• 한국세라믹학회지
• /
• 제46권2호
• /
• pp.170-174
• /
• 2009

$BaTiO_3$ powder was synthesized by the solid-state reaction of fine $BaTiO_3$ and $TiO_2$ raw materials. Fine grinding media of 50 and 300 microns were used for obtaining fine particulate mixture of $BaTiO_3$ and $TiO_2$ with high homogeneity. Effect of the size of grinding media on the synthesis mechanism of $BaTiO_3$ was discussed on the basis of the particulate morphology and thermogravimetry data for the mixture powders. By using the finer grinding media, $BaTiO_3$ was formed at the lower temperature and the particle size with the relatively narrower distribution could be obtained. $BaTiO_3$ powder with the average size of 100 nm was synthesized by the solid reaction in vacuum atmosphere.

• Bulletin of the Korean Chemical Society
• /
• 제35권10호
• /
• pp.3035-3040
• /
• 2014

A new efficient catalytic method for aza/thia-Michael addition reactions of amines/thiols with higher product yields has been developed. Combining single-walled carbon nanotubes (SWCNT) with triethylammonium hydrogen phosphate (TEAP) ionic liquid (IL) can work as a catalyst. We utilized Raman spectroscopy to gain insight into the interactions between IL and SWCNT. The interactions between SWCNT with TEAP were confirmed by the increasing intensity ratios and spectral shift in wavelength of the Raman D and G bands of SWCNT. Further, the morphology of the resulting composite materials of TEAP and SWCNT was determined by using scanning electron microscopy (SEM). Higher product yield in reduced reaction time is the key advantage of using bucky gel as a catalyst for Michael reaction.

• 한국분말재료학회지
• /
• 제20권3호
• /
• pp.221-227
• /
• 2013

$TiB_2$-reinforced iron matrix composite (Fe-$TiB_2$) powder was in-situ fabricated from titanium hydride ($TiH_2$) and iron boride (FeB) powders by the mechanical activation and a subsequent reaction. Phase formation of the composite powder was identified by X-ray diffraction (XRD). The morphology and phase composition were observed and measured by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively. The results showed that $TiB_2$ particles formed in nanoscale were uniformly distributed in Fe matrix. $Fe_2B$ phase existed due to an incomplete reaction of Ti and FeB. Effect of milling process and synthesis temperature on the formation of composite were discussed.

• 한국분말재료학회지
• /
• 제23권6호
• /
• pp.442-446
• /
• 2016

The sol-gel method is the simplest method for synthesizing monodispersed silica particles. The purpose of this study is to synthesize uniform, monodisperse spherical silica nanoparticles using tetraethylorthosilicate (TEOS) as the silica precursor, ethanol, and deionized water in the presence of ammonia as a catalyst. The reaction time and temperature and the concentration of the reactants are controlled to investigate the effect of the reaction parameters on the size of the synthesized particles. The size and morphology of the obtained silica particles are investigated using transmission electron microscopy and particle size analysis. The results show that monodispersed silica particles over a size range of 54-504 nm are successfully synthesized by the sol-gel method without using any additional process. The nanosized silica particles can be synthesized at higher TEOS/$H_2O$ ratios, lower ammonia concentrations, and especially, higher reaction temperatures.

• 한국산학기술학회:학술대회논문집
• /
• 한국산학기술학회 2000년도 추계학술대회
• /
• pp.39-41
• /
• 2000

Newly modified spray Pyrolysis system was developed to Produce ultra Pure and fine Powder by spray Pyrolysis Process. In this system, raw material solution was effectively atomized and sprayed into the reaction furnace. Also, thermal decomposition process fully completed in the three zone reaction furnace, and produced powder was effectively collected. A technology to reduce impurities in complex acid solution below 20ppm was also developed. The characteristics of produced powder were studied by changing the reaction conditions such as reaction temperature, the injection velocity of the solution and air, nozzle tip size and concentration of solution. The morphology of powder had spherical shape under the most experimental conditions, and the composition and the particle size distribution were almost uniform. Under the most experimental conditions average particle size of most produced powder was below 100nm.

• 연구논문집
• /
• 통권24호
• /
• pp.63-79
• /
• 1994

This article reports a experimental study of the method to achieve a bond joint at lower temperature in a short time. DC magnetron sputtering of Sn, Sn/Pb, Sn/In and Sn/Cu on copper substrate was provided as an interlayer for Cu to Cu bonding under the air environment. Various examination was conducted and investigated on the effect of experimental parameters such as coating materials, coating time(or coating thickness), bonding temperature and bonding time etc. Bonding was performed at the temperature of $210^\circC-320^\circC$ for 0sec and interfacial reaction between the coated layer and copper substrate was examined using optical, scanning electron microscope and x-ray diffractometer. From the obtained results, it was found that intermetallic compounds layer consisted of $\eta-phase(Cu_6Sn_5)$ and $\beta-phase(Cu_3Sn)$ was formed at the joint interface for almost all coating materials. But the dominant phase formed in the preetched Cu substrate coated with Sn was $\beta-phase$. A characteristic morphology looks like a reaction ring, which was believed as the strong interconnecting regions between two substrates, was found to be formed on the reaction surface of copper substrates. The morphologies and compositions of the intermetallics, which depends on the regions of the reaction surface, was appeared as greatly different. Based on above results, the new bonding process to make the joint at lower temperature for short time can be admitted as a feasible process.

• 한국재료학회지
• /
• 제33권10호
• /
• pp.385-392
• /
• 2023

A solution combustion process for the synthesis of hollandite (BaAl₂Ti₆O₁₆) powders is described. SYNROC (synthetic rock) consists of four main titanate phases: perovskite, zirconolite, hollandite and rutile. Hollandite is one of the crystalline host matrices used for the disposal of high-level radioactive wastes because it immobilizes Sr and Lns elements by forming solid solutions. The solution combustion synthesis, which is a self-sustaining oxi-reduction reaction between a nitrate and organic fuel, generates an exothermic reaction and that heat converts the precursors into their corresponding oxide products in air. The process has high energy efficiency, fast heating rates, short reaction times, and high compositional homogeneity. To confirm the combustion synthesis reaction, FT-IR analysis was conducted using glycine with a carboxyl group and an amine as fuel to observe its bonding with metal element in the nitrate. TG-DTA, X-ray diffraction analysis, SEM and EDS were performed to confirm the formed phases and morphology. Powders with an uncontrolled shape were obtained through a general oxide-route process, confirming hollandite powders with micro-sized soft agglomerates consisting of nano-sized primary particles can be prepared using these methods.

• 공업화학
• /
• 제9권7호
• /
• pp.1004-1010
• /
• 1998

Single-jet 반회분식 결정화 반응기에서 동력투입량, 반응물의 주입시간 및 주입방법등 반응조건의 변화가 란타늄 옥살레이트 결정입자의 반응성 결정화에 미치는 영향에 대해 실험적으로 조사하였다. 란타늄 옥살레이트 결정입자의 크기분포는 반응조건에 관계없이 monomodal 형태의 크기분포를 나타내었으나 평균결정크기는 반응조건에 크게 영향을 받았다. 동력투입량이 증가할수록, 반응물의 주입속도가 빠를수록, 란타늄 옥살레이트의 결정입자크기는 감소하였으나 상대적 유도시간은 증가하였다. 반응물의 주입방법에 있어서 옥살산 용액이 주입되는 경우보다 염화란타늄 용액이 주입되는 경우에 결정입자는 크게 나타났으며 상대적 유도시간은 감소하였다. 그리고 결정입자의 형태는 모두 침상형으로 반응조건의 변화에 크게 영향을 받지 않았다.

• Bulletin of the Korean Chemical Society
• /
• 제18권8호
• /
• pp.831-840
• /
• 1997

Core/shell structured composite metal oxides of Fe2O3/MgO were prepared by thermal decomposition of Fe(acac)3 adsorbed on the surface of MgO cores. The morphology of the composites conformed to that of the MgO used as the cores. Broad powder X-ray diffraction peaks shifted toward larger d, large BET surface area (∼350 m2/g), and the size of crystalline domains in nano range (4 nm), all corroborate to the nanocrystallinity of the Fe2O3/MgO composite which was prepared by using nanocrystalline MgO as the core. By use of microcrystalline MgO as the core, microcrystalline Fe2O3/MgO composite was prepared, and it had small BET surface area of less than 35 m2/g. AFM measurements on nanocrystalline Fe2O3/MgO showed a collection of spherical aggregates (∼80 nm dia) with a very rough surface. On the contrary, microcrystalline Fe2O3/MgO was a collection of plate-like flat crystallites with a smooth surface. The nitrogen adsorption-desorption behavior indicated that microcrystalline Fe2O3/MgO was nonporous, whereas nanocrystalline Fe2O3/MgO was mesoporous. Bimodal distribution of the pore size became unimodal as the layer of Fe2O3 was applied to nanocrystalline MgO. The macropores in a wide distribution which the nanocrystalline MgO had were absent in the nanocrystalline Fe2O3/MgO. The decomposition of CCl4 was largily enhanced by the overlayer of Fe2O3 on nanocrystalline MgO making the reaction between nanocrystalline Fe2O3/MgO and CCl4 be nearly stoichiometric. The reaction products were environmentally benign MgCl2 and CO2. Such an enhancement was not attainable with the microcrystalline samples. Even for the nanocrystalline MgO, the enhancement was not attained, if not with the Fe2O3 layer. Without the layer of Fe2O3, it was observed that the nanocrystalline domain of the MgO transformed into microcrystalline one as the decomposition of CCl4 proceeded on its surface. It appeared that the layer of Fe2O3 on the particles of nanocrystalline Fe2O3/MgO blocked the transformation of the nanocrystalline domain into microcrystalline one. Therefore, in order to attain stoichiometric reaction between CCl4 and Fe2O3/MgO core/shell structured composite metal oxide, the morphology of the core MgO has to be nanocrystalline, and also the nanocrystalline domains has to be sustained until the core was exhausted into MgCl2.

• 한국주조공학회지
• /
• 제33권1호
• /
• pp.13-21
• /
• 2013

The effects of rare earth element (R.E.) and cooling rate on the eutectic reaction of flake graphite cast irons were studied by combined analysis of macro/micro-structure and cooling curve data. The correlation between eutectic reaction parameter and macro/micro-structure was systematically investigated. Two sets of chemical compositions with the different addition of R.E. were designed to cast. Three types of molds for cylindrical specimens with the different diameters were prepared to analyze cooling rate effect. The difference between undercooling temperature and cementite eutectic temperature (${\Delta}T_1=T_{U}-T_{E,C}$), which is increased by adding R.E. and decreased by increasing cooling rate, is considered to be a suitable eutectic reaction parameter for predicting graphite morphology. According to the criterion, A-type graphite is mainly suggested to form for ${\Delta}T_1$ over $20^{\circ}C$. Eutectic reaction time (${\Delta}t$), which is decreased by adding R.E. or increasing cooling rate, is a suitable eutectic reaction parameter for predicting eutectic cell size. Eutectic cell size is found to decrease in a proportion to the decrease of ${\Delta}t$.