• Title/Summary/Keyword: high pressure synthesis

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Fabrication of the poly (methyl methacrylate)/clay (modified with fluorinated surfactant) nanocomposites using supercritical fluid process (초임계 공정을 이용한 poly(methyl methacrylate)/클레이 나노복합체 제조)

  • Kim, Yong-Ryeol;Jeong, Hyeon-Taek
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.2
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    • pp.231-237
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    • 2014
  • The supercritical fluids (SCFs) have been widely used for material synthesis and processing due to their remarkable properties including low viscosity, high diffusivity and low surface tension. Carbon dioxide is one of the suitable solvents in SCFs processes in terms of its advantages such as easy processibility (with low critical temperature and pressure), inexpensive, nonflammable, nontoxic, and readily available. However, it has generally low solubility for high molecular weight polymers with the exception of fluoropolymers and siloxane polymers. Therefore, hydrocarbon solvents and hydrochlorofluorocarbons have been used for various SCFs process by its high solubility for high molecular weight polymers. In this report, a PMMA/clay nanocomposites were fabricated by using supercritical fluid process. The $Na^+$-MMT(montmorillonites)was modified by a fluorinated surfactant which is able to enhance compatibility with the chlorodifluoromethane(HCFC-22) and thus, improve dispersability of the clay in the polymer matrix. The PMMA/fluorinated surfactant modified clay nanocomposite shows enhanced mechanical and thermal properties which characterized by X-raydiffraction(XRD), Thermo gravimetric analysis(TGA), Dynamic mechanical analysis (DMA) and Transmission electron microscopy (TEM).

Direct Incorporation of Carbon Dioxide to Poly(GMA) Using Quaternary Ammonium Salt Catalysts (4차 암모늄염 촉매를 이용한 Poly(GMA)에의 이산화탄소 직접 고정화)

  • Sung, Chung-Ki;Kim, Kyung-Hoon;Moon, Jeong-Yeol;Chun, Sung-Woo;Na, Suk-Eun;Park, Dae-Won
    • Applied Chemistry for Engineering
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    • v.10 no.1
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    • pp.129-134
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    • 1999
  • This study is related to the investigation of the direct incorporation of $CO_2$ to polymer using quaternary ammonium salt catalysts. Quaternary ammonium salts showed good catalytic activity of $CO_2$ fixation in the synthesis of poly[(1,3-dioxolane-2-oxo-4-yl)methyl methacrylate] [poly(DOMA)] by the direct incorporation of $CO_2$ to poly(glycidyl methacrylate)[poly(GMA)]. Among the salts tested, the ones with higher alkyl chain length and with more nucleophilic counter anion showed higher catalytic activity. The yield of carbon dioxide addition increased with the reaction temperature. Kinetic study was carried out by measuring the variation of $CO_2$, pressure in a high pressure batch reactor. The reaction rate was first order to the concentration of poly(GMA) and $CO_2$, respectively. The rate constant was $0.69L/mol{\cdot}h$ and Henry's constant of $CO_2$ in DMSO at $80^{\circ}C$ was $6.8{\times}10^{-4}mol/L{\cdot}KPa$.

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Low-temperature synthesis of nc-Si/a-SiNx: H quantum dot thin films using RF/UHF high density PECVD plasmas

  • Yin, Yongyi;Sahu, B.B.;Lee, J.S.;Kim, H.R.;Han, Jeon G.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.341-341
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    • 2016
  • The discovery of light emission in nanostructured silicon has opened up new avenues of research in nano-silicon based devices. One such pathway is the application of silicon quantum dots in advanced photovoltaic and light emitting devices. Recently, there is increasing interest on the silicon quantum dots (c-Si QDs) films embedded in amorphous hydrogenated silicon-nitride dielectric matrix (a-SiNx: H), which are familiar as c-Si/a-SiNx:H QDs thin films. However, due to the limitation of the requirement of a very high deposition temperature along with post annealing and a low growth rate, extensive research are being undertaken to elevate these issues, for the point of view of applications, using plasma assisted deposition methods by using different plasma concepts. This work addresses about rapid growth and single step development of c-Si/a-SiNx:H QDs thin films deposited by RF (13.56 MHz) and ultra-high frequency (UHF ~ 320 MHz) low-pressure plasma processing of a mixture of silane (SiH4) and ammonia (NH3) gases diluted in hydrogen (H2) at a low growth temperature ($230^{\circ}C$). In the films the c-Si QDs of varying size, with an overall crystallinity of 60-80 %, are embedded in an a-SiNx: H matrix. The important result includes the formation of the tunable QD size of ~ 5-20 nm, having a thermodynamically favorable <220> crystallographic orientation, along with distinct signatures of the growth of ${\alpha}$-Si3N4 and ${\beta}$-Si3N4 components. Also, the roles of different plasma characteristics on the film properties are investigated using various plasma diagnostics and film analysis tools.

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A Study on Fabrication and Characterization of Inorganic Insulation Material by Hydrothermal Synthesis Method (2) (수열합성법을 이용한 무기계 단열소재 제조방법 및 특성에 관한 연구 (2))

  • Seo, Sung-Kwan;Chu, Yong-Sik;Lee, Jong-Kyu;Song, Hun;Park, Jae-Wan
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.1 no.3
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    • pp.225-232
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    • 2013
  • The inorganic insulating material was fabricated with quartzite, ordinary portland cement(OPC), lime, anhydrous gypsum and foaming agent by hydrothermal reaction. The inorganic insulating material was fabricated by using autoclave chamber under high-temperature and high-pressure. The inorganic insulating material is a porous lightweight concrete. Because of its porous structure, properties of inorganic insulating material were light-weight and high-heat insulation property. Properties of fabricated inorganic insulating material were $0.26g/cm^3$ in specific gravity, 0.4MPa in compressive strength and 0.064W/mK in thermal conductivity. In this study, the inorganic insulating material was fabricated and analyzed at different size of quartzite/OPC, various foaming reagent and functional additives to improve the properties. Consequently, polydimethylsiloxane can improve density and thermal conductivity. Especially, polydimethylsiloxane showed excellent improvement in compressive strength.

Development of Matrix for the Immobilization of High Level Radioactive Waste : Study on the Synthesis of Ce-pyrochlore (고준위 핵페기물의 고정화를 위한 메트릭스 개발 : Ce파이로클로어 합성 연구)

  • ;;;Yudintsev, S. V²
    • Economic and Environmental Geology
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    • v.35 no.2
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    • pp.97-102
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    • 2002
  • Ce-pyrochlore (CaCe $Ti_2 $O_7)was synthesized to study its properties and phase relations in CaO-Ce $O_2$-Ti $O_2$ system because Ce-pyrochlore was known as a promising material for the immobilization of radioactive actinide. The samples were prepared from the high purity starling materials under the pressure of 200~400 kg/$\textrm{cm}^2$ at room temperature, and annealed at 1000~ 150$0^{\circ}C$. The Synthesized samples were analysed and indentified with XRD and SEM/EDS methods. The optimal formation condition of Ce-pyrochlore was at 130$0^{\circ}C$ under $O_2$ atmosphere and the chemical composition of it wasCa$Ca_{1-x}Ti_{2-y}O_{7-x-2y}$(x=0.03-0.05, y=0.02~0.04) At temperature between 130$0^{\circ}C$ 140$0^{\circ}C$, Ce-pyrochlore underwent rapidly the incongruent decomposition to perovskite. Ce-perovskite, a partial solid solution between perovskite and loparite (C $e_{0.66}$Ti $O_3$), was observed as a major phase above 140$0^{\circ}C$.>.

Thermoelectric Efficiency Improvement in Vacuum Tubes of Decomposing Liquid Lithium-Ammonia Solutions (진공튜브 속에서 분해하는 리튬암모니아 솔루션의 열전효율 향상)

  • Lee, Jungyoon;Kim, Miae;Shim, Kyuchol;Kim, Jibeom;Jeon, Joonhyeon
    • Korean Chemical Engineering Research
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    • v.51 no.3
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    • pp.358-363
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    • 2013
  • Lithium-ammonia (Li-$NH_3$) solutions are possible to be successfully made under the vacuum condition but there still remains a problem of undergoing stable and reliable decomposition in vacuum for high-efficiency thermoelectric power generation. This paper describes a new method for improving the thermoelectric conversion efficiency of Li-$NH_3$ solutions in vacuum. The proposed method uses a 'U'-shaped Pyrex vacuum tube for the preparation and decomposition of pure fluid Li-$NH_3$ solutions. The tube is shaped so that a gas passageway ('U') connecting both legs of the 'U' helps to balance pressure inside both ends of the tube (due to $NH_3$ gasification) during decomposition on the hot side. Thermoelectric experimental results show that solution reaction in the 'U'-shaped tube proceeds more stably and efficiently than in the 'U'-shaped tube, and consequently, thermoelectric conversion efficiency is improved. It is also proved that the proposed method can provide a reversible reaction, which can rotate between synthesis and decomposition in the tube, for deriving the long-time, high-efficiency thermoelectric power.

Studies on the synthesis and characteristics of calcium sulfonate complex grease (칼슘 술폰산염 컴플렉스 그리스 합성과 특성 연구)

  • Woo, Jaegu;Lee, Dongkyu;Ha, KiRyong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.7
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    • pp.8-15
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    • 2019
  • In this study, we synthesized a calcium sulfonate complex grease and a lithium complex grease to investigate their physical, rheological and tribological properties. The thermal stability of the calcium sulfonate was higher than $300^{\circ}C$ and the lithium complex grease was $245^{\circ}C$ in the dropping point test. In the grease viscosity measurement, the calcium sulfonate complex grease was measured as $7.0Pa{\cdot}s$ and the lithium complex grease was as $4.5Pa{\cdot}s$. Therefore, it was confirmed that the calcium sulfonate complex grease is superior to the lithium complex grease in terms of thermal stability and cohesiveness. In the 4-ball wear test, the calcium sulfonate complex grease was measured to be 0.43 mm and the lithium complex grease to 0.85 mm. In the 4-ball extreme pressure test, calcium sulfonate complex grease was measured as 620 kgf and the lithium complex grease was as 125 kgf. Therefore, it was confirmed that the calcium sulfonate complex grease is superior to the lithium complex grease in abrasion resistance and load-bearing property. It was found that the calcium sulfonate complex grease is more effective than the lithium complex grease in the lubrication at high temperature and high load.

Synthesis and Characterization of Interfacial Properties of Glycerol Surfactant (글리세롤계 계면활성제 합성 및 계면 특성에 관한 연구)

  • Lim, JongChoo;Lee, Seul;Kim, ByeongJo;Lee, JongGi;Choi, KyuYong
    • Applied Chemistry for Engineering
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    • v.22 no.4
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    • pp.376-383
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    • 2011
  • The CMCs of LA and LA3 nonionic surfactants obtained from the reaction between glycidol and lauryl alcohol were found to be $0.97{\times}10^{-3}mol/L$ and $1.02{\times}10^{-3}mol/L$ respectively and the surface tensions for 1 wt% surfactant were 26.99 and 27.48 mN/m respectively. Dynamic surface tension measurements using a maximum bubble pressure tensiometer showed that the adsorption rate of surfactant molecules at the interface between the air and the surfactant solution was found to be relatively fast in both surfactant systems, presumably due to the high mobility of surfactant molecules. The contact angles of LA and LA3 nonionic surfactants were 27.8 and $20.9^{\circ}$ respectively and the dynamic interfacial tension measurement by a spinning drop tensiometer showed that interfacial tensions at equilibrium condition in both systems were almost the same. Also both surfactant systems reached equilibrium in 2~3 min. Both surfactant solutions showed high stability when evaluated by conductometric method and the LA nonionic surfactant system provided the higher foam stability than the LA3 nonionic surfactant system. The phase behavior experiments showed a lower phase or oil in water (O/W) microemulsion in equilibrium with an excess oil phase at all temperatures studied. No three-phase region was observed including a middle-phase microemulsion or a lamellar liquid crystalline phase.

Synthesis and Anti-corrosion Properties of Succinic Acid Alkyl Half-amide Derivatives (숙신산 알킬 하프-아마이드 유도체의 합성 및 해수에 대한 방청성능)

  • Baek, Seung-Yeob;Kim, Young-Wun;Chung, Keun-Wo;Yoo, Seung-Hyun;Kim, Nam-Kyun
    • Clean Technology
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    • v.17 no.4
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    • pp.314-324
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    • 2011
  • Several amide derivatives have been used as additives for base oil of metal working fluids and pressure working oils. In this paper, a series of succinic acid alkyl half-amide derivatives were synthesized as over 97% yields by ring-opening reaction of succinic anhydride and several amines and were soluble in 100 N base oil within 1 wt% concentration. The structures of the synthesized amides were confirmed by $^1H$-NMR, FT-IR spectrum and GC analysis. Anti-corrosion properties of the amides in sea water were evaluated through ASTM D665 method and weight loss method. As the results of anti-corrosion properties, the properties of the amides with shorter alkyl chain and high concentration showed better performance than those with longer alkyl chain and low concentration. Also, the dialkyl amides showed better anti-corrosion properties than those of the monoalkyl amides. Inhibition efficiency% (IE%) was over 93% in the concentration of 40 ppm and corrosion rate (CR) was below 0.5 mm/year in the same concentration.

Synthesis of Uniformly Doped Ge Nanowires with Carbon Sheath

  • Kim, Tae-Heon;;Choe, Sun-Hyeong;Seo, Yeong-Min;Lee, Jong-Cheol;Hwang, Dong-Hun;Kim, Dae-Won;Choe, Yun-Jeong;Hwang, Seong-U;Hwang, Dong-Mok
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.289-289
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    • 2013
  • While there are plenty of studies on synthesizing semiconducting germanium nanowires (Ge NWs) by vapor-liquid-solid (VLS) process, it is difficult to inject dopants into them with uniform dopants distribution due to vapor-solid (VS) deposition. In particular, as precursors and dopants such as germane ($GeH_4$), phosphine ($PH_3$) or diborane ($B_2H_6$) incorporate through sidewall of nanowire, it is hard to obtain the structural and electrical uniformity of Ge NWs. Moreover, the drastic tapered structure of Ge NWs is observed when it is synthesized at high temperature over $400^{\circ}C$ because of excessive VS deposition. In 2006, Emanuel Tutuc et al. demonstrated Ge NW pn junction using p-type shell as depleted layer. However, it could not be prevented from undesirable VS deposition and it still kept the tapered structures of Ge NWs as a result. Herein, we adopt $C_2H_2$ gas in order to passivate Ge NWs with carbon sheath, which makes the entire Ge NWs uniform at even higher temperature over $450^{\circ}C$. We can also synthesize non-tapered and uniformly doped Ge NWs, restricting incorporation of excess germanium on the surface. The Ge NWs with carbon sheath are grown via VLS process on a $Si/SiO_2$ substrate coated 2 nm Au film. Thin Au film is thermally evaporated on a $Si/SiO_2$ substrate. The NW is grown flowing $GeH_4$, HCl, $C_2H_2$ and PH3 for n-type, $B_2H_6$ for p-type at a total pressure of 15 Torr and temperatures of $480{\sim}500^{\circ}C$. Scanning electron microscopy (SEM) reveals clear surface of the Ge NWs synthesized at $500^{\circ}C$. Raman spectroscopy peaked at about ~300 $cm^{-1}$ indicates it is comprised of single crystalline germanium in the core of Ge NWs and it is proved to be covered by thin amorphous carbon by two peaks of 1330 $cm^{-1}$ (D-band) and 1590 $cm^{-1}$ (G-band). Furthermore, the electrical performances of Ge NWs doped with boron and phosphorus are measured by field effect transistor (FET) and they shows typical curves of p-type and n-type FET. It is expected to have general potentials for development of logic devices and solar cells using p-type and n-type Ge NWs with carbon sheath.

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