• Journal of Pharmaceutical Investigation
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• v.35 no.2
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• pp.89-94
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• 2005

The micron or nano-sized lysozyme as a model protein drug was prepared using solution enhanced dispersion by supercritical fluid (SEDS) process at various conditions (e.g., solvent, temperature and pressure) to investigate the feasibility of pulmonary protein drug delivery. The lysozyme particles prepared were characterized by laser diffraction particle size analyzer, scanning electron microscopy (SEM) and powder X-ray diffractometry (PXRD). The biological activity of lysozyme particles after/before SEDS process was also examined. Lysozyme was precipitated as spherical particles. The precipitated particles consisted of 100 - 200 nm particles. Particle size showed the precipitates to be agglomerates with primary particles of size $1\;-\;5 \;{\mu}m$. The biological activity varied between 38 and 98% depending on the experimental conditions. There was no significant difference between untreated lysozyme and lysozyme after SEDS process in PXRD analysis. Therefore, the SEDS process could be a novel method to prepare micron or nano-sized lysozyme particles, with minimal loss of biological activity, for the pulmonary delivery of protein drug.

• Bulletin of the Korean Chemical Society
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• v.33 no.6
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• pp.1845-1850
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• 2012

Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.

• Journal of Powder Materials
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• v.30 no.5
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• pp.431-435
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• 2023

An irradiation hardening of Inconel 718 produced by selective laser melting (SLM) was studied based on the microstructural observation and mechanical behavior. Ion irradiation for emulating neutron irradiation has been proposed owing to advantages such as low radiation emission and short experimental periods. To prevent softening caused by the dissolution of γ' and γ" precipitates due to irradiation, only solution annealing (SA) was performed. SLM SA Inconel 718 specimen was ion irradiated to demonstrate the difference in microstructure and mechanical properties between the irradiated and non-irradiated specimens. After exposing specimens to Fe³⁺ ions irradiation up to 100 dpa (displacement per atom) at an ambient temperature, the hardness of irradiated specimens was measured by nano-indentation as a function of depth. The depth distribution profile of Fe³⁺ and dpa were calculated by the Monte Carlo SRIM (Stopping and Range of Ions in Matter)-2013 code under the assumption of the displacement threshold energy of 40 eV. A transmission electron microscope was utilized to observe the formation of irradiation defects such as dislocation loops. This study reveals that the Frank partial dislocation loops induce irradiation hardening of SLM SA Inconel 718 specimens.

• Journal of the Korean Society for Heat Treatment
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• v.28 no.1
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• pp.17-23
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• 2015

Hydroxyapatite coatings were fabricated by a room temperature spray method on zirconia substrates and the influence of heat-treatment on their microstructure was also investigated. Phase composition of coated hydroxyapatite films was similar to the starting powder, but the grain size of hydroxyapatite particles was reduced to the size of nano-scale about 100 nm. Grain size, particle compactness, and adhesiveness to zirconia of hydroxyapatite coatings were increased with heat-treatment temperature, but some of cracks by heat-treatment above $1100^{\circ}C$ were initiated between hydroxyapatite coatings and zirconia substrate. Heat-treated hydroxyapatite layers show the dissolution in SBF solution for 5 days. Hydroxyapatite-coated specimen heat-treated at $1100^{\circ}C$ for 1 h has a good biocompatibility, which specimen induced the nanocrystalline hydroxyapatite precipitates on the coating surface by the immersion in SBF solution for 5 days.

• Korean Journal of Materials Research
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• v.26 no.5
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• pp.235-240
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• 2016

Appropriate thermo-mechanical properties of nickel-based superalloys are achieved by heat treatment, which induces precipitation and solid solution hardening; thus, information on the temperature ranges of precipitation and dissolution of the precipitates is essential for the determination of the heat treatment condition. In this study, thermal analyses of nickel-based superalloys were performed by differential scanning calorimetry method under conditions of various heating rates of 5, 10, 20, or 40K/min in a temperature range of 298~1573K. Precipitation and dissolution temperatures were determined by measuring peak temperatures, constructing trend lines, and extrapolating those lines to the zero heating rate to find the exact temperature under isothermal condition. Determined temperatures for the precipitation reactions were 813, 952, and 1062K. Determined onset, peak, and offset temperatures of the first dissolution reaction were 1302, 1388, and 1406K, respectively, and those values of the second dissolution reaction were 1405, 1414, and 1462K. Determined solvus temperature was 1462K. The study showed that it was possible to use a simple method to obtain accurate phase transition temperatures under isothermal condition.

• Proceedings of the Korean Society for Technology of Plasticity Conference
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• 2001.05a
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• pp.147-150
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• 2001

The ARB (Accumulative Rolling Bonding) Process was applied to a 6061 Al alloy to obtain ultra-fine grains. After 4 ARB cycles at $315^{\circ}C$, original equilibrium large grains were transformed to ultra-fine grains of several hundred nano-meter size with nonequilibrium grain boundaries. At lower number of cycles, microsutcture of highly-tangled dislocation cells were observed. Large grains and coarsened precipitates filled the microstructure of specimens experienced ARB cycles more than 5. Sliding wear tests using a pin-on-disk type wear tester were conducted on the ARB processed 6061 Al alloy plate. Wear rates of the 6061 Al alloy increased with the increase of ARB cycle number as well as the applied load. Worn surfaces and debris, cross-sections of the worn specimen were examined with scanning electron microscopy (SEM) to investigate the wear mechanism of the ultra-fine grained 6061 Al Tensile properties of the 6061 Al alloy were also studied and used to correlate the wear test results with the microstructures, which evolved continuously with the number of ARB cycles.

• Journal of the Korean Society for Heat Treatment
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• v.23 no.6
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• pp.309-314
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• 2010

Microstructures and grain growth behaviors at elevated temperatures have been investigated for extruded Mg-2%Zn and Mg-2%Zn-0.3%Zr alloys, in order to clarify the role of Zr in grain stability of Mg-Zn alloy. The grain size of Zr-free alloy increased continuously with an increase in annealing temperature, when isochronally annealed for 60 min from 573 to 723K, while the grains of the Zr-containing alloy were relatively stable up to 723 K. The activation energies for grain growth ($E_g$) between 573 and 723 K were calculated as 77.8 and 118.6 kJ/mole for the Mg-2%Zn and Mg-2%Zn-0.3%Zr alloys, respectively, which indicates that grains in the Zr-added alloy possess higher thermal stabilities at elevated temperatures. TEM observations on the annealed Mg-2%Zn and Mg-2%Zn-0.3%Zr alloys revealed that enhanced grain stability resulting from Zr addition into Mg-Zn alloy would be ascribed to the restriction of grain growth by stable Zn-Zr nano-precipitates distributed in the microstructure.

• Journal of Welding and Joining
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• v.33 no.5
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• pp.26-30
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• 2015

Hastelloy X in this study was applied in jet engine F-15 air fighter as shroud to isolate the engine from outer skin. After 15 years operation at elevated temperature the mechanical properties decreased gradually due to the precipitation of continues second phases in the grain boundaries and precipitated inside the grain. The crack happened at the edge of the shroud due to the thermal and mechanical stress from jet engine. Selective TEM analysis found that the grain boundaries consist of $M_{23}C_6$ carbide, $M_6$ Ccarbide and small percentage of sigma(${\sigma}$) phase. Furthermore, it was confirmed the nano size of ${\sigma}$ and miu (${\mu}$) phase inside the grain. In this study, it was investigated the microstructure of the degraded shroud component and HAZ of repair welded shroud. In the HAZ, it was observed the dissolution of the $M_{23}C_6$ carbides and smaller precipitates, the migration of the undissolved larger $M_{23}C_6$ carbide and $M_6$ Ccarbide. It is also observed the liquation due to the simply melt of the segregated precipitates in the grain boundaries. Interestingly, the segregated second phases which simply melt in the grain boundaries more easily happened at higher heat input welding condition. High temperature tensile test was done at $300^{\circ}C$, $700^{\circ}C$ and $900^{\circ}C$. It was obtained that the toughness of welded sample is lower compare to the non-welded sample. The solution heat treatment at $1170^{\circ}C$ for 5 minutes was suggested to obtain a better mechanical properties of the shroud. The high cycle fatigue number of the repair welded shroud shows a much lower compare to the shroud. In addition, the high cycle fatigue number at room temperature after solution heat treatment was almost double compare to the before solution heat treatment under 420-500MPa stress amplitude. However, the high cycle fatigue number of repaired welded sample was shown a much lower compare to the non- welded shroud and solution treated shroud. One of the main reasons to decrease the tensile strength and the high cycle fatigue properties of the repair welded shroud is the formation of the liquid phase in HAZ.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.5
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• pp.175-180
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• 2016

ZnO nanoparticles were synthesized by aqueous preparation routes of a precipitation and a hydrothermal process. In the processes, the powders were formed by mixing aqueous solutions of Zn-nitrate hexahydrate ($Zn(NO_3)_2{\cdot}6H_2O$) with NaOH aqueous solution under controlled reaction conditions such as Zn precursor concentration, reaction pH and temperature. Single ZnO phase has been obtained under low Zn precursor concentration, high reaction pH and high temperature. The synthesized particles exhibited flakes (plates), multipods or rods morphologies and the crystallite sizes and shapes would be efficiently controllable by changing the processing parameters. The hydrothermal method showed advantageous features over the precipitation process, allowing the precipitates of single ZnO phase with higher crystallinity at relatively low temperatures below $100^{\circ}C$ under a wider pH range for the Zn precursor concentration of 0.1~1 M.

• Korean Journal of Materials Research
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• v.30 no.10
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• pp.542-549
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• 2020

Effects of Sc addition on microstructure, electrical conductivity, thermal conductivity and mechanical properties of the as-cast and as-extruded Al-2Zn-1Cu-0.3Mg-xSc (x = 0, 0.25, 0.5 wt%) alloys are investigated. The average grain size of the as-cast Al-2Zn-1Cu-0.3Mg alloy is 2,334 ㎛; however, this value drops to 914 and 529 ㎛ with addition of Sc element at 0.25 wt% and 0.5 wt%, respectively. This grain refinement is due to primary Al₃Sc phase forming during solidification. The as-extruded Al-2Zn-1Cu-0.3Mg alloy has a recrystallization structure consisting of almost equiaxed grains. However, the as-extruded Sc-containing alloys consist of grains that are extremely elongated in the extrusion direction. In addition, it is found that the proportion of low-angle grain boundaries below 15 degree is dominant. This is because the addition of Sc results in the formation of coherent and nano-scale Al₃Sc phases during hot extrusion, inhibiting the process of recrystallization and improving the strength by pinning of dislocations and the formation of subgrain boundaries. The maximum values of the yield and tensile strength are 126 MPa and 215 MPa for the as-extruded Al-2Zn-1Cu-0.3Mg-0.25Sc alloy, respectively. The increase in strength is probably due to the existence of nano-scale Al₃Sc precipitates and dense Al₂Cu phases. Thermal conductivity of the as-cast Al-2Zn-1Cu-0.3Mg-xSc alloy is reduced to 204, 187 and 183 W/MK by additions of elemental Sc of 0, 0.25 and 0.5 wt%, respectively. On the other hand, the thermal conductivity of the as-extruded Al-2Zn-1Cu-0.3Mg-xSc alloy is about 200 W/Mk regardless of the content of Sc. This is because of the formation of coherent Al₃Sc phase, which decreases Sc content and causes extremely high electrical resistivity.