-11.75 respectively. In the range above pH 12.50, acicular $\alpha$-FeOOH was formed. Basicity of product solution produced in the range of pH 10.7511.75 was increased slightly as compared with basicity of reastants due to hydroxly ion(OH-) formed by dissociation crystal growth controller. Citric acid which is acted as a crystal growth controller was adsorbed in the form of itrate anion(R-COO-) on the ferric hydroxide and exerted important role on the formation to the needle-like $\alpha$-${Fe}_{2}{O}_{3}$ particles in this reaction system.