• Bulletin of the Korean Chemical Society
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• v.15 no.5
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• pp.379-386
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• 1994

Reactions of 1',2-bis(diphenylphosphino)-l-(N,N-dimethylaminomethyl)ferrocene (FcNPP) with $M(CO)_6$ (M=Cr, Mo, W) in the presence of TMNO (Trimethylamine oxide) in a stoichiometric ratio of 1 : 1.5 : 3.5 produced a series of Gp 6 metal carbonyl derivatives with a variety of coordination modes: M(CO)$_4({\eta}^2$-FcNPP-P,P) (M=Cr, Mo, W), $M(CO)_5({\eta}^1-FcNPP-P) (M=Mo, W)\;,\; M_2(CO)_9({\eta}^1\;,\;{\eta}^2-FcNPP-P,P,N) (M=Cr, Mo)\;,\;M_2(CO)_{10}({\eta}^1\;,\;{\eta}^1-FcNPP-P,P) (M=Cr, Mo, W)\;, and\;W(CO)_4({\eta}^2-FcNPP(O)-P,N)$. All these complexes were characterized by microanalytical and spectroscopic techniques. In one case, the structure of W(CO)$_4({\eta}^2$-FcNPP(O)-P,N) was determined by X-ray crystallography. Crystals are monocinic, space group P$2_{1/C}$, with a=10.147(2), b=19.902(3), c=19.821(4) ${\AA},\;{\beta}=96.88(2)^{\circ},\;V=3974(l){\AA}^3$, Z=4, and $D_{calc}=1.64 g cm^{-3}$. The geometry around the central tungsten metal is a distorted octahedron, with the nitrogen and phosphorus atoms being cis to each other. Some of these complexes exhibited catalytic activities in the allylic oxidation and epoxidation of cholesterly acetate. Other oxidation products were also formed with the different chemical yields and product distribution depending upon the ligand and the central metal.

• Bulletin of the Korean Chemical Society
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• v.10 no.2
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• pp.191-196
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• 1989

We obtained the new complexes, $Fe{\eta}^4-R,R'-TPSCp](CO)_3$(R,R'-TPSCp = 1,1-disubstituted 2,3,4,5-Tetraphenyl-1-Silacyclopenta-2,4-diene; R = Ph, R' = Cl, R = R' = Cl) from the reaction of the corresponding R,R'-TPSCp with ironpentacarbonyl under reflux in toluene. Also, the analogous complexes with R = R' = Me and R = Me, R' = Cl were obtained in an identical manner. We have determined the crystal structure of $Fe[Ph(Cl)-TPSCp](CO_)3$ by using Mo ka, ${\lambda}$ = 0.71069${\AA}$, where the unit cell was found to be monoclinic with a = 9.042 (6)${\AA}$, b = 19.870 (9)${\AA}$, c = 17.426 (9)${\AA}$ and ${\beta}$ = 96.28(4)$^{\circ}$. The butadiene moiety of TPSCp ring is planar and the dihedral angle of the butadiene plane and C4-Si-C25 plane was opened up to 41.8$^{\circ}$. The C-C distances in the butadiene moiety were found to be 1.4346, 1.462, and 1.440 ${\AA}$, respectively. It may be said that the four ${\pi}$-electrons are delocalized over the four carbons in five membered ring through coordination with ironcarbonyl. In this complex Fe is either in distorted tetrahedron environment with the centroid of the four C-atom butadiene moiety and three carbons of the three carbonyls or in distorted square-pyramidal environment with two midpoints of double bonds of the butadiene moiety and two carbons of carbonyl defining the base of the pyramid and the carbon of remaining carbonyl the apex.

• Oral Biology Research
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• v.42 no.4
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• pp.187-197
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• 2018

Chemical agents such as minocycline (MC) and citric acid (CA) were suggested in the treatment of contaminated implant surface. In this study, MC-HCl treatment was performed to enhance surface characteristics of titanium alloy surface. The purpose of this study was to assess the characteristics and the biocompatibility of Ti-6Al-4V surface treated by MC. Alpha-beta titanium alloy (Ti-6Al-4V) samples were prepared and they were divided into 6 groups according to chemical concentration and treatment time. These groups include 1) group I, non-treated smooth titanium alloy; 2) group II, MC 1.5 mg/mL for 1 hour; 3) group III, MC 1.5 mg/mL for 24 hours; 4) group IV, MC 15 mg/mL for 10 minutes; 5) group V, MC 100 mg/mL for 5 minutes; 6) group VI, pH1 CA for 3 minutes. The analysis of the surface characteristics of MC-treated titanium alloy was executed using scanning electron microscopy, roughness test, and X-ray photoelectron spectroscopy (XPS). Cell adhesion and MTT assay was done using MC3T3 cell. Titanium surfaces treated with MC indicated a more smoothened surface microstructure. For group II and III, the new peaks of rutile TiO2 were found. Group II and V have more basic group of Ti-OH form in XPS. In MTT assay, all MC-treated groups showed significantly higher cell viability compared to control. The surface roughness, crystal structure, surface hydrophilicity, cell viability of smooth titanium surface was improved by MC treatment. Compared with the control experiment and CA-treated group, smooth titanium surface treated with MC showed improved surface characteristics and cell biocompatibility.

• Korean Journal of Materials Research
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• v.34 no.1
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• pp.27-33
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• 2024

Al₂O₃ has excellent sintering properties and is important in semiconductor manufacturing processes that require high-temperature resistance and chemical inertness in a plasma environment. In this study, a comprehensive analysis of the chemical characteristics, physical properties, crystal structure, and dispersion stability of three commercially available Al₂O₃ powders was conducted. The aim was to provide a technological foundation for selecting and utilizing appropriate Al₂O₃ powders in practical applications. All powders exhibited α-Al₂O₃ as the main phase, with the presence of beta-phase Na₂O-11Al₂O₃ as the secondary phase. The highest Na⁺ ion leaching was observed in the aqueous slurry state due to the presence of the secondary phase. Although the average particle size difference among the three powders was not significant, distinct differences in particle size distribution were observed. ALG-1SH showed a broad particle size distribution, P162 exhibited a bimodal distribution, and AES-11 displayed a uniform unimodal distribution. High-concentration Al₂O₃ slurries showed differences in viscosity due to ion release when no dispersant was added, affecting the electrical double-layer thickness. Polycarboxylate was found to effectively enhance the dispersion stability of all three powders. In the dispersion stability analysis, ALG-1SH exhibited the slowest sedimentation tendency, as evidenced by the low TSI value, while P162 showed faster precipitation, influenced by the particle size distribution.

• Composites Research
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• v.31 no.2
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• pp.43-50
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• 2018

The effects of deposition temperature on chemical vapor deposited silicon carbide (CVD-SiC) were studied to obtain high deposition rates and excellent bending strength characteristics. Silicon carbide prepared at $1250{\sim}1400^{\circ}C$ using methyltrichlorosilane(MTS : $CH_3SiCl_3$) by hot-wall CVD showed deposition rates of $95.7{\sim}117.2{\mu}m/hr$. The rate-limiting reaction showed the surface reaction at less than $1300^{\circ}C$, and the mass transfer dominant region at higher temperature. The activation energies calculated by Arrhenius plot were 11.26 kcal/mole and 4.47 kcal/mole, respectively. The surface morphology by the deposition temperature changed from $1250^{\circ}C$ pebble to $1300^{\circ}C$ facet structure and multi-facet structure at above $1350^{\circ}C$. The cross sectional microstructures were columnar at below $1300^{\circ}C$ and isometric at above $1350^{\circ}C$. The crystal phases were all identified as ${\beta}$-SiC, but (220) peak was observed from $1300^{\circ}C$ or higher at $1250^{\circ}C$ (111) and completely changed to (220) at $1400^{\circ}C$. The bending strength showed the maximum value at $1350^{\circ}C$ as densification increased at high temperatures and the microstructure changed from columnar to isometric. On the other hand, at $1400^{\circ}C$, the increasing of grain size and the direction of crystal growth were completely changed from (111) to (220), which is the closest packing face, so the bending strength value seems to have decreased.

• Journal of the Korean Chemical Society
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• v.40 no.1
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• pp.28-36
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• 1996

The pentanuclear complexes have been obtained by the reactions of molybdenum(VI) and tungsten(VI) polynuclear complexes with molybdenum(O) and tungsten(O) dinitrosyl mononuclear complexes, and methylthioamidoxime. The prepared complexes (n-Bu4N)2[Mo4O12Mo(NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2](1), (n-Bu4N)2[W4O12Mo(NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2](2), (n-Bu4N)2[Mo4O12W (NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2] (3) have been characterized by elemental analysis, infrared, UV-visible and 1H NMR spectra. The complexes are elucidated the cis-{M(NO)2}2+(M = Mo, W) unit and a slight delocalization by spectroscopy. The structure of (n-Bu4N)2[W4O12Mo(NO) 2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2] was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P21}a$, a = 22.14(2) $\AA$, b = 14.93(1) $\AA$, c = 23.20(1) $\AA$, $\beta$ = 111.08(6) $\AA$, V = 7155(9) $\AA$, Z = 4, final R = 0.072 for 6191(I > $3\sigma(I)).$ The structure of complex forms two dinuclear [W2O5{CH3SCH2C(NH2)NHO}{CH3SCH2C(NH)NO}] and a central {Mo(NO)2} 2+ core. The geometric structure of the {Mo(NO)2} 2+unit is the formally cistype and C2v symmetry.

• Korean Journal of Materials Research
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• v.10 no.1
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• pp.97-106
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• 2000

In these respects the purpose of this research is manufacturing Co-W-P alloy thin film on the corning glass 2948 by electroless plating method using $NaH_2PO_2H_2O$ (sodium hypophosphite) as a reductant, and analyzing deposition rate, alloy composition, microstructure, and magnetic characteristics at various pH's and temperatures. For Co-P alloy thin film, the reductive deposition reaction occurred only in basic condition, not in acidic condition. The deposition rate increased as the pH and temperature increased, and the optimum condition was found at the pH of 10 and the temperature of 8$0^{\circ}C$. Also magnetic characteristics was found to be most excellent at the pH of 9 and the temperature of 7$0^{\circ}C$, resulting in the coercive force of 870Oe and the squareness of 0.78. At this condition, the contents of P was 2.54% and the thickness of the film was 0.216$\mu\textrm{m}$. For crystal orientation, we could not observe fcc for $\beta$-Co. On the other hand, (1010), (0002), (1011) orientation of hcp for $\alpha$-Co was observed. We could confirm the formation of longitudinal magnetization from dominant (1010) and (1011) orientation of Co-P alloy. For Co-W-P alloy thin film, coercive force was 500Oe and squareness was 0.6. For crystal orientation, (0002) orientation of $\alpha$-Co was dominatly found. Then we could confirm the formation of perpendicular magnetization. The content of P was constant at 0.8$\pm$0.2% and the content of W increased as the concentration of Na$_2$WO$_4$increased. When the concentration of Na$_2$WO$_4$was 0.1mol/L, the composition of W was 20%. We observed the changes of magnetic characteristics and microstructure of thin film depositions of Co-W-P by the heat treatment. For heat treatment, the temperature was increased step by step to 10$0^{\circ}C$, 20$0^{\circ}C$, 30$0^{\circ}C$, and 40$0^{\circ}C$ and it took 1 hour at each step in the reductive condition of hydrogen gas. By the heat treatment, flatness of surface was improved, but there were no changes on the magnetic characteristics and the microstructures.

• Korean Journal of Materials Research
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• v.9 no.3
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• pp.274-281
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• 1999

Usually sputtering and electroless plating methods were used for manufacturing metal-alloy thin film magnetic memory devices. Since electroless plating method has many merits in mass production and product variety com­pared to sputtering method, many researches about electroless plating have been performed in the United State of America and Japan. However, electroless plating method has not been studied frequently in Korea. In these respects the purpose of this research is manufacturing Co-Mn-P alloy thin film on the corning glass 2948 by electroless plating method using sodium hypophosphite as a reductant, and analyzing deposition rate, alloy composition, microstructure, and magnetic characteristics at various pH's and temperatures. For Co-P alloy thin film, the reductive deposition reaction 0$\alpha$urred only in basic condition, not in acidic condition. The deposition rate increased as the pH and temperature increased, and the optimum condition was found at the pH of 10 and the temperature of $80^{\circ}C$. Also magnetic charac­teristics was found to be most excellent at the pH of 9 and the temperature of $70^{\circ}C$, resulting in the coercive force of 8700e and the squareness of 0.78. At this condition, the contents of P was 2.54% and the thickness of the film was $0.216\mu\textrm{m}$. For crystal orientation, we could not observe fcc for $\beta$-Co. On the other hand,(1010), (0002), (1011) orientation of hcp for a-Co was observed. We could confirm the formation of longitudinal magnetization from dominant (1010) and (1011) orientation of Co-P alloy. For Co-Mn-P alloy deposition, coercive force was about 1000e more than that of Co P alloy, but squareness had no difference. For crystal orientation, (l01O) and (lOll) orientation of $\alpha$-Co was dominant as same as that of Co- P alloy. Likewise we could confirm the formation of longitudinal magnetization.

• Journal of the Korean Chemical Society
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• v.45 no.3
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• pp.242-246
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• 2001

The quaternary thiophosphates, $A_2NiP_2S_6$ (A=Rb, Cs), have been synthesized with halide fluxes and structurally characterized by single-crystal X-ray diffraction technique. These compounds crystallize in the space group $C_{2h}^5-P2_1/n$ of the monoclinic system with two formula units in a cell of dimensions a=5.960(2), b=12.323(4), $c=7.491(3)\AA$, $\beta=97.05(3)^{\circ}$, and $V=546.0(3)\AA^3$ for Rb2NiP2S6 and a=5.957(4), b=12.696(7), $c=7.679(4)\AA$, $b=93.60(5)^{\circ}$, and $V=579.7(5)\AA^3$ for $Cs_2NiP_2S_6.$ These compounds are isostructural. The structure of $Cs_2NiP_2S_6$ is made up of one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chains along the a axis and these chains are isolated by $Cs^+$ ions. The Ni atom is octahedrally coordinated by six S atoms. These Ni$S_6$ octahedral units are linked by sharing three m-S atoms of the $[P_2S_6^{4-}]$ anions to form the infinite one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chain. For $Cs_2NiP_2S_6$, the magnetic susceptibility reveals an antiferromagnetic exchange interaction below 8K,which corresponds to the Neel temperature ($T_N$). Above $T_N$, this compound obeys Curie-Weiss law. The magnetic moment, C, and ${\theta}forCs_2NiP_2S_6$ are 2.77 B.M., 0.9593 K, and -19.02 K, respectively. The effective magnetic moment obtained from the magnetic data is agreed with the spin-only value of $Ni^{2+}d^8$(2.83 B.M.) system.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.56 no.9
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• pp.1602-1608
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• 2007

The composites were fabricated, respectively, using 61[vol.%] SiC-39[vol.%] $TiB_2$ and using 61[vol.%] SiC-39[vol.%] $ZrB_2$ powders with the liquid forming additives of 12[wt%] $Al_2O_3+Y_2O_3$ by hot pressing annealing at $1650[^{\circ}C]$ for 4 hours. Reactions between SiC and transition metal $TiB_2$, $ZrB_2$ were not observed in this microstructure. The result of phase analysis of composites by XRD revealed SiC(6H, 3C), $TiB_2$, $ZrB_2$ and $YAG(Al_5Y_3O_{12})$ crystal phase on the Liquid-Phase-Sintered(LPS) $SiC-TiB_2$, and $SiC-ZrB_2$ composite. $\beta\rightarrow\alpha-SiC$ phase transformation was occurred on the $SiC-TiB_2$ and $SiC-ZrB_2$ composite. The relative density, the flexural strength and Young's modulus showed the highest value of 98.57[%], 249.42[MPa] and 91.64[GPa] in $SiC-ZrB_2$ composite at room temperature respectively. The electrical resistivity showed the lowest value of $7.96{\times}10^{-4}[\Omega{\cdot}cm]$ for $SiC-ZrB_2$ composite at $25[^{\circ}C]$. The electrical resistivity of the $SiC-TiB_2$ and $SiC-ZrB_2$ composite was all positive temperature coefficient resistance (PTCR) in the temperature ranges from $25[^{\circ}C]$ to $700[^{\circ}C]$. The resistance temperature coefficient of composite showed the lowest value of $1.319\times10^{-3}/[^{\circ}C]$ for $SiC-ZrB_2$ composite in the temperature ranges from $100[^{\circ}C]$ to $300[^{\circ}C]$ Compositional design and optimization of processing parameters are key factors for controlling and improving the properties of SiC-based electroconductive ceramic composites.