• Title/Summary/Keyword: SiC size

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Shape-Selective Catalysis over Zeolite. An Attempt in the Alkylation of Biphenyl

  • Sugi, Yoshihiro;Komura, Kenichi;Kim, Jong Ho
    • Applied Chemistry for Engineering
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    • v.17 no.3
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    • pp.235-242
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    • 2006
  • Liquid phase alkylation of biphenyl (BP) was studied over large pore zeolites. Selective formation of the least bulky products, 4,4'-diisopropylbiphenyl (4,4'-DIPB) occurred only in the isopropylation of BP over some large pore molecular sieves. H-mordenites (MOR) gave the highest selectivity among them. The dealumination of MOR enhanced catalytic activity and the selectivity of 4,4'-DIPB because of the decrease of coke-deposition. Non-selective catalysis occurs on external acid sites over MOR with the low $SiO_2/Al_2O_3$ ratio because severe coke-deposition deactivates the acid sites inside the pores by blocking pore openings. The selectivity of DIPB isomers was changed with reaction temperature. Selective formation of 4,4'-DIPB was observed at moderate temperatures such as $250^{\circ}C$, whereas the decrease of the selectivity of 4,4'-DIPB occurred at higher temperatures as $300^{\circ}C$. However, 4,4'-DIPB was almost exclusive isomer in the encapsulated DIPB isomers inside the pores even at high temperatures. These decreases of the selectivity of 4,4'-DIPB are due to the isomerization of 4,4'-DIPB on the external acid sites. Some 12-membered molecular sieves, such as SSZ-24, MAPO-5 (M:Mg, Zn, Si), SSZ-31, and ZSM-12, which have straight channels, gave 4,4'-DIPB with moderate to high selectivity; however; SSZ-55, SSZ-42, and MAPO-36 (M: Mg, Zn) gave lower selectivity because of cages in 12-membered one dimensional channels. Three dimensional H-Y and Beta zeolites also yield 4,4'-DIPB in low yield because of their wide circumstances for the isopropylation of BP. The increasing the size of alkylating agent enhanced the shape-selective alkylaiton even for the zeolites, such as UTD-1. The ethylation of BP to ethylbiphenyls (EBPs) and diethylbiphenyls (DEBPs) over MOR was non-selective. The ethylation of BP to EBPs was controlled kinetically. However, there was difference in reactivity of EBPs and DEBPs for their further ethylation. 4-EBP was ethylated preferentially among the isomers, although the formation of 4,4'-DEBP was less selective. The least bulky 4-EBP and 4,4'-DEBP have the highest reactivity among EBPs and DEBPs for the ethylation to polyethylbiphenyls (PEBPs). These results show that the environments of MOR pores are too loose for shape selective formation of the least bulky isomers, 4-EBP and 4,4'-DEBP in the ethylation of BP, and that MOR pores have enough space for the further ethylation of 4,4'-DEBP.

A study on the synthesis and crystal growth of the MFI type zeolite, silicalite under highgravity (고중력에서 MFI 형 Zeolite 인 Silicalite 결정의 합성 및 성장에 관한 연구)

  • Kim, Wha-Jung;Lee, Joon
    • Applied Chemistry for Engineering
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    • v.2 no.2
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    • pp.97-107
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    • 1991
  • Highly-siliceous dealuminated zeolite, silicalite(end member of ZSM-5) was synthesized from a batch composition of 2.55 $Na_2O-5.0$ TPABr-$100SiO_2-2800H_2O $ at $180^{\circ}C$ and at times ranging from one to seven days of reaction time. Autoclaves containing the synthesis mixture were centrifuged within the specially-equipped convection oven to provide an elevated gravitational force field like 30 and 50 G. Tests were also conducted at normal gravity. For synthesis performed under elevated gravities, average and maximum crystal sizes were substantially greater than those synthesized under normal gravity and product yields were also found to be affected by elevated gravity ; that is, product yields were substantially enhanced under elevated gravity from 4 % to 55 % with respect to normal gravity. The average crystal sizes of silicalite synthesized at normal gravity were 50 to $70{\mu}m$ over an entire range of reaction time, one to seven days while the average crystal sizes synthsized under elevated gravities, 30 and 50 G, were 160 to $190{\mu}m$ respectively. For the elevated gravity, in particular, two separate nucleations and growths were observed. For examples, at 50G, large crystals of $200{\mu}m$ were produced through the second growing stage after 5 days of reaction following the rapid first growing stage where fairly large crystals of $135{\mu}m$ were produced only in 2 days of reaction. The maximum crystal sizes obtained through the above two growing stages were 190 and $300{\mu}m$, respectively. A discussion of how elevated gravity affects nucleation, growth, yield and crystal size of silicalite is presented.

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Interconnection Process and Electrical Properties of the Interconnection Joints for 3D Stack Package with $75{\mu}m$ Cu Via ($75{\mu}m$ Cu via가 형성된 3D 스택 패키지용 interconnection 공정 및 접합부의 전기적 특성)

  • Lee Kwang-Yong;Oh Teck-Su;Won Hye-Jin;Lee Jae-Ho;Oh Tae-Sung
    • Journal of the Microelectronics and Packaging Society
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    • v.12 no.2 s.35
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    • pp.111-119
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    • 2005
  • Stack specimen with three dimensional interconnection structure through Cu via of $75{\mu}m$ diameter, $90{\mu}m$ height and $150{\mu}m$ pitch was successfully fabricated using subsequent processes of via hole formation with Deep RIE (reactive ion etching), Cu via filling with pulse-reverse electroplating, Si thinning with CMP, photolithography, metal film sputtering, Cu/Sn bump formation, and flip chip bonding. Contact resistance of Cu/Sn bump and Cu via resistance could be determined ken the slope of the daisy chain resistance vs the number of bump joints of the flip chip specimen containing Cu via. When flip- chip bonded at $270^{\circ}C$ for 2 minutes, the contact resistance of the Cu/Sn bump joints of $100{\times}100{\mu}m$ size was 6.7m$\Omega$ and the Cu via resistance of $75{\mu}m$ diameter, $90{\mu}m$ height was 2.3m$\Omega$.

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Utilizability of Waste Concrete Powder as a Material for Soil Pavement (흙도로포장용 재료로서 폐콘크리트 미분말의 활용성 연구)

  • Kim, Yong-Jic;Choi, Yun-Wang;Kim, Young-Jin
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.3 no.3
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    • pp.277-282
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    • 2015
  • This study is conducted to utilize waste concrete powder (WCP) made as a by-product manufacturing high quality recycled aggregate. The blaine fineness of the used waste concrete powder was $928cm^2/g$. As the main characteristic of waste concrete powder, it showed an angular type similar to cement, but hydrated products were attached on the surface of particles. In addition, the size of the particles of waste concrete powder was larger than OPC and in terms of chemical components it had higher $SiO_2$ contents. For using WCP in soil cement-based pavement, the qualities, physical and chemical properties, of WCP should be researched. In the first step, the specified compressive strength of mortar for two types of clay sand soil and clay soil respectively was experimented to be 15 MPa and then optimum mixing ratio of chemical solidification agent were decided in the range of 1.5 - 3.0% in the replacement with cement weight content. In the second step, based on the prior experimental results, recycling possibility of WCP in soil cement-based pavement was studied. In the result of experiment the mixing ratio of WCP were 5, 10, 15 and 20% in the replacement with soil weight and the compressive strength of mortar was somewhat decreased according to the increase of the mixing ratio of WCP.

Effects of the Precipitation of Carbides and Nitrides on the Texture Structures in Extra Low Carbon Steel Sheets containing B, Nb and Ti(ll) (B, Nb및 Ti를 함유한 극저탄소강에서 탄화물 및 질화물의 석출이 집합조직에 미치는 영향(ll))

  • Lee, Jong-Mu;Yun, Guk-Han;Lee, Do-Hyeong
    • Korean Journal of Materials Research
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    • v.3 no.2
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    • pp.131-139
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    • 1993
  • Abstract Alloying elements such as AI, Ti, Nb and B in the extra low carbon AI-killed steel precipitate as nitrides or carbides and change the recrystallization texture structure of the steel during heattreatment with the result of strong effects on the deep drawability of the steel sheet. In this study the effects of fine precipitates such as nitrides and carbides on the texture of extra low carbon steels into which Ti, Nb, B, P, Si and Mn were added as alloying elements were investigated by means of TEM, SEM and optical microscopic analyses. Fine N$b_2$C and T$i_2$AIN precipitates are mainly observed in the steel containing both Nb and Ti, while fine AIN and coarse BN precipitates are observed in the Nb~containing steel and coarse T${i_4}{N_3}$ and ${N_10}{N_22}$/T$i_68$ precipitates are observed in the Ti-containing steel. The grain size of the Ti containing steel is larger than that of the Nb containing steel and that of the one containing both Nb and Ti.

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Microstructure and Microdefects of Diamond Thin Films Deposited by MPECVD (마이크로웨이브 화학증착법에 의한 다이아몬드 박막의 미세구조오 미세결함)

  • Lee, Se-Hyeon;Lee, Yu-Gi;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.6 no.8
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    • pp.833-840
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    • 1996
  • Diamond thin films were deposited on p-type (100) Si wafers using MPECVD. Prior to deposition, ultrasonic striking was done to improve density of nucleation sites with dimond powder of 40~$60\mu$m size. Then diamond thin films were deposited at $^900{\circ}C$, 40Torr and 1000W microwave power using ${CH}_{4}$ and ${H}_{2}$ gases. The purity, the morphology and the microstructur'e and microdefects of diamond thin films were characterized by Raman spectroscopy, SEM and TEM, repectively. In Raman spectroscopy the peaks of non-diamond phase increased as ${CH}_{4}$, concentration increased. In SEM, the morphology of diamond thin films varied from crystalline to cauliflower as ${CH}_{4}$, concentration increased. As ${CH}_{4}$ con centration increased, the density of defects increased, with most defects being {III} twin. ${MTP}_{5}$, were formed with five (II]) planes. As these (Ill) Planes were twinned, ${MTP}_{5}$, represented five-fold symmetry. ]n the interfaces, defects in diamond thin films fanned out from small regions implying nucleation sites.

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Fundamental Research on Reactivity of Silica Source in the Rapidly Cured Inorganic Micro-Defect-Free(MiDF) Concrete (촉진 양생한 무기계 MiDF 콘크리트에서 실리카질 원료의 반응성에 관한 기초 연구)

  • Choi, Hong-Beom;Kim, Jin-Man
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.7 no.2
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    • pp.166-173
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    • 2019
  • In this paper, the reaction properties of silica source in the accelerated curing conditions using autoclave and the fundamental properties of inorganic Micro Defect Free(MiDF) concrete using silica source are studied. Studies show that Si ions elution rate from silica source in autoclave curing is higher in amorphous source. In tap water conditions, solids which is source after autoclaved curing show a higher mass reduction in amorphous materials, which is attributed to the higher elution rate of ion. In $Ca(OH)_2$ solution conditions, amorphous materials show higher mass increase, due to increase in C-S-H minerals. From experiment for influence on the properties of MiDF concrete by using nano silica materials, the specimen with silica fume shows an increase in compressive strength and a decrease in absorption depending on replacement rate up to 5.5%, while nano silica with amorphous phase and high-fineness shows a decrease in compressive strength and decrease in the water absorption. The specimen with nano silica increases the pore below 10,000nm, but reduces pore between 10,000 and 100,000nm. The above results show that the porosity and absorption rate of MiDF concrete can be reduced by using amorphous nano-size silica. However, to reduce the pore of 50 to 10,000nm, better dispersion of nano material in the cement matrix will be necessary. We will focus on the this item in the next research.

Ni/Au Electroless Plating for Solder Bump Formation in Flip Chip (Flip Chip의 Solder Bump 형성을 위한 Ni/Au 무전해 도금 공정 연구)

  • Jo, Min-Gyo;O, Mu-Hyeong;Lee, Won-Hae;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.6 no.7
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    • pp.700-708
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    • 1996
  • Electroless plating technique was utilized to flip chip bonding to improve surface mount characteristics. Each step of plating procedure was studied in terms pf pH, plating temperature and plating time. Al patterned 4 inch Si wafers were used as substrstes and zincate was used as an activation solution. Heat treatment was carried out for all the specimens in the temperature range from room temperature to $400^{\circ}C$ for $30^{\circ}C$ minutes in a vacuum furnace. Homogeneous distribution of Zn particles of size was obtained by the zincate treatment with pH 13 ~ 13.5, solution concentration of 15 ~ 25% at room temperature. The plating rates for both Ni-P and Au electroless plating steps increased with increasing the plating temperature and pH. The main crystallization planes of the plated Au were found to be (111) a pH 7 and (200) and (111) at pH 9 independent of the annealing temperature.

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Manufacture of the Hydrophobic HY-type Zeolite-honeycomb and Its Adsorption/Desorption Characteristics for the Benzene, o-xylene, and MEK (소수성 HY-형 제올라이트제 하니컴의 제조 및 그 하니컴의 벤젠, o-xylene, MEK에 대한 흡.탈착특성)

  • Mo, Se-Young;Jeon, Dong-Hwan;Kwon, Ki-Seung;Sohn, Jong-Ryeul
    • Journal of Korean Society for Atmospheric Environment
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    • v.23 no.1
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    • pp.84-96
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    • 2007
  • We performed the experiments to manufacture the hydrophobic $200cells/in^2$-zeolite honeycomb using HY-type zeolite of Si/Al ratio of 80 for separating and removing the VOCs emitted from small and medium size-plants by adsorption and to determine the drying method for the honeycomb at $105^{\circ}C$ without cracking, then measured performances of the honeycomb to adsorb the benzene, o-xylene, and MEK and to desorb the benzene and MEK saturated on the honeycomb by the nitrogen gas as the desorption gas. As a results, the good honeycomb was formed and the honeycomb was not cracked when the mixing ratio of the zeolite to bentonite to methyl cellulose to polyvinyl alcohol to glycerine to water is 100 : 8.73 : 2.18 : 4.19 : 1.38 : 126 and dried the honeycomb at $105^{\circ}C$ for 24 hours in the drying oven. The shape of the dried honeycomb was not changed after calcination, and the compressive strengths of the honeycomb after drying and calcination were 6.7 and $0.69kg/cm^2$, respectively. The adsorption efficiencies of the honeycomb for benzene, o-xylene, and MEK were $92{\sim}96%$ at the room temperature. The desorption efficiency at $180^{\circ}C$ was higher than that at $150^{\circ}C\;by\;1.5{\sim}13.8%$ depending on the flow rate of the nitrogen gas, and it was found that desorption efficiency is higher than 85% at $180^{\circ}C$ and 1.0L/min of the nitrogen gas. At $180^{\circ}C$ and 0.2 L/min, the concentration of the benzene and MEK in the used desorption gas are higher than 40,000 and 50,000ppm, respectively, so it be used as the fuel for preheating the desorption gas fed into the column in desorption cycle.

Microstructural Analysis on $UO_2$ and $UO_2$-4wt% $CeO_2$ by Using Additives in Reducing and Oxidizing Atmospheres

  • Kim, Han-Soo;Kim, Si-Hyung;Lee, Young-Woo;Na, Sang-Ho
    • Nuclear Engineering and Technology
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    • v.28 no.5
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    • pp.458-466
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    • 1996
  • The effects of dopants on the modification of microstructure of UO$_2$ and UO$_2$-4wt%CeO$_2$ sintered pellets have been studied in hydrogen and $CO_2$/CO mixture atmospheres by using $Ta_2O_5$, TiO$_2$ and $Nb_2O_5$ as sintering additives. The dopant were added as oxide powders and homogenized by attrition milling. The mixed powders were pressed, and then sintered in hydrogen at 1$700^{\circ}C$ , or in oxidizing atmosphere using Controlled $CO_2$/CO mixtures at 125$0^{\circ}C$. Both density and microstructure of UO$_2$ are modified by the addition of dopants in reducing atmosphere. The sintered density is increased with $Ta_2O_5$ addition up to 0.33wt% and subsequently decreased with higher content of the additive. The effect on the densification and the gain growth are apparent with the addition of 0.24wt% $Nb_2O_5$. With 0.lwt% titania and 0.6wt% $Ta_2O_5$, the sintered density is decreased, but the grain size is increased. In oxidizing atmosphere, the grain sizes for UO$_2$ doped with the above additives are smaller than that for pure UO$_2$. The grain size of Ta or Nb-doped UO$_2$ is decreased with increasing $CO_2$/CO ratio, but that of pure UO$_2$or T-doped UO$_2$ is increased. A large portion of second phases is observed in UO$_2$ doped with 0.lwt% TiO$_2$ sintered in hydrogen atmosphere, while, in $CO_2$/CO atmospheres, the second phases or dopant agglomerates are not observed. For UO$_2$-4wt%CeO$_2$ mixed oxide, the effect of additives on the gain growth is not so much as that for the pure UO$_2$. This is attributed to the formation of clusters by dopant cations and Ce ions, so that the additives contribute to a lesser exent to the grain growth for the mixed oxide.

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