• Title/Summary/Keyword: crystallization reaction

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Synthesis and Characterization of Particle-filled Glass/G lass-Ceramic Composites for Microelectronic Packaging (I)

  • Hong, Chang-Bae;Lee, Kyoung-Ho
    • Journal of the Microelectronics and Packaging Society
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    • v.6 no.1
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    • pp.11-21
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    • 1999
  • For microelectronic packaging application, the crystallizable glass powder in CaO-$A1_2O_3-SiO_2-B_2O_3$system was mixed with various amounts of alumina inclusions (\approx 4 $\mu \textrm{m}$), and its sintering behavior, crystallization behavior, and dielectric constant were examined in terms of vol% of alumina and the reaction between the alumina and the glass. Sintering of the CASB glass powder alone at $900^{\circ}C$ resulted in full densification (99.5%). Sintering of alumina-filled composite at $900^{\circ}C$ also resulted in a substantial denslfication higher than 97% of theoretical density, In this case, the maximum volume percent of alumina should be less than 40%. XRD analysis revealed that there was a partial dissolution of alumina into the glass. This alumina dissolution, however, did not show the particle growth and shape accommodation. Therefore, the sintering of both the pure glans and the alumina-filled composite was mainly achieved by the viscous flow and the redistribution of the glass. Alumina dissolution accelerated the crystallization initiation time at $1000^{\circ}C$ and hindered the densification of the glass. Dielectric constants of both the alumina-filled glass and the glass-ceramic composites were increased with increasing alumina content and followed rule of mixture. In case of the glass-ceramic matrix composites showed relatively lower dielectric constant than the glass matrix composite. Furthermore, as alumina content increased, crystallization behavior of the glass was changed due to the reaction between the glass and the alumina. As alumina reacted with the glass matrix, the major crystallized phase was shifted from wollastonite to gehlenite. In this system, alumina dissolution strongly depended on the particle size: When the particle size of alumina was increased to 15 $\mu\textrm{m}$, no sign of dissolution was observed and the major crystallized phase was wollastonite.

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Synthetic Characteristics of AlPO$_4$-5 Molecular Sieve (AlPO$_4$-5 분자체의 합성 특성)

  • Sung Hwa Jhung;Suk Bong Hong;Young Sun Uh;Hakze Chon
    • Journal of the Korean Chemical Society
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    • v.37 no.10
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    • pp.867-873
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    • 1993
  • Influences of crystallization time and $H_2O/Al_2O_3$ ratio of the reaction mixtures on the synthesis of AlPO$_4$-5 molecular sieve have been studied by X-ray powder diffraction, nitrogen adsorption, scanning electron microscope (SEM), and solid state $^{27}$Al magic angle spinning nuclear magnetic resonance (MAS NMR) techniques. The degree of crystallinity of AlPO$_4$-5 follows a sigmoid pattem as crystallization time increases. The induction period is shorter than 1 h when the crystallization process is carried out at 150$^{\circ}$C. The conversion of reactants to product, AlPO$_4$-5, can be clearly observed, and all of the determined physical properties change abruptly after about 2 h. It is found that increase in $H_2O/Al_2O_3$ ratio of the reaction mixtures not only changes the crystal morphology from aggregates to hexagonal single crystals, but also results in the formation of longer AlPO$_4$-5 crystals.

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Production of Structured Lipid Containing Capric and Conjugated Linoleic Acids and Studies of Physicochemical Characteristics (Capric acid와 conjugated linoleic acid를 함유한 재구성 지질의 합성 및 특성연구)

  • Shin, Jung-Ah;Lee, Ki-Teak
    • Korean Journal of Food Science and Technology
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    • v.36 no.4
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    • pp.537-541
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    • 2004
  • Based on reaction time and substrate molar ratio, structured lipid (SL-corn) was produced at 1:2:2(corn oil/capric acid/CLA) and 4% immobilized lipase from Rhizomucor miehei (RM IM). Reaction was carried out for 24 hr at $55^{\circ}C$ in 1-L stirred-batch reactor. After reaction, 13.3 mol% capric acid and 8.9%, CLA were incorporated into corn oil. Iodine and saponification values of SL-corn were 68 and 202, respectively. Tocopherol content decreased after reaction (about 39%). SL-corn showed more yellowish color than corn oil (p<0.05). Reversed-phase HPLC indicated triacylglycerol species containing capric acid in SL-corn resulted in faster crystallization than that of corn oil.

A Study on the Characteristics of Amorphous TiAl by P/M Processing

  • Han, Chang-Suk;Jeon, Seung-Jin
    • Journal of the Korean Society for Heat Treatment
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    • v.29 no.2
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    • pp.51-55
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    • 2016
  • The P/M processing of titanium aluminide using amorphous TiAl is developed by which it is possible to overcome inherent fabricability problems and to obtain a fine microstructure. A high quality amorphous TiAl powder produced by reaction ball milling shows clear glass transition far below a temperature at the onset of crystallization in differential scanning calorimetry above a heating rate of 0.05 K/s. We obtained a fully dense compact of amorphous TiAl powders, encapsulated in a vacuumed can, via viscous flow by hot isostatic pressing (HIP). Isothermally annealing of HIP'ed amorphous compact under a pressure of 196 MPa shows a progressive growth of ${\gamma}-TiAl$ phase with ${\alpha}2$ ($Ti_3Al$), which is characterized by increasing sharpness of X-ray peaks with temperature. Fully dense HIP'ed compact of titanium aluminide TiAl shows a high hardness of 505 Hv, suggesting strengthening mechanisms by sub-micron sized grain of ${\gamma}-TiAl$ and particle-dispersion by second phase constituent, ${\alpha}2$.

The Effects of Temperature and Pressure on Synthesis of Zeolite 4A from Coal Fly Ash by Hydrothermal Reaction (석탄 비산회로부터 수열법에 의한 제올라이트 4A의 합성시 온도와 압력의 영향)

  • Yoon, Cheol;Yeon, Ik-Jun;Kim, Kwang-Yul
    • Journal of the Korean Applied Science and Technology
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    • v.16 no.3
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    • pp.217-221
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    • 1999
  • This study was carried out to synthesis the zeolite using the bituminous coal fly ash emitted from power plant that occurs several environmental problems. In spite of fly ash has contained high content of $SiO_2$ and $Al_2O_3$, it disposed mainly landfill. If the effective methods to recover the $SiO_2$ and $Al_2O_3$ were developed, the fly ash could be utilized valuable raw materials. In this study, fly ash was used as raw material to synthesize the zeolite by pressurized hydrothermal reaction. Also, experimental parameters included temperature($70{\sim}110^{\circ}C$, and pressure($140{\sim}200$ psi) of crystallization were investigated. The more crystallization pressure was increased, the more Zeolite 4A was synthesized at 70 and $90^{\circ}C$. Zeolite 4A of metastable phase tend to be transformed into sodalite of stable phase at $110^{\circ}C$.

Polymorphism of Calcium Carbonate Crystal by Silk Digested Amino Acid (실크 분해 아미노산에 의한 탄산칼슘 결정의 polymorphism)

  • Kim, Jin-Ho;Kim, Jong Min;Kim, Woo Sik;Kim, In Ho
    • Korean Chemical Engineering Research
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    • v.46 no.6
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    • pp.1107-1112
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    • 2008
  • Crystallization of calcium carbonate was performed by using aqueous calcium chloride and sodium carbonate for operational simplicity. Reaction time, solute concentrations, pH, and organic additive were varied to get calcium carbonate crystals. Silk fibroin was used as the additive to understand the change of morphology of calcium carbonate crystal. The crystals were analyzed by FE-SEM, XRD, and FT-IR. Reaction time, and pH mainly affected the morphology of crystals. Besides, it was found that silk fibroin inhibited the formation of vaterite and promoted the calcite forms.

A Study on the Phosphorus Removal from Wastewater by Eggshell (난각을 이용한 폐수중의 인 제거에 관한 연구)

  • Kim, Min-Su;Kang, Seon-Hong
    • Journal of Korean Society of Water and Wastewater
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    • v.18 no.2
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    • pp.174-180
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    • 2004
  • This study is a fundamental research to test the applicability of abandoned eggshell as seed material for crystallization reaction. Eggshell was calcinated at $850^{\circ}C$ and ground to lesser than 0.42mm. The calcination characteristics of eggshell were examined by X-ray diffraction (XRD). The effect of initial calcium concentration, alkalinity, reaction temperature condition, seed dosage were studied by batch test. For the low concentration sample(P concentration is under 50mg/L), more than 90% of P can be removed. The effect of initial calcium concentration(0~120mg/L) was performed. At the result of the test, more than 50mg/L calcium concentration has high removal efficiency. Alkalinity effect was studied for synthetic solution(100mg/L initial P, 50mg/L calcium, 0.025% seed dosage) with 0~300mg/L bicarbonate alkalinities. For synthetic solution(100mg/L initial P, 50mg/L calcium, 100mg/L bicarbonate alkalinity, 0.025% seed dosage), the phosphorus concentration was examined with $10{\sim}35^{\circ}C$. In addition, calcinated eggshell was injected to swine wastewater to test the applicability to actual wastewater.

Treatment of N, P of Auto-Thermal Thermophilic Aerobic Digestion Filtrate with Struvite Crystallization (Struvite 결정화 반응을 이용한 고온 소화 여과액의 N, P 처리 특성)

  • Choo, Yeon-Duk;Kim, Keum-Yong;Ryu, Hong-Duck;Lee, Sang-Ill
    • Journal of Korean Society of Environmental Engineers
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    • v.33 no.11
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    • pp.783-789
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    • 2011
  • Recently, auto-thermal thermophilic aerobic digestion (ATAD) has a great attention for destruction of wasted sludge biomass in wastewater treatment plant. Reduction of sludge concentration has been successfully achieved with pilot scale ATAD and ceramic filtration process in field condition. However, high concentration of COD, total nitrogen (TN) and total phosphorus (TP) was observed in filtrate, which should be treated before recirculation of filtrate to biological wastewater treatment plant. This study was focused on removal of nitrogen and phosphorus contained in the filtrate of ATAD, using struvite crystallization method. The effect of operational and environmental parameters (such as, N, P and Mg ion concentration and molar ratio, pH, reaction time, agitation strength, seed dosage, and reaction temperature) on the treatment of TN and TP with struvite crystallization were evaluated. Magnesium (as $MgCl_26H_2O$) and phosphorus (as $K_2HPO_4$) ions were, if necessary, added to increase nitrogen removal efficiency by the crystal formation. Average concentration of $NH_4^+-N$ and $PO_4^{3-}-P$ of the filtrate were 1716.5 mg/L and 325.5 mg/L, respectively. Relationship between removal efficiencies of nitrogen and phosphorus and molar ratios of $Mg^{2+}$ and $PO_4^{3-}-P$ to $NH_4^+-N$ was examined. Crystal formation and nitrogen removal efficiencies were significantly increased as increasing molar ratios of magnesium and phosphorus to nitrogen. As molar ratio of $Mg^{2+}:PO_4^{3-}-P:NH_4^+-N$ were maintained to 2 : 1 : 1 and 2 : 2 : 1, removal efficiencies of nitrogen and phosphorus were 71.6% and 99.9%, and 93.8% and 98.6%, respectively. However, the effect of reaction time, mixing intensity, seed dose and temperature on the struvite crystallization reaction was not significant, comparing to those of molar ratios. Settled sludge volume after struvite crystallization was observed to be reduced with increase of seed dose and to be increased at high temperature.

Synthesis of $Cu_2ZnSnSe_4$ compound by solid state reaction using elemental powders

  • Wibowo, Rachmat Adhi;Alfaruqi, Muhammad H.;Jung, Woon-Hwa;Kim, Kyoo-Ho
    • 한국신재생에너지학회:학술대회논문집
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    • 2009.06a
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    • pp.134-137
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    • 2009
  • Commercially available elemental powders of Cu, Zn, Sn and Se were employed for crystallizing a stannite-type $Cu_2ZnSnSe_4$ compound by means of solid state reaction. $Cu_2ZnSnSe_4$ reaction chemistry was also modeled based on differential-thermal analysis and X-ray powder diffraction results. It was observed that Se tends to react preferably with Cu to form CuSe and $CuSe_2$ phases at low reaction temperature. The formation of $Cu_5Zn_8$ intermetallic phase was found to be the intermediate reaction path for the binary ZnSe formation. A solid state reaction at $320^{\circ}C$ reacted elemental powderst obinary selenides of CuSe, ZnSe and SnSe completely. The crystallization of $Cu_2ZnSnSe_4$ was was detected to begin at $300^{\circ}C$ and its weight fraction increased with an increase of reaction temperature, which most probably formed from the reaction between $Cu_2SnSe_3$ and ZnSe.

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Crystallization of srAl2O4 Synthesized by the Polymerized Complex Method (착체중합법으로 합성한 srAl2O4의 핵생성 관찰)

  • 김형준;박정현
    • Journal of the Korean Ceramic Society
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    • v.41 no.6
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    • pp.439-443
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    • 2004
  • SrAl$_2$O$_4$ powder was prepared by polymerized complex method and its nucleation was observed at different temperatures and times. Problems of inhomogeneity and high synthesis temperature induced by solid state reaction could be solved by using polymeric precursors. The process of decomposition by heat treatment above 40$0^{\circ}C$ was observed by Scanning Electron Microscopy (SEM) and elemental analyzer. Crystallization of SrAl$_2$O$_4$ occured at about 90$0^{\circ}C$ and its crystalline size. which was determined by using Transmission Electron Microscopy (TEM) and X-Ray Diffractometer (XRD). was about 30∼50 nm.