• Corrosion Science and Technology
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• v.22 no.6
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• pp.393-398
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• 2023

Properties of hafnium nitride (HfN) coatings are affected by deposition conditions, most often by the sputtering technique. Appropriate use of different magnetron sputtering modes allows control of the structural development of the film, thereby enabling adjustment of its properties. This study compared properties of HfN coatings deposited by direct current magnetron sputtering (dcMS), mid-frequency direct current magnetron sputtering (mfMS), and inductively coupled plasma-assisted magnetron sputtering (ICPMS) systems. The microstructure, crystalline, and mechanical properties of these HfN coatings were investigated by field emission electron microscopy, X-ray diffraction, atomic force microscopy, and nanoindentation measurements. HfN coatings deposited using ICPMS showed smooth and highly dense microstructures, whereas those deposited by dcMS showed rough and columnar structures. Crystalline structures of HfN coatings deposited using ICPMS showed a single δ-HfN phase, whereas those deposited using dcMS and mfMS showed a mixed δ-HfN and HfN_0.4 phases. Their performance were increased in the order of dcMS < mfMS < ICPMS, with ICPMS achieving a value of 47.0 GPa, surpassing previously reported results.

• Journal of the Korean Vacuum Society
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• v.10 no.2
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• pp.234-240
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• 2001

The diffusion barrier properties of TiN by using Cu(Mg) alloy film have been investigated. Cu(Mg) alloy film was deposited on air-exposed TiN film. Upon annealing, interfacial MgO of 100 $\AA$ has been formed due to the reaction of Mg with oxygen existed on the surface of TiN. Combined MgO/TiN structure prevented the interdiffusion of Cu and Si up to $800^{\circ}C$. To improve the adhesion of Cu(Mg) alloy film to the TiN, TiN layer was treated by $O_2$ plasma, followed by vacuum annealing at $300^{\circ}C$. It was found that increased oxygen on the surface of TiN film by plasma treatment enhanced segregation of Mg toward the interface, resulting in the formation of dense MgO layer. Improved adhesion characteristics have been formed through this treatment. However, increased power of $O_2$ plasma led to the formation of TiO$_2$ and decreased the Mg content to be segregated to the interface, resulting in the decrease in adhesion property. In addition, the deposition of 50 ${\AA}$ Si on the TiN enhanced the adhesion of Cu(Mg) alloy to TiN without deteriorating the TiN diffusion barrier characteristics.

• Korean Journal of Materials Research
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• v.30 no.7
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• pp.359-368
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• 2020

This study is aimed at improving the plasma resistance of Al₂O₃ ceramics on which plasma resistant YAS(Y₂O₃-Al₂O₃-SiO₂) frit is melt-coated using a simple heat-treatment process. For this purpose, the results of phase analysis and microstructural observations of the prepared YAS frits and the coating layers on the Al₂O₃ ceramics according to the batch compositions are compared and discussed with regard to the results of plasma resistance test. The prepared YAS frits consist of crystalline or amorphous or co-existing crystalline and amorphous phases according to the batch compositions, depending on the role and content of each raw material. The prepared YAS frit is melt-coated on the densely sintered Al₂O₃ ceramics, resulting in a dense coating layer with a thickness of at least ~ 80 ㎛. The YAS coating layer consists of crystalline YAG(Y₃Al₅O₁₂), Y₂Si₂O₇, and Al₂O₃ phases, and YAS glass phase. Plasma resistance of YAS coated Al₂O₃ ceramics is strongly dependent on the content of the YAG(Y₃Al₅O₁₂) and Y₂Si₂O₇ crystalline phases in the coating layer, especially on the content of the YAG phase. Comparing the weight loss of YAS coating ceramics with values obtained for commercial Y₂O₃, Al₂O₃, and quartz ceramics, the plasma resistance of the YAS coating ceramics is 6 times higher than that of quartz, 2 times higher than that of Al₂O₃, and 50 % of the resistance of Y₂O₃.

• Korean Journal of Animal Reproduction
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• v.16 no.1
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• pp.21-38
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• 1992

The present study was carried out to investigate morphologic changes in the corpus luteum of the pregnant rat by electron microscope after administration of prostaglandin F2$\alpha$(PGF2$\alpha$). Pregnant rates were treated with PGF2$\alpha$(1,500$\mu\textrm{g}$/rat) and their corpura lutea were observed morphologically. The results obtained in this study were summarized as follows ; 1. The weight of the ovaries and corpura lutea were decreased slightly at 8~24 hours after PGF2$\alpha$ administratin but no significant differences were observed. 2. The number of corpora lutea and luteal cells decreased slightly at 12~48 hours and 18~24 hours after PGF2$\alpha$ tretment but there were no signifciant differences between control and treatment. 3. The weight of uterus and the unmber of embryo decreased slightly at 96 hours and at 18~96 hours after PGF2$\alpha$ administration but no significant differences were obtained. 4. In the electron microscopic observatons, lipid droplets which are electron dense and appear in the cytoplasm moderately increased in number after PGF2$\alpha$ treatment. The lipid droplets were surrounded by mitochodria and appeared in the autophagic vacuoles. 5. Moderated and high electron dense mitochondria which are round or elongated in shape showed pleomorphism from 3 hours after PGF2$\alpha$ treatment. Destruction of tubular of vesicular cristae was observed at 6 hours after the treatment. Dense body and myelin figures in matrix of mitochondria were also appeared. 6. Well-developed smooth endoplasmic reticulum(sER) showed tubular or vesicular cisternae. A number of whorl membranes containing ribosomes, mitochondria and lipid droplets were observed at 1.5 hour after treatment. sER was abundant in luteal cells at 12 hours were treatment. 7. Well-developed Golgi pparatus appeared obviously 6 hours and more prominently at 12 hours. Those Golgi vesicles were remarkably dilated. 8. Generally, a few rough endoplasmic reticulum (rER) were appeared after treatment and cisternae showed slight dilatation. No differences among the treatments were observed. However, slight dilation of cisternae was observed at 1.5 hours after treatment. 9. Ribosomes composed of free and polyribosomes were abundant before treatment but polyribosomes were appeared at 12 to 24 hours after treatment. 10. Intercellular space were slightly extended at 3 hours and markedly extended at 12 hours. Numerous microvillous protrusions were observed at these times. Membranous multivesicular structures and autophagic vacuoles were also appeared in the intercellular space. 11. At 3 hours after the treatment, autophagic vacuoles appeared in the cytoplasm of the cell. They increased in number with time and were observed to transfer to the intercellular space. Lysosomal dense body appeared in the cytoplasm and the inclusion body was also observed in nucleus at 12 to 24 hours after treatment.

• Korean Journal of Materials Research
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• v.20 no.11
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• pp.559-569
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• 2010

The liquid-phase sintering method was used to prepare a glass lens forming core composed of SiC-$Al_2O_3-Y_2O_3$. Spark plasma sintering was used to obtain dense sintered bodies. The sintering characteristics of different SiC sources and compositions of additives were studied. Results revealed that, owing to its initial larger surface area, $\alpha$-SiC offers sinterability that is superior to that of $\beta$-SiC. A maximum density of $3.32\;g/cm^3$ (theoretical density [TD] of 99.7%) was obtained in $\alpha$-SiC-10 wt% ($6Al_2O_3-4Y_2O_3$) sintered at $1850^{\circ}C$ without high-energy ball milling. The maximum hardness and compression stress of the sintered body reached 2870 Hv and 1110 MPa, respectively. The optimum ultra-precision machining parameters were a grinding speed of 1243 m/min, work spindle rotation rate of 100 rpm, feed rate of 0.5 mm/min, and depth of cut of $0.2\;{\mu}m$. The surface roughnesses of the thus prepared final products were Ra = 4.3 nm and Rt = 55.3 nm for the aspheric lens forming core and Ra = 4.4 nm and Rt = 41.9 for the spherical lens forming core. These values were found to be sufficiently low, and the cores showed good compatibility between SiC and the diamond-like carbon (DLC) coating material. Thus, these glass lens forming cores have great potential for application in the lens industry.

• Journal of Powder Materials
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• v.12 no.6 s.53
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• pp.422-427
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• 2005

The $Al_2O_3$ with various phases were prepared by simple ex-situ hydrolysis and spark plasma sintering (SPS) process of Al powder. The nano bayerite $(\beta-Al(OH)_3)$ phase was derived by hydrolysis of commercial powder of Al with micrometer size, whereas the bohemite (AlO(OH)) phase was obtained by hydrolysis of nano Al powder synthesized by pulsed wire evaporation (PWE) method. Compaction as well as dehydration of both nano bayerite and bohemite was carried out simultaneously by SPS method, which is used to fabricate dense powder compacts with a rapid heating rate of $100^{\circ}C$ per min. under the pressure of 50MPa. After compaction treatment in the temperature ranges from $100^{\circ}C\;to\; 1100^{\circ}C$, the bayerite and bohemite phases change into various alumina phases depending on the compaction temperatures. The bayerite shows phase transition of $Al(OH)_3{\to}{\eta}-Al_2O_3{\to}{\theta}-Al_2O_3{\to}\alpha-Al_2O_3$ sequences. On the other hand, the bohemite experiences the phase transition from AlO(OH) to ${\gamma}-Al_2O_3\;at\;350^{\circ}C.$ It shows AlO(OH) ${\gamma}-Al_2O_3{\to}{\delta}-Al_2O_3{\to}{\alpha}-Al_2O_3$ sequences. The ${\gamma}-Al_2O_3$ compacted at $550^{\circ}C$ shows a high surface area $(138m^2/g)$.

• Journal of the Korean Ceramic Society
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• v.42 no.8 s.279
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• pp.567-574
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• 2005

Densification of SiC powder with additives of total amount of2, 4, 8 $wt\%$ Al-B-C was carried out by Spark Plasma Sintering (SPS). The unique features of the process are the possibilities of a very fast heating rate and a short holding time to obtain fully dense materials. The heating rate and applied pressure were kept at $100^{\circ}C/min$ and 40 MPa, while the sintering temperature and holding time varied from 1700 - $1800^{\circ}C$ for 10 - 40 min, respectively. The SPS-sintered specimens with different amount of Al-B-C at $1800^{\circ}C$ reached near-theoretical density. The $3C{\rightarrow}6H,\;15R{\rightarrow}4H$ phase transformation of SiC was enhanced by increasing the additive amount. The microstructure of SiC sintered up to $1750^{\circ}C$ consisted of fine equiaxed grains. In contrast, the growth of large elongated grains in small matrix grains was shown in sintered bodies at $1800^{\circ}C$, and the plate-like grains interlocking microstructure had been developed by increasing the holding time at $1800^{\circ}C$. The grain growth rate decreases with increasing amount of Al-B-C in SiC starting powder, however, the both of volume fraction and aspect ratio of large grains in sintered body increased.

• Journal of Powder Materials
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• v.20 no.6
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• pp.453-459
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• 2013

Lanthanum/gadolinium zirconate coatings are deposited via suspension plasma spray with suspensions fabricated by a planetary mill and compared with hot-pressed samples via solid-state reaction. With increase in processing time of the planetary mill, the mean size and BET surface area change rapidly in the case of lanthanum oxide powder. By using suspensions of planetary-milled mixture between lanthanum or gadolinium oxide and nano zirconia, dense thick coatings with fully-developed pyrochlore phases are obtained. The possibilities of these SPS-prepared coatings for TBC application are also discussed.

• Journal of the Korean institute of surface engineering
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• v.49 no.6
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• pp.595-603
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• 2016

Rare-earth zirconates, including lanthanum zirconate and gadolinium zirconate, have been investigated as ones of the most promising candidates for next-generation thermal barrier coating (TBC) materials due to their excellent properties such as low thermal conductivity, chemical stability at high temperature and so on. In this study, TBCs with three compositions, in the $La_2O_3-Gd_2O_3-ZrO_2$ system with reduced rare-earth contents from $RE_2Zr_2O_7$ compositions, were fabricated by using suspension plasma spray with different suspension preparation methods. The phase formation, microstructure, and thermal properties of TBCs were examined. In particular, each coating exhibited single fluorite phase and a dense, vertically-separated microstructure. The potential of coatings with rare-earth zirconates for TBC applications was also discussed.

• Journal of the Korean Ceramic Society
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• v.51 no.6
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• pp.598-604
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• 2014

Considerable research efforts have been explored attempting to enhance the thermal durability of thermal barrier coatings (TBCs) at the high operating temperatures of gas turbines. In this study, the suspension plasma spray (SPS) process was applied to produce TBCs with a segmented structure by using an yttria-stabilized zirconia (YSZ) suspension. Four different experiment sets were carried out by controlling the ratio between surface roughness of the bond coat and feed stock size ($R_a/D_{50}$) in order to examine the effect of $R_a/D_{50}$ ratio on the microstructure of SPS-prepared coatings. When the $R_a/D_{50}$ had a high value of 11.8, a deposited thick coating turned out to have a cone-type columnar microstructure. In contrast, at the low $R_a/D_{50}$ values of 2.9 and 0.18, a deposited thick coating appeared to have a dense, vertically-cracked microstructure. However, with the very low $R_a/D_{50}$ value of 0.05 the coating was delaminated.