• Bulletin of the Korean Chemical Society
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• v.35 no.7
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• pp.2043-2048
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• 2014

Two isomers of a new tetraaza macrotricycle 2,2,4,9,9,11-hexaazamethyl-1,5,8,12-tetraazatricyclo[$10.2.2^{5.8}$]-octadecane ($L^2$) containing additional N-$CH_2CH_2$-N linkages, C-meso-$L^2$ and C-racemic-$L^2$, have been prepared by the reaction of 1-bromo-2-chloroethane with C-meso-$L^1$ or C-racemic-$L^1$ ($L^1$ = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane). Both C-meso-$L^2$ and C-racemic-$L^2$ react with copper(II) ion to form $[Cu(C-meso-L^2)]^{2+}$ or $[Cu(C-racemic-L^2)]^{2+}$ in dehydrated ethanol, but do not with nickel(II) ion under similar conditions. Crystal structure of [Cu(C-racemic-$L^2$)($H_2O$)]$(ClO_4)_2$ shows that the complex has distorted square-pyramidal coordination geometry with an apically coordinated water molecule. Unexpectedly, the Cu-N distances [2.016(3)-2.030(3) ${\AA}$] of [Cu(C-racemic-$L^2$)($H_2O$)]$(ClO_4)_2$ are longer than those [1.992(3)-2.000(3) ${\AA}$] of [Cu(C-racemic-$L^1$)($H_2O$)]$(ClO_4)_2$. As a result, $[Cu(C-racemic-L^2)(H_2O)]^{2+}$ exhibits weaker ligand field strength than $[Cu(C-racemic-L^1)(H_2O)]^{2+}$. The copper(II) complexes readily react with CN- ion to yield the cyano-bridged dinuclear complex $[Cu_2(C-meso-L^2)_2CN]^{3+}$ or $[Cu_2(C-racemic-L^2)_2CN]^{3+}$. Spectra and chemical properties of $[Cu(C-meso-L^2)]^{2+}$ and $[Cu_2(C-meso-L^2)_2CN]^{3+}$ are not quite different from those of $[Cu(C-racemic-L^2)]^{2+}$ and $[Cu_2(C-racemic-L^2)_2CN]^{3+}$, respectively.

• Journal of the Korean Ceramic Society
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• v.39 no.9
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• pp.846-850
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• 2002

A PMN-PT-BT/Ag composite was prepared by surface modification with MgO sol with hoping to suppress silver's migration during sintering. The mixture of PbO, $N_2O_5,\;TiO_2\;with\;Mg(NO_3)_2$ instead of MgO was ball milled, the solvent was removed and then the dried powders were calcined at 950$^{\circ}C$/1h. The calcined powder were treated with 3.0 mol% $Ag_2O$ and 1.0 wt% MgO sol and calcined at 550$^{\circ}C$/1h. The dielectrics sintered at 1000$^{\circ}C$/4h under a flowing oxygen showed the density of 7.84g/$cm^3$, the room temperature dielectric constant of 18400, the dielectric loss of 2.4%, the specific resistivity of $0.24{\times}10^{12}{\Omega}{\cdot}cm$. It also showed the bending strength of $120.7{\pm}11.26$ MPa and the fracture toughness of $0.87{\pm}0.002\;MPam^{1/2}$ which were comparable to commercial PZT. The microstructure sonsisted of grains of ∼4${\mu}m$. SEM and SIMS analysis showed that Ag grew as ∼1${\mu}m$ and excess MgO as ∼0.5${\mu}m$.

• 한국신재생에너지학회:학술대회논문집
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• 2006.06a
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• pp.162-165
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• 2006

AZO (ZnO:Al) were fabricated by RF magnetron sputtering In $H_2/Ar(5%\;H_2)$ atmosphere, and structural, electrical and optical properties were investigated. The substrate temperatures were varied at RT, $100^{\circ}C,\;150^{\circ}C$ and$200^{\circ}C$. The resistivity of the films grown in $H_2/Ar(5%\;H_2)$ were reduced from $7.67{\times}10^{-4}{\Omega}\;cm$ to $5.95{\times}10^{-4}{\Omega}\;cm$ comparing that Ar (100%) and the transmittance of the ZnO:Al films in the visible range was 85%.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.2
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• pp.99-104
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• 2017

Refractories used in low-rank coal gasification reactors are usually exposed in a highly corrosive $H_2S$ gas at less than $1000^{\circ}C$, and their mechanical properties such as erosion resistance and fracture strength decline with the exposure time. However, the cause of the degradation of the mechanical properties has little reported yet. In this paper, two kinds of castable refractories with different refractoriness had been exposed in a $H_2O/N_2/H_2S$ mixed gas with high $H_2S$ content for 100 hours at $900^{\circ}C$, and the changes of microstructure, crystalline phases and erosion resistance were compared before and after the corrosion test. The weight of the refractories decreases due to the elution of silica in the specimens after the corrosion test. The capillary porosities of the samples are reduced, but the erosion resistance of the samples is fatally weakened after the corrosion test. There also are changes in constituent phases; dmitryivanovite ($CaAl_2O_4$) and amorphous silica ($SiO_2$) disappear, and gypsum ($CaSO_4{\cdot}2H_2OS$) and kaolinite ($Al_2Si_2O_5(OH)_4$) newly appear after the corrosion test. It is obvious that the phase change from dmitryivanovite that works as a binding agent in the castable refractory to gypsum is the main reason of the degradation of the erosion resistance, because the mechanical properties of gypsum are much poorer than those of dmitryivanovite.

• Korean Journal of Materials Research
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• v.8 no.12
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• pp.1158-1164
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• 1998

Aluminium sulfate solution was prepared by sulfuric acid treatment from gibbsite. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was precipitated from aluminium sulfate solution by adding it into ethylalcohol. From XRD analysis as-prepared $Al_2(SO_4)_3$ · $nH_2O$ was confirmed to have mixed-crystalization water(n=18, 16, 12, 6). The average water of crystalization calculated from thermogravimetry(TG) was 14.7. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was thermally decomposed and converted to $Al_2(SO_4)_3$ at $800^{\circ}C$, $\gamma-Al_2O_3$ at $900-1000^{\circ}C$, and $\alpha-Al_2O_3$ at $1200^{\circ}C$. Ni-doped $\gamma-Al_2O_3$, was synthesized from the slurry of as-prepared $\gamma-Al_2O_3$, with the ratio of [Ni]/[Al]=0.5. The reaction conditions of synthesis were determined as initial pH 9.0 and temperature $80^{\circ}C$ The basicity(pH) of slurry was controlled by using urea and $NH_4OH$ solution. Urea was also used for deposition-precipitation. For determining termination of reaction, the data acquisition was performed by oxidation reduction potential(ORP), conductivity and pH value in the process of reaction. Termination of the reaction was decided by observing the reaction steps and rapid decrease in conductivity. On the other hand, BET(Brunauer, Emmett and Teller) and thermal diffusity of Ni- doped $\gamma-Al_2O_3$, with various content of Ni were measured and compared. Thermal stability of Ni- doped $\gamma-Al_2O_3$ at $1250^{\circ}C$ was confirmed from BET and XRD analysis. The surface state of Ni-doped $\gamma-Al_2O_3$ was investigated by X-ray photoelectron spectroscopy(XPS). The binding energy at $Ni2P_{3/2}$ increased with increasing the formation of $NiAl_2O_4$ phase.

• Journal of the Korean Ceramic Society
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• v.27 no.8
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• pp.1064-1070
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• 1990

ZrO2 fine powders were prepared by hydrolysis, adding 0.1, 0.2, 0.3, 0.4, 0.5, 0.6mol/1H2O/ethanol to 0.1 mol/l Zr(OC3H7)4/ethanol. When hydrolized by adding 0.1mol/l Zr(OC3H7)4/ethanol to 0.1, 0.2mol/l H2O/ethanol., spherical monodispersed ZrO2 fine powders were obtained. And in this condition average sizes were about 0.5, 0.3${\mu}{\textrm}{m}$, respectively. The more H2O/ethanol concentration increased, the more the particle size decreased and the particles were agglomerated strongly. Prepared powders were amorphous and hydrates. The calcined powders with 43$0^{\circ}C$ and 100$0^{\circ}C$ were showed tetragonal and monoclinic phase, respectively.

• Journal of the Korean Ceramic Society
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• v.30 no.8
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• pp.664-670
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• 1993

Potassium tetratitanate (K2Ti4O9) and Potassium hexatitanate (K2Ti6O13) fibers have been prepared by the slow-cooling calcination process in a temperature range from 125$0^{\circ}C$ to 95$0^{\circ}C$ using the K2CO3 and TiO2 as the starting materials. Optimum fiber growth conditions have been also investigated by changing the physical parameters, such as calcination time and temperature, and cooling rate. Relatively long K2Ti4O9 fibers ( 1.2mm) have been grown with quite a high aspect ratio (c/a 500)when the starting material with a nominal composition of K2O and TiO2 with 1:4 was calcined at 115$0^{\circ}C$ for 4h, and then was slowly cooled to 95$0^{\circ}C$ with a rate of 2$0^{\circ}C$/h. In case of a K2O.6TiO2 composition, acicular shaped K2Ti6O13 fibers with 20~300${\mu}{\textrm}{m}$ long and low aspect ratio (c/a 10~15) have been formed irrespective of the coolign rate. The growth condition of fibers have been discussed based upon the phase diagram of K2O-TiOa2.

• Korean Journal of Crystallography
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• v.8 no.2
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• pp.144-148
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• 1997

the molecular and crystal 3-dimensional structure of bentazone, C10H12N2O3S, has been determined from single crystal x-ray diffraction study. Crystal system is monoclinic: a=8.7817(9)Å, b=9.6059(9) Å, c=13.574(9) Å, β=97.269(1)', V=1136.1(6)Å, space group : P21/c, z=4. The molecular structure model was solved by direct method and refined by full matrix least squares. The final reliable factor, R, is 0.045 for 1396 independent reflections(Fo2>4σFo2). A molecule has a staggered conformation with thiocarbazin ring and isopropyl functional group and the molecules by hydrogen bonds are cross stacked along the c-axis.

• Bulletin of the Korean Chemical Society
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• v.31 no.12
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• pp.3745-3748
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• 2010

Pd(II) p-tolylamide Pd(2,6-$(Ph_2PCH_2)_2C_6H_3$)(NH($C_6H_4Me$-p)) (1) was metathetically prepared by the reaction of Pd(2,6-$(Ph_2PCH_2)_2C_6H_3$)Cl with NaNH($C_6H_4Me$-p). Treatment of 1 with carbon dioxide affords the palladium(II) carbamate Pd(2,6-$(Ph_2PCH_2)_2C_6H_3$)(OC(O)NH($C_6H_4Me$-p)) (2), quantitatively. Complex 2 reacts with HX (X = Cl, OTf) to give Pd(2,6-$(Ph_2PCH_2)_2C_6H_3$)X, $NH_2$(p-Tol) and $CO_2$. Reaction of the palladium(II) carbamate with MeI produced Pd(2,6-$(Ph_2PCH_2)_2C_6H_3$)I along with generation of methyl N-tolylcarbamate MeOC(O)NH($C_6H_4Me$-p), exclusively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1997.11a
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• pp.275-278
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• 1997

We investigated effectness of sort and volume of conductive agent to charge/discharge capacity of LiMn$_2$O$_4$. LiMn$_2$O$_4$is prepared by reacting stoichiometric mixture of LiOH . $H_2O$ and MnO$_2$(mole ratio 1 : 2) and heating at 80$0^{\circ}C$ for 24h, 36h, 48h, 60h and 72h. All LiMn$_2$O$_4$cathode active materials show spinel structure. Cathode active materials calcined at 80$0^{\circ}C$ for 36h, charge/discharge characteristics and cycle stability have remarkable advantages. Used that super-s-black and 20wt% as conductive agent in LiMn$_2$O$_4$, it is excellent than property of cathode used Acetylene black or mixture of Super-s-black and acetylene black at charge/discharge capacity and cycle stability. Also, specific efficiency of cathode is excellent as over 98% and that of first cycle is excellent as 92%.