• 한국세라믹학회지
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• 제21권3호
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• pp.231-238
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• 1984

Heavy metal fluoride glasses exhibit considerable promise as high transparency materials from the UV to the IR. These glasses are prepared by fusion of the mixture of metal fulorides($ZrF_4$, $BaF_2$, $LaF_3$ etc) at 800-1, 00$0^{\circ}C$ under the inert$(N_2)$ or reactive ($CCl_4$, $Cl_2$) atmosphere following the casting into glass on cooling. Infrared absorption at the 3, 400 cm-1 -OH peak has been measured as a function of thickness for several ZrF-$BaF_2$-LaF and $HfF_4$-$BaF_2$-$LaF_3$ glasses to separate contributions from bulk and surface -OH. For glasses melted under $CCl_4$ reactive atmosphere the peak is due almost entirely to surface-OH. and melting in a closed reactor was best for removing -OH. In ambient atmosphere the -OH peak exhibited no time dependence over a 30 d period indicating a very small rate of surface attack by atmospheric H2O. Removal of -OH absorption processing was generally easier and more complete for the $BaF_2$/ThF4-glasses than for the $ZrF_4$-or $HfF_4$-based glasses.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3444-3450
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• 2013

Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

• 한국재료학회지
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• 제14권2호
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• pp.141-145
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• 2004

Silicon nitride thin films were deposited by atomic layer deposition (ALD) technique in a batch-type reactor by alternating exposures of precursors. XJAKO200414714156408$_4$ or$ SiH_2$$Cl_2$ was used as the Si precursor, $NH_3$ was used as the N precursor, and the deposited films were characterized comparatively. The thickness of the film linearly increased with the number of deposition cycles, so that the thickness of the film can be precisely controlled by adjusting the number of cycles. As compared with the deposition using$ SiCl_4$, the deposition using $SiH_2$$Cl_2$ exhibited larger deposition rate at lower precursor exposures, and the deposited films using $SiH_2$$Cl_2$ had lower wet etch rate in a diluted HF solution. Silicon nitride films with the Si:N ratio of approximately 1:1 were obtained using either Si precursors at $500^{\circ}C$, however, the films deposited using $SiH_2$$Cl_2$ exhibited higher concentration of H as compared with those of the $SiC_4$ case. Silicon nitride thin films deposited by ALD showed similar physical properties, such as composition or integrity, with the silicon nitride films deposited by low-pressure chemical vapor deposition, lowering deposition temperature by more than $200^{\circ}C$.

• Bulletin of the Korean Chemical Society
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• 제26권11호
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• pp.1795-1802
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• 2005

Potential energy curves and internuclear (M-X) distance variations for dissociation reactions of $[MX_4]^{2-}$ into ($[MX_3]^-$ + $X^-$) have been calculated using ab initio Hartree-Fock (HF), second order M$\ddot{o}$ller-Plesset perturbation (MP2), and Density Functional Theory (DFT) methods with a triple zeta plus polarization (TZP) basis set. The equilibrium geometrical structures of $[MX_4]^{2-}$ are optimized to tetrahedral geometry for $[NiX_4]^{2-}$ and square planar geometry for ($[PdX_4]^{2-}$ and $[PtX_4]^{2-}$). The bond (M-X) distances of $[NiCl_4]^{2-}$, $[NiBr_4]^{2-}$, $[PdCl_4]^{2-}$, $[PdBr_4]^{2-}$, $[PtCl_4]^{2-}$, and $[PtBr_4]^{2-}$ at the DFT level are 2.258, 2.332, 2.351, 2.476, 2.367, and 2.493 $\AA$, respectively. The dissociation energies for the bond dissociation of ($[MX_3]^-$${\cdot}{\cdot}{\cdot}$$X^-$) at the DFT level are found to be 4.73 eV for $[NiCl_4]^{2-}$, 4.89 eV for $[NiBr_4]^{2-}$, 4.93 eV for $[PdCl_4]^{2-}$, 5.57 eV for $[PdBr_4]^{2-}$, 5.44 eV for $[PtCl_4]^{2-}$, and 5.87 eV for $[PtBr_4]^{2-}$. As the (M${\cdot}{\cdot}{\cdot}$X) distance of ($[MX_3]^-$${\cdot}{\cdot}{\cdot}$$X^-$) increases, the distance variation (Rt) of trans (M-X) bond at the trans-position is shorter than those (Rc) of two cis (M-X) bonds at the cisposition. Simultaneously the atomic charge variation of trans-X atom is more positive than those of equilibrium $[MX_4]^{2-}$ structures, while the variation of leaving X group is more positive.

• 한국재료학회지
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• 제22권5호
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• pp.243-248
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• 2012

ZrN nanoparticles were prepared by an exothermic reduction of $ZrCl_4$ with $NaN_3$ in the presence of NaCl flux in a nitrogen atmosphere. Using a solid-state combustion approach, we have demonstrated that the zirconium nitride nanoparticles synthesis process can be completed in only several minutes compared with a few hours for previous synthesis approaches. The chemistry of the combustion process is not complex and is based on a metathesis reaction between $ZrCl_4$ and $NaN_3$. Because of the low melting and boiling points of the raw materials it was possible to synthesize the ZrN phase at low combustion temperatures. It was shown that the combustion temperature and the size of the particles can be readily controlled by tuning the concentration of the NaCl flux. The results show that an increase in the NaCl concentration (from 2 to 13 M) results in a temperature decrease from 1280 to $750^{\circ}C$. ZrN nanoparticles have a high surface area (50-70 $m^2/g$), narrow pore size distribution, and nano-particle size between 10 and 30 nm. The activation energy, which can be extracted from the experimental combustion temperature data, is: E = 20 kcal/mol. The method reported here is self-sustaining, rapid, and can be scaled up for a large scale production of a transition metal nitride nanoparticle system (TiN, TaN, HfN, etc.) with suitable halide salts and alkali metal azide.

• 공업화학
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• 제4권2호
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• pp.318-323
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• 1993

CFC-11$(CFCl_3)$의 대체품인 HCFC-123$(CF_3CHCl_2)$의 합성을 위하여 Pentachloroethane($CHCl_2CCl_3$)을 제조하고, 이것을 antimony pentahalide 촉매의 존재하에서 불화수소와 반응시켰다. $CHCl_2CCl_3$의 불소화 반응은 촉매와 반응물간의 Cl-F교환 mechanism에 의해 진행되었으며 $CHCl_2CCl_3$의 불화도는 반응온도가 높을수록 증가하는 경향을 보여 주었다. 촉매농도 또한 생성물의 불화도에 영향을 미치나 반응온도에 비해 상대적으로 낮았다. $CCl_3CFCl_2$, $CFCl_2CFCl_2$, $CF_2ClCFCl_2$와 같은 부산물의 생성원인을 규명하기 위한 실험을 실시하여 부산물 생성 mechanism을 제안하였다.

• 전기화학회지
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• 제5권4호
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• pp.183-188
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• 2002

The structure of species formed in $NbCI_5-I-ethyl-3-methylimidazolium$ chloride (EMIC) room-temperature molten salt (RTMS) was examined with the Raman spectroscopic measurement and ab initio molecular orbital calculation. The equilibrium structures of $NbCl_5,\;NbCl_6^-,\;Nb_2CI_{10},\;Nb_2CI_{11}^-,\;Nb_3CI_6^-,\;NbCI_6^--EMI^+\;(in\;which\;NbCI_6^-$ anion approaches $EMI^+$ cation with strong interaction) and $Nb_2CI_{11}^--EMI^+$ were obtained with the HF/LANL2DZ level of calculation. The harmonic frequencies at each equilibrium structure were compared with Raman spectra. The harmonic frequencies of $NbCI_6^--EMI^+,\; Nb_2CI_{11}^--EMI^+,\;and\;Nb_2CI_{10}$ were in good agreement with the Raman spectra of RTMS melts. In the $NbCI_5-EMIC RTMS$, the main species were $NbCI_6^-\;and\;EMI^+$. In the $NbCl_5-EMIC$ RTMS added $NbCl_5\;over\;50mol\%$, small amount of $Nb_2CI_{11}^-\;and\; Nb_2CI_{10}$ were also formed. The structures of anions and cation in the RTMS distorted from free ions with Coulomb force.

• Bulletin of the Korean Chemical Society
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• 제17권12호
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• pp.1149-1153
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• 1996

Ab initio and extended Huckel calculations were carried out on the isomers of trans-RhCl(η2-C2H2)(PH3)2 (1). Due to π-back donation in 1 complex, the rotational energy barrier of alkyne ligand is computed to be in the range of 18.6-25.2 kcal/mol at MP4 levels. The optimized hydrido-alkynyl complex (2) at ab initio level has the distorted trigonal bipyramidal structure. Vinylidene complex (3) is computed to be more stable than 1 complex by 17.1 kcal/mol at MP4//MP2 level. The stabilities of isomers show similar trend at the various level calculations, that is, EHT, MP4//HF, and MP4//MP2 levels. The optimized geometries at ab initio level are in reasonable agreement with experimental data. A detailed account of the bonding in each isomers (1-3) have been carried out in terms of orbital analyses.

• 한국재료학회:학술대회논문집
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• 한국재료학회 1992년도 춘계학술발표회
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• pp.26-27
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• 1992

반도체 기억소자 contact hole의 선택적 충진의 최적 조건을 연구하기 위하여 무전해Ni도금방법을 채택하여 실리콘의 활성화와 선택적 도금의 공정조건이 Contact Hole 도금피막의 제반 특성에 미치는 영향을 조사하였다. p형 실리콘 100 소지 표면의 활성화 처리는 RCA처리에 의해 먼저 표면을 세척한 다음 온도, PdCl$_2$농도, 시간. 교반의 영향을 조사하였다 전처리의 최적조건은 7$0^{\circ}C$, 0.5M HF, ImM PdCl$_2$, 2mM EDTA, 90second이었다. 무전해도금은 NiS0$_4$.6$H_2O$를 DMAB를 환원제로 하여 온도, DMAB 농도, pH, 도금시간의 영향을 조사하였다. 무전해 도금 피막은 비교적 우수한 접촉저 항을 나타냈다. 1$\mu$m의 도금막을 얻는 데 본 실험조건에서 DMAB의 농도가 8mM일 때 30 분이 소요되었다. 도금막의 표면은 온도가 낮을수록 pH가 높을수록 평활하였고,특히 온도 6$0^{\circ}C$와 pH6.8에서 가장 우수하였다. 미세경도는 600Hv 정도였으며, 결정립의 크기 가 증가할수록 저항과 미세경도가 감소하였다.

• 전기의세계
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• 제28권9호
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• pp.43-50
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• 1979

Silicon nitride films were chemically deposited on silicon substrates by reacting SiCl$_{4}$ and NH$_{3}$ in a nitrogen atmosphere at 700~1100 .deg.C. The deposition rate increased rapidly with deposition temperature upto about 1000 .deg.C, and became less temperature dependent above this temperature. The etch rate of films in buffered HF solution decreased, with an increase of deposition temperature, and a heat treatment at a temperature higher than that of the deposition considerably reduced the etch rate. It indicates that the heat treatment resulted in a densification of the films. Surface charge density of 3~4 * 10$^{11}$ /cm$^{2}$ was determined from the C-V characteristics of MNS diode, and it was also found that surface charge density depended on deposition temperature, but not film thickness. The current-voltage characteristics displayed a logI-V$^{1}$2/ dependence in the temperature range of 300~500.deg.K. Measurement of the slope of this characteristics and its dependence on temperature and bias polarity suggest that conduction in sili con nitride films arises from the Poole-Frenkel mechanism.