• Title/Summary/Keyword: Solvothermal Synthesis

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Synthesis of Nano-Sized Y3Al5O12:Ce3+ Phosphors Prepared by High Energy Beads Milling Process and Their Luminescence Properties

  • Song, Hee-Jo;Kim, Dong-Hoe;Park, Jong-Hoon;Han, Byung-Suh;Hong, Kug-Sun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.386-386
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    • 2012
  • For white light emitting diode (LED) applications, it has been reported that Y3Al5O12:Ce3+ (YAG:Ce) in nano-sized phosphor performs better than it does in micro-sized particles. This is because nano-sized YAG:Ce can reduce internal light scattering when coated onto a blue LED surface. Recently, there have been many reports on the synthesis of nano-sized YAG particles using bottom-up method, such as co-precipitation method, sol-gel process, hydrothermal method, solvothermal method, and glycothermal method. However, there has been no report using top-down method. Top-down method has advantages than bottom-up method, such as large scale production and easy control of doping concentration and particle size. Therefore, in this study, nano-sized YAG:Ce phosphors were synthesized by a high energy beads milling process with varying beads size, milling time and milling steps. The beads milling process was performed by Laboratory Mill MINICER with ZrO2 beads. The phase identity and morphology of nano-sized YAG:Ce were characterized by X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FESEM), respectively. By controlling beads size, milling time and milling steps, we synthesized a size-tunable and uniform nano-sized YAG:Ce phosphors which average diameters were 100, 85 and 40 nm, respectively. After milling, there was no impurity and all of the peaks were in good agreement with YAG (JCPDS No. 33-0040). Luminescence and quantum efficiency (QE) of nano-sized YAG:Ce phosphors were measured by fluorescence spectrometer and QE measuring instrument, respectively. The synthesized YAG:Ce absorbed light efficiently in the visible region of 400-500 nm, and showed single broadband emission peaked at 550 nm with 50% of QE. As a result, by considering above results, high energy beads milling process could be a facile and reproducible synthesis method for nano-sized YAG:Ce phosphors.

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Adsorption and Photocatalytic Degradation of Dyes Using Synthesized Metal-Organic Framework NH2-MIL-101(Fe) (합성 금속-유기 골격체 NH2-MIL-101(Fe)를 이용한 염료의 흡착 및 광분해 제거)

  • Lee, Joon Yeob;Choi, Jeong-Hak
    • Journal of Environmental Science International
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    • v.27 no.7
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    • pp.611-620
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    • 2018
  • In this study, a metal-organic framework (MOF) material $NH_2$-MIL-101(Fe) was synthesized using the solvothermal method, and characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), UV-visible spectrophotometry, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), and surface area measurements. The XRD pattern of the synthesized $NH_2$-MIL-101(Fe) was similar to the previously reported patterns of MIL-101 type materials, which indicated the successful synthesis of $NH_2$-MIL-101(Fe). The FT-IR spectrum showed the molecular structure and functional groups of the synthesized $NH_2$-MIL-101(Fe). The UV-visible absorbance spectrum indicated that the synthesized material could be activated as a photocatalyst under visible light irradiation. FE-SEM and TEM images showed the formation of hexagonal microspindle structures in the synthesized $NH_2$-MIL-101(Fe). Furthermore, the EDS spectrum indicated that the synthesized material consisted of Fe, N, O, and C elements. The synthesized $NH_2$-MIL-101(Fe) was then employed as an adsorbent and photocatalyst for the removal of Indigo carmine and Rhodamine B from aqueous solutions. The initial 30 min of adsorption for Indigo carmine and Rhodamine B without light irradiation achieved removal efficiencies of 83.6% and 70.7%, respectively. The removal efficiencies thereafter gradually increased with visible light irradiation for 180 min, and the overall removal efficiencies for Indigo carmine and Rhodamine B were 94.2% and 83.5%, respectively. These results indicate that the synthesized MOF material can be effectively applied as an adsorbent and photocatalyst for the removal of dyes.

Easy and Fast Synthesis of Pd-MWCNT/TiO2 by the Sol-Gel Method and its Recyclic Photodegradation of Rhodamine B

  • Ye, Shu;Ullah, Kefayat;Zhu, Lei;Meng, Ze-Da;Sun, Qian;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.50 no.4
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    • pp.251-256
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    • 2013
  • Multiwalled carbon nanotubes (MWCNTs) modified with Pd and $TiO_2$ composite catalysts were synthesized by the sol-gel method followed by solvothermal treatment at low temperature. The chemical composition and surface structure were characterized by X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Photocatalytic recycle degradation experiments were carried out under both UV and visible light irradiation in the presence of MWCNT/$TiO_2$ and Pd-MWCNT/$TiO_2$ composites. As expected, the nanosized Pd-MWCNT/$TiO_2$ photocatalysts had enhanced activity over the non Pd treated MWCNT/$TiO_2$ material in the degradation of a rhodamine B (Rh.B) solution. An increase in photocatalytic activity was observed and attributed to an increase in the photo-absorption effect by MWCNTs and the cooperative effect of Pd and $TiO_2$ nanoparticles. According to the recycled results, the as-prepared Pd-MWCNT/$TiO_2$ sample had a good effect on it.

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

  • Lee, Won-Woo;Shin, Chae-Ho;Park, Han-Sung;Choi, Young-Min;Ryu, Beyong-Hwan
    • Korean Journal of Materials Research
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    • v.18 no.10
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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.

One-pot synthesis of silica-gel-based adsorbent with Schiff base group for the recovery of palladium ions from simulated high-level liquid waste

  • Wu, Hao;Kim, Seong-Yun;Ito, Tatsuya;Miwa, Misako;Matsuyama, Shigeo
    • Nuclear Engineering and Technology
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    • v.54 no.10
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    • pp.3641-3649
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    • 2022
  • A simple solvothermal reaction was used to prepare a 3-aminopropyl-functionalized silica-gel-based adsorbent for adsorbing Pd(II) from the nitric acid solution. Scanning electron microscopy, fourier transform infrared spectroscopy, and thermogravimetry analysis were performed on the as-synthesized adsorbent to demonstrate the successful introduction of Schiff base groups. Batch experiments were used to investigate the effects of contact time, nitric acid concentration, solution temperature, and adsorption capacity. It is worth noting that the prepared adsorbent exhibited a higher affinity toward Pd(II) with the uptake approximately 100% even in a 2 M HNO3 solution. At an equilibrium time of 5 h, the maximum adsorption capacity of Pd(II) was estimated to be 0.452 mmol/g. The adsorbed Pd(II) could be completely eluted by dissolving 0.2 M thiourea solution in 0.1 M HNO3. Using a combination of particle-induced X-ray emission analysis and an X-ray photoelectron spectrometer, the adsorbed Pd was found to be uniformly distributed on the surface of the prepared adsorbent and the existing species were Pd(II) and zero-valent Pd(0). Due to the desirable performances, facile preparation method, and abundant raw material source, the prepared adsorbent demonstrated a high application potential in the recovery of Pd(II) from simulated high-level liquid waste treatment.

Synthesis of Ceria Nanoparticles Using Supercritical Methanol with Various Surface Modifiers (초임계 메탄올을 이용한 표면개질된 세리아 나노입자의 합성)

  • Ahn, Ki Ho;Shin, Nae-Chul;Kim, Minsoo;Youn, Yong-Suk;Hong, Giyoung;Lee, Youn-Woo
    • Korean Chemical Engineering Research
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    • v.50 no.4
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    • pp.678-683
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    • 2012
  • Ceria is one of the most important catalytic materials which can be used in three-way catalysts, waste water treatment, petroleum refining, etc. So far, many methods have been studied to produce ceria nanoparticles. In this study, ceria nanoparticles were prepared via solvothermal synthesis using supercritical methanol in short reaction time using a batch reactor. The size of synthesized ceria nanoparticles in supercritical methanol is 6 nm without capping agent, which is smaller than that made in supercritical water at the same conditions of $400^{\circ}C$ and 30 MPa. Size difference results from density and critical point difference between water and methanol and slow reaction rate at the surface of ceria particles in supercritical methanol which reduces crystal growth rate. Several organic compounds were added to modify the surface of ceria nanoparticles, and in-situ surface modification was confirmed by FT-IR and TGA analysis. Surface modified ceria nanoparticles have excellent dispersibility in organic solvent. Size and shape of surface modified ceria particles can be controlled by adjusting molar ratio of modifier to precursor and selection of modifier.