• 제목/요약/키워드: 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
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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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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합성 금속-유기 골격체 NH2-MIL-101(Fe)를 이용한 염료의 흡착 및 광분해 제거 (Adsorption and Photocatalytic Degradation of Dyes Using Synthesized Metal-Organic Framework NH2-MIL-101(Fe))

  • 이준엽;최정학
    • 한국환경과학회지
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    • 제27권7호
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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
    • 한국세라믹학회지
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    • 제50권4호
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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.

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.

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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    • 제54권10호
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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.

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

  • 안기호;신내철;김민수;윤용석;홍기영;이윤우
    • Korean Chemical Engineering Research
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    • 제50권4호
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    • pp.678-683
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    • 2012
  • 세리아 미세입자는 자동차, 석유공정, 폐수처리 등 다양한 분야에서 촉매로서 널리 쓰이고 있는 중요한 물질이다. 이제까지, 세리아 미세입자를 제조하기 위한 다양한 제조법이 연구되었는데, 본 연구에서는 짧은 반응시간과 간단한 공정이 가능한 초임계 메탄올을 이용하는 입자 제조 공정을 통해 세리아 나노입자를 제조하였다. 회분식 반응기를 이용하여 짧은 시간 안에 세리아 나노입자를 제조하는데 성공하였다. 초임계 메탄올을 이용하여 세리아 나노입자를 제조하는 경우, 다른 첨가제 없이도 약 6 nm의 크기를 갖는 나노입자를 합성할 수 있었다. 이 크기는 같은 온도와 압력조건의 초임계수를 이용하여 표면개질제 없이 합성한 입자보다 훨씬 작은 크기이다. 이는 초임계수와 초임계 메탄올의 밀도 차이와, 초임계 메탄올에서의 세리아 표면에서 일어나는 결정성장을 제한하는 반응, 그리고 초임계 메탄올과 초임계수의 임계점의 차이에서 기인하는 것이다. 또한 여러 가지 유기물을 표면개질제로 첨가하여 표면을 개질한 세리아 나노입자를 제조하였으며, FT-IR과 HR-TEM, TGA를 통해 이를 확인할 수 있었다. 표면을 개질한 세리아 나노입자는 표면개질을 하지 않은 세리아 나노입자와는 다르게, 유기용매에 대한 분산성이 뛰어났으며, 표면개질제로 사용하는 유기물의 양과 종류를 조절함으로써 세리아 나노입자의 크기와 모양을 조절할 수 있었다.