• 제목/요약/키워드: Synthesis parameters

검색결과 691건 처리시간 0.026초

용매열 공정을 이용한 세리아(CeO2) 나노분말의 합성 및 분산거동 (Synthesis and Dispersion of Ceria(CeO2) Nanoparticles by Solvothermal Process)

  • 임태섭;옥지영;최연빈;김봉구;손정훈;정연길
    • 한국재료학회지
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    • 제30권7호
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    • pp.376-382
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    • 2020
  • CeO2 nanoparticles, employed in a lot of fields due to their excellent oxidation and reduction properties, are synthesized through a solvothermal process, and a high specific surface area is shown by controlling, among various process parameters in the solvothermal process, the type of solvent. The synthesized CeO2 nanoparticles are about 11~13 nm in the crystallite size and their specific surface area is about 65.38~84.65 ㎡/g, depending on the amount of ethanol contained in the solvent for the solvothermal process; all synthesized CeO2 nanoparticles shows a fluorite structure. The dispersibility and microstructure of the synthesized CeO2 nanoparticles are investigated according to the species of dispersant and the pH value of the solution; an improvement in dispersibility is shown with the addition of dispersants and control of the pH. Various dispersing properties appear according to the dispersant species and pH in the solution with the synthesized CeO2 nanoparticles, indicating that improved dispersing properties in the synthesized CeO2 nanoparticles can be secured by applying dispersant and pH control simultaneously.

Synthesis and Photocatalytic Properties of Thermally Stable Metal-Oxide Hybrid Nanocatalyst with Ultrathin Oxide Encapsulation

  • Naik, Brundabana;Moon, Song Yi;Kim, Sun Mi;Jung, Chan Ho;Park, Jeong Young
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.317.2-317.2
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    • 2013
  • Ultrathin oxide encapsulated metal-oxide hybrid nanocatalysts have been fabricated by a soft chemical and facile route. First, SiO2 nanoparticles of 25~30 nm size have been synthesized by modified Stobber's method followed by amine functionalization. Metal nanoparticles (Ru, Rh, Pt) capped with polymer/citrate have been deposited on functionalized SiO2 and finally an ultrathin layer of TiO2 coated on surface which prevents sintering and provides high thermal stability while maximizing the metal-oxide interface for higher catalytic activity. TEM studies confirmed that 2.5 nm sized metal nanoparticles are well dispersed and distributed throughout the surface of 25 nm SiO2 nanoparticles with a 3-4 nm TiO2 ultrathin layer. The metal nanoparticles are still well exposed to outer surface, being enabled for surface characterization and catalytic activity. Even after calcination at $600^{\circ}C$, the structure and morphology of hybrid nanocatalysts remain intact confirm the high thermal stability. XPS spectra of hybrid nanocatalyst suggest the metallic states as well as their corresponding oxide states. The catalytic activity has been evaluated for high temperature CO oxidation reaction as well as photocatalytic H2 generation under solar simulation. The design of hybrid structure, high thermal stability, and better exposure of metal active sites are the key parameters for the high catalytic activity. The maximization of metal-TiO2 interface interaction has the great role in photocatalytic H2 production.

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액상법에 의한 Carbon Nanofiber 제조 및 특성 분석 (Preparation and Characterization of Carbon Nanofiber from Liquid Phase Carbon Source)

  • 이원우;신채호;박한성;최영민;류병환
    • 한국재료학회지
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    • 제18권10호
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    • pp.564-570
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    • 2008
  • Nanostructured carbon materials have been found to have applications in fuel cell electrodes, field emitters, electronic devices, sensors and electromagnetic absorbers, etc. Especially, the CNF (carbon nanofiber) can be expected to play an important role in catalyst supporters for fuel cell electrodes and chemical reactions. In this study, we synthesized CNF from a liquid phase carbon source by a solvothermal method. In addition, we studied the parameters for the preparation of CNF by controlling heating and cooling rates, synthesis temperature and time. We characterized the CNF by SEM/TEM, XRD, Raman spectroscopy and EDS. We found that the heating and cooling rate have strong effects on the CNF formation and growth. We were able to prepare the best CNF at the heating rate of $10^{\circ}$/min, at $450^{\circ}$ for 60 minutes, and at the cooling rate of $4^{\circ}$/min. As a result of Raman spectra, we found that the sample showed two characteristic Raman bands at ${\sim}1350cm^{-1}$ (D band) and ${\sim}1600cm^{-1}$ (G band). The G band indicates the original graphite feature, but the D band has been explained as a disorder feature of the carbon structure. The diameter and length of the CNF was about $15{\sim}20nm$, and over $1{\mu}$, respectively.

Resol형 페놀수지의 합성과 반응특성 (Synthesis of Resol Type Phenol Resins and Their Reaction Properties)

  • 김동권;조지은;김정훈;박인준;이수복
    • 공업화학
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    • 제16권2호
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    • pp.288-291
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    • 2005
  • Resol형 페놀수지(phenol-formaldehyde (PF) resin)는 페놀(phenol: P)에 포름알데히드(formaldehyde: F)를 첨가하여 반응시키는 부가반응과 물을 제거하는 축합반응에 의해 합성된다. 본 연구에서는 부가반응 반응변수인 F/P몰비, 촉매의 농도, 반응온도 및 반응시간 등의 영향에 관하여 연구하였다. 또한 반응시간의 조절에 따른 합성된 페놀수지의 분자량과 점도에 미치는 영향을 조사하였다. 실험결과, 부가반응에서 촉매농도와 반응온도가 높아질수록 반응시간은 크게 감소되는 경향을 나타내었다. 또한 축합반응에서 페놀수지의 점도는 반응시간이 증가할수록 1500cps에서 9000 cps까지 증가하였고, 분자량은 500~1100 g/mol 범위의 저 분자량을 나타내었다.

A study on membrane technology for surface water treatment: Synthesis, characterization and performance test

  • Haan, Teow Yeit;Shah, Mubassir;Chun, Ho Kah;Mohammad, Abdul Wahab
    • Membrane and Water Treatment
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    • 제9권2호
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    • pp.69-77
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    • 2018
  • The use of membrane as an innovative technology for water treatment process has now widely been accepted and adopted to replace the conventional water treatment process in increasing fresh water production for various domestic and industrial purposes. In this study, ultrafiltration (UF) membranes with different formulation were fabricated via phase inversion method. The membranes were fabricated by varying the polymer concentration (16 wt%, 18 wt%, 20 wt%, and 21 wt%). A series of tests, such as field emission scanning electron microscope (FESEM), pore size and porosity, contact angle, and zeta potential were performed to characterize the membranes. The membrane performance in terms of permeation flux and rejection were evaluated using a laboratory bench-scale test unit with mine water, lake water and tube well as model feed solution. Long hour filtration study of the membranes provides the information on its fouling property. Few pore blocking mechanism models were proposed to examine the behaviour of flux reduction and to estimate the fouling parameters based on different degree of fouling. 21 wt% PVDF membrane with smaller membrane pore size showed an excellent performance for surface water treatment in which the treated water complied with NWQS class II standard.

Synthesis and Characterization of Group VI Metal Carbonyl Complexes Containing closo-1,2-$(PPh_2)_2$-1,2-$C_2B_1_0H_1_0$ and Their Conversion to Metal Carbene Complexes

  • 박영일;김세진;고재정;강상욱
    • Bulletin of the Korean Chemical Society
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    • 제18권10호
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    • pp.1061-1066
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    • 1997
  • The complexes M(CO)4-1,2-(PPh2)2-1,2-C2B10H10 (M=Cr 2a, Mo 2b, W 2c) have been prepared in good yields from readily available bis-diphenylphosphino-o-carboranyl ligand, closo-1,2-(PPh2)2-1,2-C2B10H10 (1), by direct reaction with Group Ⅵ metal carbonyls. The infrared spectra of the complexes indicate that there is an octahedral disposition of chelate bis-diphenylphosphino-o-carboranyl ligand around the metal atom. The crystal structure of 2a was determined by X-ray diffraction. Complex 2a crystallizes in the monoclinic space group P21/n with cell parameters a = 12.2360(7), b = 17.156(1), c = 16.2040(6) Å, V = 3354.1(3) Å3, and Z =4. Of the reflections measured a total of 2514 unique reflections with F2 > 3σ(F2) was used during subsequent structure refinement. Refinement converged to R1 = 0.066 and R2 = 0.071. Structural studies showed that the chromium atom had a slightly distorted pseudo-octahedral configuration about the metal center with two phosphine groups of o-carborane occupying the equatorial plane cis-orientation to each other. These metal carbonyl complexes are rapidly converted to the corresponding metal carbene complexes, [(CO)3M=C(OCH3)(CH3)]-1,2-(PPh2)2-1,2-C2B10H10 (M= Cr 3a, Mo 3b, W 3c), via alkylation with methyllithium followed by O-methylation with CF3SO3CH3.

Synthesis of Novel (Be,Mg,Ca,Sr,Zn,Ni)3O4 High Entropy Oxide with Characterization of Structural and Functional Properties and Electrochemical Applications

  • Arshad, Javeria;Janjua, Naveed Kausar;Raza, Rizwan
    • Journal of Electrochemical Science and Technology
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    • 제12권1호
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    • pp.112-125
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    • 2021
  • The new emerging "High entropy materials" attract the attention of the scientific society because of their simpler structure and spectacular applications in many fields. A novel nanocrystalline high entropy (Be,Mg,Ca,Sr,Zn,Ni)3O4 oxide has been successfully synthesized through mechanochemical treatment followed by sintering and air quenching. The present research work focuses on the possibility of single-phase formation in the aforementioned high entropy oxide despite the great difference in the atomic sizes of reactant alkaline earth and 3d transition metal oxides. Structural properties of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide were explored by confirmation of its single-phase Fd-3m spinel structure by x-ray diffraction (XRD). Further, nanocrystalline nature and morphology were analyzed by scanning electron microscopy (SEM). Among thermal properties, thermogravimetric analysis (TGA) revealed that the (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is thermally stable up to a temperature of 1200℃. Whereas phase evolution in (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide before and after sintering was analyzed through differential scanning calorimetry (DSC). Electrochemical studies of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide consists of a comparison of thermodynamic and kinetic parameters of water and hydrazine hydrate oxidation. Values of activation energy for water oxidation (9.31 kJ mol-1) and hydrazine hydrate oxidation (13.93 kJ mol-1) reveal that (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is catalytically more active towards water oxidation as compared to that of hydrazine hydrate oxidation. Electrochemical impedance spectroscopy is also performed to get insight into the kinetics of both types of reactions.

Optimization and Packed Bed Column Studies on Esterification of Glycerol to Synthesize Fuel Additives - Acetins

  • Britto, Pradima J;Kulkarni, Rajeswari M;Narula, Archna;Poonacha, Sunaina;Honnatagi, Rakshita;Shivanathan, Sneha;Wahab, Waasif
    • Korean Chemical Engineering Research
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    • 제60권1호
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    • pp.70-79
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    • 2022
  • Biodiesel production has attracted attention as a sustainable source of fuel and is a competitive alternate to diesel engines. The glycerol that is produced as a by-product is generally discarded as waste and can be converted to green chemicals such as acetins to increase bio-diesel profitability. Acetins find application in fuel, food, pharmaceutical and leather industries. Batch experiments and analysis have been previously conducted for synthesis of acetins using glycerol esterification reaction aided by sulfated metal oxide catalysts (SO42-/CeO2-ZrO2). The aim of this study was to optimize process parameters: effects of mole ratio of reactants (glycerol and acetic acid), catalyst concentration and reaction temperature to maximize glycerol conversion/acetin selectivity. The optimum conditions for this reaction were determined using response surface methodology (RSM) designed as per a five-level-three-factor central composite design (CCD). Statistica software 10 was used to analyze the experimental data obtained. The optimized conditions obtained were molar ratio - 1:12, catalyst concentration - 6 wt.% and temperature -90 ℃. A packed bed reactor was fabricated and column studies were performed using the optimized conditions. The breakthrough curve was analyzed.

Synthesis of Hyaluronic Acid Microsphere Crosslinked with Polyethylene Glycol Diglycidyl Ether Prepared by A Simple Fluidic Device

  • Yuk, Sujeong;Jeong, Dayeon;Lee, Yongjun;Lee, Deuk Yong
    • 대한의용생체공학회:의공학회지
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    • 제42권6호
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    • pp.251-258
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    • 2021
  • Hyaluronic acid (HA) microspheres (MSs) crosslinked with polyethylene glycol diglycidyl ether (PEGDE) are prepared using a simple fluidic device (SFD) to investigate the optimized parameters. A solution mixture of PEGDE in 2-methyl-1-propanol was prepared as a continuous phase in SFD. HA solutions of 1 wt% concentration were introduced into SFD as a discontinuous phase. The HA solution prepared by stirring for more than 48 h exhibited spherical MSs at the needle tip inside the ring cap. As the flow rate of the continuous phase increased from 0.7 to 1.9 mL/min, the diameter of the MS decreased from 173±36 ㎛ to 129±13 ㎛. Although the PEGDE concentration in the range of 0.2 to 1.8 vol% did not affect the diameter of the MS, the microstructure of MS, consisting of inner hollow void and wall, was changed. The inner void and wall size decreased and increased from 79.5 ㎛ to 57.2 ㎛ and from 10.3 ㎛ to 21.4 ㎛, respectively, with increasing PEGDE concentration from 0.2 vol% to 1.8 vol%. FT-IR peaks located around 2867 cm-1 and 1088 cm-1 indicated that the HA MS prepared at different PEGDE concentrations were chemically crosslinked. The HA MSs containing different PEGDE concentrations exhibited quantitative cell viability of more than 98%. L-929 cells adhered well to the HA MSs and proliferated continuously with increasing culture time to 48 h regardless of PEGDE concentration, implying that the HA MSs are clinically safe and effective.

Absolute Dimensions And Period Changes Of The Semi-Detached Algol Type Binary XZ Canis Minoris

  • Kim, Hye-Young;Kim, Chun-Hwey;Hong, Kyeongsoo;Jeong, Min-Ji;Park, Jang-Ho;Song, Mi-Hwa;Lee, Jae Woo;Lee, Chung-Uk
    • 천문학회보
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    • 제44권2호
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    • pp.64.1-64.1
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    • 2019
  • The first high-resolution spectroscopic and new multiband photometric observations of the semi-detached Algol type binary XZ CMi were performed at the Bohyunsan Optical Astronomy Observatory (BOAO) and the Sobaeksan Optical Astronomy Observatory (SOAO), respectively. A total of 34 spectra were obtained using the 1.8 m reflector of the BOAO equipped with the Bohyunsan Optical Echelle Spectrograph to construct the radial velocity (RV) curves of the eclipsing pair. New BVRI photometric light curves were also covered by using the SOAO 61cm reflector and a CCD camera. A detailed analysis of all eclipse timings shows that the orbital period of XZ CMi has varied in an upward parabolic variation superposed on a sinusoidal oscillation with a period of 38.0 yr and a semi-amplitude of 0.0071 days. From the spectral analysis, the effective temperature and the projected rotational velocity of the primary component were determined to be Teff,1 = 7387±161 K and v1sini = 122±6 km s-1, respectively. Our simultaneous synthesis of the double-lined RV and BVRI light curves gives the reliable system parameters of XZ CMi with a mass ratio (q) of 0.314, an orbital inclination (i) of 81.9 deg and a large temperature difference (∆T) of 2481 K. The individual masses and radii of both components are M1 = 1.91±0.08M, M2 = 0.60±0.02M, R1 = 1.60±0.02R, R2 = 1.13±0.02R, respectively. Although the primary component is located inside the δ Sct and γ Dor instability strips, no evidence of pulsation in the system was detected. The possible evolutionary status of XZ CMi is discussed.

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