• Journal of the Korean Ceramic Society
• /
• v.28 no.4
• /
• pp.315-323
• /
• 1991

The preparation of zirconium carbide powders by the halogenide process of ZrCl4-C-Mg system (1:1:2, molar ratio) was studied between 300。 and 120$0^{\circ}C$ under Ar gas flow (200 mι/min). The formation mechanism and kinetics of zirconium carbide and characteristics of the synthesized powder were examined by TG-DTA, XRD, SEM and PSA. 1) The formation mechanism of zirconium carbide were as follows, above 30$0^{\circ}C$ ZrCl4(S)+Mg(s)longrightarrowZrCl2(s)+MgCl2(s) above 40$0^{\circ}C$ ZrCl2(S)+Mg(s)longrightarrowZr(s)+MgCl2(s) above 50$0^{\circ}C$ Zr(s)+C(s)longrightarrowZrC(s) 2) The apparent activation energy of the reduction-carbonization at temperature of 800$^{\circ}$to 100$0^{\circ}C$ was 11.9 kcal/mol. 3) The lattice parameter and the crystallite size of ZrC which was produced from the mixture powder of ZrCl4, C and Mg (1:1:2, molar ratio) at 100$0^{\circ}C$ for 1 h were 4.700A and 180A, respectively. 4) The powders obtained from the mixture powder of ZrCl4, C and Mg(1:1:2, molar ratio) at 100$0^{\circ}C$ for 1 h were agglomerate with the average size of about 13${\mu}{\textrm}{m}$ in SEM micrograph.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.4
• /
• pp.1221-1224
• /
• 2013

The atomic layer deposition (ALD) of $ZrO_2$ was conducted in ultrahigh vacuum (UHV) conditions. The surface was exposed to $ZrCl_4$ and $H_2O$ in sequence and the surface species produced after each step were identified in situ with X-ray photoelectron spectroscopy (XPS). $ZrCl_4$ is molecularly adsorbed at 140 K on the $SiO_2$/Si(111) surface covered with OH groups. When the surface is heated to 300 K, $ZrCl_4$ loses two Cl atoms to produce $ZrCl_2$ species. Remaining Cl atoms of $ZrCl_2$ species can be completely removed by exposing the surface to $H_2O$ at 300 K followed by heating to 600 K. The layer-by-layer deposition of $ZrO_2$ was successfully accomplished by repeated cycles of $ZrCl_4$ dosing and $H_2O$ treatment.

• Polymer(Korea)
• /
• v.39 no.1
• /
• pp.169-173
• /
• 2015

Metallocene was supported on the silica, which was functionalized with aminosilanes such as aminopropyltrimethoxysilane (1NS) or N-[3-(trimethoxysilyl)propyl]ethylenediamine (2NS), and ionic liquids such as 1-butyl-4-methylpyridinium chloride (Cl), tributylmethylammonium chloride (Amm), benzyldimethyltetradecylammonium chloride (Ben), 1-butyl-1-methylpyrrolidinium chloride (Pyr), and then ethylene polymerizations were performed. The Zr contents of $SiO_2/1NS/IL/(n-BuCp)_2ZrCl_2$ and $SiO_2/2NS/IL/(n-BuCp)_2ZrCl_2$ were lower than those of only aminosilane-treated silicas. However, the polymerization activity of $SiO_2/1NS/IL/(n-BuCp)_2ZrCl_2$ was higher than that of $SiO_2/1NS/(n-BuCp)_2ZrCl_2$. The polymerization activity of $SiO_2/2NS/IL/(n-BuCp)_2ZrCl_2$ was lower than that of $SiO_2/2NS/(n-BuCp)_2ZrCl_2$ due to much lower Zr content.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
• /
• v.10 no.4
• /
• pp.229-236
• /
• 2012

A molten salt technology using $Li_2O$-LiCl has been extensively investigated to recover uranium metal from spent fuels in the field of nuclear energy. In the reduction process, it is an important point to maintain the concentration of $Li_2O$. $ZrO_2$ is inevitably contained in the spent fuels because Zr is one of the main components of fuel rod hulls. Therefore, the fate of $ZrO_2$ in $Li_2O$-LiCl molten salt has been investigated. It was found that $Li_2ZrO_3$ and $Li_4ZrO_4$ were formed chemically and electrochemically and they were not reduced to Zr. The recycling of $Li_2O$ is the key mechanism ruling the total reaction in the electrolytic reduction process. However, $ZrO_2$ will have a role as a $Li_2O$ sink.

• Polymer(Korea)
• /
• v.36 no.1
• /
• pp.111-116
• /
• 2012

A functionalization of mesoporous materials with organosilane was carried out via a post-synthesis grafting method and $(n-BuCp)_2ZrCl_2$/methylaluminoxane (MAO) as subsequently immobilized on the functionalized mesoporous materials for ethylene polymerization. Organosilanes having amine, cyano or imidazoline group such as $N$-[(3-trimethoxysilyl)propyl]ethylenediamine (2NS), 4-(triethoxysilyl)butyronitrile (1NCy), 1-(3-triethoxysilylpropyl)-2-imidazoline (2NIm) were used for the surface functionalization of mesoporous materials. In the SBA-15/2NS/$(n-BuCp)_2ZrCl_2$ catalyst preparation, the amount of MAO in feed increased with an decrease in the Zr content of the supported catalyst, and Al content in the supported catalyst increased. The ethylene homopolymerization activity of SBA-15/2NS/$(n-BuCp)_2ZrCl_2$ dramatically increased as the amount of MAO in feed increased. Furthermore, when the immobilization time was 6 hrs, SBA-15/2NS/$(n-BuCp)_2ZrCl_2$ showed the highest activity. The activities of supported 2NS-, 1NCy-, 2NIm-functionalized catalysts decreased in the following order, SBA-15/2NS/ > SBA-15/2NIm/ > SBA-15/1NCy/$(n-BuCp)_2ZrCl_2$. 2NS and 2NIm which have two amine groups per silane molecule were shown to interact with $(n-BuCp)_2ZrCl_2$ strongly compared to 1NCy which has one amine group. Thus, the activities increased with an increase in the nitrogen and the Zr content of the supported catalysts.

• Journal of Powder Materials
• /
• v.18 no.4
• /
• pp.359-364
• /
• 2011

Zr-Ti alloy powders were successfully synthesized by magnesium thermal reduction of metal chlorides. The evaporated and mixed gasses of $ZrCl_4+TiCl_4$ were injected to liquid magnesium and the chloride components were reduced by magnesium leading to the formation of $MgCl_2$. The released Zr and Ti atoms were then condensed to particle forms inside the mixture of liquid magnesium and magnesium chloride, which could be dissolved fully in post process by 1~5% HCl solution at room temperature. By the fraction-control of individually injected $ZrCl_4$ and $TiCl_4$ gasses, the final compositions of produced alloy powders were changed in the ranges of Zr-0 wt.%~20 wt.%Ti and their purity and particle size were about 99.4% and the level of several micrometers, respectively.

• Journal of the Korean Ceramic Society
• /
• v.50 no.6
• /
• pp.446-450
• /
• 2013

TRISO coated particles with a ZrC barrier layer were fabricated by a fluidized-bed chemical vapor deposition (FBCVD) method for a use in a very high temperature gas-cooled reactor (VHTR). The ZrC layer was deposited by the reaction between $ZrCl_4$ and $CH_4$ gases at $1500^{\circ}C$ in an $Ar+H_2$ mixture gas. The amount of free carbon codeposited with in ZrC was changed by controlling the dilution gas ratio. Near-stoichiometric ZrC phase was also deposited when an impeller was employed to a $ZrCl_4$ vaporizer which effectively inhibited the agglomeration of $ZrCl_4$ powders during the deposition process. A near-stoichiometric ZrC coating layer had smooth surface while ZrC containing the free carbon had rough surface with tumulose structure. Surface roughness of ZrC increased further as the amount of free carbon increased.

• Journal of the Korean Ceramic Society
• /
• v.24 no.4
• /
• pp.397-403
• /
• 1987

Pb(Zr0.52Ti0.48)O3 powders were prepared by hydrothermal synthesis. Using soluble salts such as Pb(NO3)2, TiCl4 and ZrOCl2$.$8H2O and oxide such as PbO and TiO2 as starting materials, PZT powder was hydrothermally synthesized at the temperature range between 150$^{\circ}C$ and 200$^{\circ}C$. The result showed that reactivity by alkali was decreased in the sequence of Pb(NO3)2, TiCl4, ZrOCl2, PbO, TiO2 and ZrO2. Using the first three soluble salts, PZT powder was synthesiged at 150$^{\circ}C$ for 1hr. In PbO-TiCl4-ZrOCl2 system, PZT powder was synthesized at 150$^{\circ}C$ for 8rs. In Pb(NO3)2-TiO2-ZrOCl2 system, PZT powder was synthesized at 150$^{\circ}C$ for 16hrs, in PbO-TiO2-ZrOCl2 system, the powder was synthesized at 200$^{\circ}C$ for 8hrs.

• Journal of Integrative Natural Science
• /
• v.4 no.3
• /
• pp.177-181
• /
• 2011

The catalytic dehydrocoupling of bis(1-sila-3-butyl)benzene 1 and 2-phenyl-1,3-disilapropane 2 by $Cp_2ZrCl_2$/Red-Al and $Cp_2ZrCl_2$/n-BuLi was reported to compare their catalytic efficiency. The dehydrocoupling of monomeric silanes 1 with the $Cp_2ZrCl_2$/Red-Al and $Cp_2ZrCl_2$/n-BuLi combination catalysts produced two phases of polymers: one is a highly cross-linked insoluble solid, and the other is noncross-linked or slightly cross-linked soluble oil and could be a precursor for the solid polymer. The dehydrocoupling of 2 with the $Cp_2ZrCl_2$/n-BuLi combination catalyst similarly produced two phases of polymers. By contrast, the catalytic reaction of 2 with the $Cp_2ZrCl_2$/Red-Al combination catalyst produced a soluble polymer via redistribution/dehydrocoupling process.

• The Korean Journal of Ceramics
• /
• v.5 no.2
• /
• pp.131-136
• /
• 1999

Yttria stabilized zirconia(YSZ) films were deposited on porous NiO substrates and quartz plates by the thermal CVD using $ZrCl_4, YCl_3$ as precursors, and $O_2$ as a reactive gas at atmospheric pressure. The evaporation temperature of $ZrCl_4$ was varied from $250^{\circ}C$ to $550^{\circ}C$ while the temperatures of $YCl_3$ and the substrate were varied from $1000^{\circ}C$ to $1030^{\circ}C$. As the evaporation temperature of $ZrCl_4$ increased, the deposition rate of $ZrO_2$ decreased, contrary to our expectation. As a result of the decreased deposition rate of $ZrO_2$, the yttria content increase. The high evaporation temperature of $ZrCl_4$ makes the well-faceted crystal while the low evaporation temperature leads to the cauliflower-shaped structure. The dependence of the evaporation temperature on the growth rate and the morphological evolution was interpreted by the charged cluster model.