In this work, TiO2 3D nanostructures (TF30) were prepared via a facile wet chemical process using ammonium hexafluorotitanate. The synthesized 3D TiO2 nanostructures exhibited well-defined crystalline and hierarchical structures assembled from TiO2 nanorods with different thicknesses and diameters, which comprised numerous small beads. Moreover, the maximum specific surface area of TiO2 3D nanostructures was observed to be 191 m2g-1, with concentration of F ions on the surface being 2 at%. The TiO2 3D nanostructures were tested as photocatalysts under UV irradiation using Rhodamine B solution in order to determine their photocatalytic performance. The TiO2 3D nanostructures showed a higher photocatalytic activity than that of the other TiO2 samples, which was likely associated with the combined effects of a high crystallinity, unique features of the hierarchical structure, a high specific surface area, and the advantage of adsorbing F ions.
A facile one-pot wet chemical process to prepare pure anatase TiO2 hollow structures using ammonium hexafluorotitanate as a precursor is developed. By defining the formic acid ratio, we fabricate TiO2 hollow structures containing fluorine on the surface. The TiO2 hollow sphere is composed of an anatase phase containing fluorine by various analytical techniques. A possible formation mechanism for the obtained hollow samples by self-transformation and Ostwald ripening is proposed. The TiO2 hollow structures containing fluorine exhibits 1.2 - 2.7 times higher performance than their counterparts in photocatalytic activity. The enhanced photocatalytic activity of the TiO2 hollow structures is attributed to the combined effects of high crystallinity, specific surface area (62 m2g-1), and the advantage of surface fluorine ions (at 8%) having strong electron-withdrawing ability of the surface ≡ Ti-F groups reduces the recombination of photogenerated electrons and holes.
In this study, the effects of Sm addition (0, 0.05, 0.2, 0.5 wt%) on the microstructure, hardness, and electrical and thermal conductivity of Al-11Si-1.5Cu aluminum alloy were investigated. As a result of Sm addition, increment in the amount of α-Al and refinement of primary Si from 70 to 10 μm were observed due to eutectic temperature depression. On the other hand, Sm was less effective at refining eutectic Si because of insufficient addition. The phase analysis results indicated that Sm-rich intermetallic phases such as Al-Fe-Mg-Si and Al-Si-Cu formed and led to decrements in the amount of primary Si and eutectic Si. These microstructure changes affected not only the hardness but also the electrical and thermal conductivity. When 0.5 wt% Sm was added to the alloy, hardness increased from 84.4 to 91.3 Hv, and electric conductivity increased from 15.14 to 16.97 MS/m. Thermal conductivity greatly increased from 133 to 157 W/m·K.
Ti has received considerable attention for aerospace, vehicle, and semiconductor industry applications because of its acid-resistant nature, low density, and high mechanical strength. A common precursor used for preparing Ti materials is TiCl4. To prepare high-purity TiCl4, a process based on the removal of VOCl3 has been widely applied. However, VOCl3 removal by distillation and condensation is difficult because of the similar physical properties of TiCl4 and VOCl3. To circumvent this problem, in this study, we have developed a process for VOCl3 removal using Cu powder and mineral oil as purifying agents. The effects of reaction time and temperature, and ratio of purifying agents on the VOCl3 removal efficiency are investigated by chemical and structural measurements. Clear TiCl4 is obtained after the removal of VOCl3. Notably, complete removal of VOCl3 is achieved with 2.0 wt% of mineral oil. Moreover, the refined TiCl4 is used as a precursor for the synthesis of Ti powder. Ti powder is fabricated by a thermal reduction process at 1,100oC using an H2-Ar gas mixture. The average size of the Ti powder particles is in the range of 1-3 μm.
In this paper, the recovery and nanoparticle synthesis of Ag from low temperature co-fired ceramic (LTCC) by-products are studied. The effect of reaction behavior on Ag leaching conditions from the LTCC by-products is confirmed. The optimum leaching conditions are determined to be: 5 M HNO3, a reaction temperature of 75℃, and a pulp density of 50 g/L at 60 min. For the selective recovery of Ag, the [Cl]/[Ag] equivalence ratio experiment is performed using added HCl; most of the Ag (more than 99%) is recovered. The XRD and MP-AES results confirm that the powder is AgCl and that impurities are at less than 1%. Ag nanoparticles are synthesized using a chemical reduction process for recycling, NaBH4 and PVP are used as reducing agents and dispersion stabilizers. UV-vis and FE-SEM results show that AgCl powder is precipitated and that Ag nanoparticles are synthesized. Ag nanoparticles of 100% Ag are obtained under the chemical reaction conditions.
F-containing TiO2 nanopowders are synthesized using simple wet processes (precipitation-based and hydrothermal) from ammonium hexafluorotitanate (AHFT, (NH4)2TiF6) as a precursor to apply as a photocatalyst for the degradation of rhodamine B (RhB). The surface properties of the prepared samples are evaluated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). The results confirm that the synthesized anatase TiO2 has sphere-like shapes, with numerous small nanoparticles containing fluorine on the surface. The photocatalytic activity of F-containing TiO2 compared with F-free TiO2 is characterized by measuring the degradation of RhB using a xenon lamp. The photocatalytic degradation of F-containing TiO2 exhibits improved photocatalytic activity, based on the positive effects of adsorbed F ions on the surface.
Core/shell CdSe/ZnS quantum dots (QDs) are synthesized by a microfluidic reactor-assisted continuous reactor system. Photoluminescence and absorbance of synthesized CdSe/ZnS core/shell QDs are investigated by fluorescence spectrophotometry and online UV-Vis spectrometry. Three reaction conditions, namely; the shell coating reaction temperature, the shell coating reaction time, and the ZnS/CdSe precursor volume ratio, are combined in the synthesis process. The quantum yield of the synthesized CdSe QDs is determined for each condition. CdSe/ZnS QDs with a higher quantum yield are obtained compared to the discontinuous microfluidic reactor synthesis system. The maximum quantum efficiency is 98.3% when the reaction temperature, reaction time, and ZnS/CdSe ratio are 270℃, 10 s, and 0.05, respectively. Obtained results indicate that a continuous synthesis of the Core/shell CdSe/ZnS QDs with a high quantum efficiency could be achieved by isolating the reaction from the external environment.
In this study, simple chemical synthesis of green emitting Cd-free InP/ZnS QDs is accomplished by reacting In, P, Zn, and S precursors by one-pot process. The particle size and the optical properties were tailored, by controlling various experimental conditions, including [In]/[MA] (MA: myristic acid) mole ratio, reaction temperature and reaction time. The results of ultraviolet–visible spectroscopy (UV-vis), and of photoluminescence (PL), reveal that the exciton emission of InP was improved by surface coating, with a layer of ZnS. We report the correlation between each experimental condition and the luminescent properties of InP/ZnS core/shell QDs. Transmission electron microscopy (TEM), and X-ray powder diffraction (XRD) techniques were used to characterize the as-synthesized QDs. In contrast to core nanoparticles, InP/ZnS core/shell treated with surface coating shows a clear ultraviolet peak. Besides this work, we need to study what clearly determines the shell kinetic growth mechanism of InP/ZnS core shell QDs.
We have investigated the washing method of as-synthesized CdSe/ZnS core/shell structure quantum dots (QDs) and the effective surface passivation method of the washed QDs using PMMA. The quantum yield (QY%) of assynthesized QDs decreases with time, from 79.3% to 21.1%, owing to surface reaction with residual organics. The decreased QY% is restored to the QY% of as-synthesized QDs by washing. However, the QY% of washed QDs also decreases with time, owing to the absence of surface passivation layer. On the other hand, the PMMA-treated QDs maintained a relatively higher QY% after washing than that of the washed QDs that were kept in toluene solution for 30 days. Formation of the PMMA coating layer on CdSe/ZnS QD surface is confirmed by HR-TEM and FT-IR. It is found that the PMMA surface coating, when combined with washing, is useful to be applied in the storage of QDs, owing to its long-term stability.
In this study, TiO2 powders are synthesized from ammonium hexafluoride titanate (AHFT, (NH4)2TiF6) as a precursor by heat treatment. First, we evaluate the physical properties of AHFT using X-ray diffraction (XRD), particle size analysis (PSA), thermogravimetric analysis (TGA), and field-emission scanning electron microscopy (FESEM). Then, to prepare the TiO2 powders, is heat-treated at 300-1300oC for 1 h. The ratio of anatase to rutile phase in TiO2 is estimated by XRD. The anatase phase forms at 500oC and phase transformation to the rutile phase occurs at 1200oC. Increase in the particle size is observed upon increasing the reaction temperature, and the phase ratio of the rutile phase is determined from a comparison with the calculated XRD data. Thus, we show that anatase and rutile TiO2 powders could be synthesized using AHFT as a raw material, and the obtained data are utilized for developing a new process for producing high-quality TiO2 powder.
A microfluidic reactor with computer-controlled programmable isocratic pumps and online detectors is employed as a combinatorial synthesis system to synthesize and analyze materials for fabricating CdSe quantum dots for various applications. Four reaction condition parameters, namely, the reaction temperature, reaction time, Cd/Se compositional ratio, and precursor concentration, are combined in synthesis condition sets, and the size of the synthesized CdSe quantum dots is determined for each condition. The average time corresponding to each reaction condition for obtaining the ultraviolet–visible absorbance and photoluminescence spectra is approximately 10 min. Using the data from the combinatorial synthesis system, the effects of the reaction conditions on the synthesized CdSe quantum dots are determined. Further, the data is used to determine the relationships between the reaction conditions and the CdSe particle size. This method should aid in determining and selecting the optimal conditions for synthesizing nanoparticles for diverse applications.
Leaching of MOCVD dust in the LED industry is an essential stage for hydro-metallurgical recovery of pure Ga and In. To recover Ga and In, the leaching behavior of MOCVD scrap of an LED, which contains significant amounts of Ga, In, Al and Fe in various phases, has been investigated. The leaching process must be performed effectively to maximize recovery of Ga and In metals using the most efficient lixiviant. Crystalline structure and metallic composition of the raw MOCVD dust were analyzed prior to digestion. Subsequently, various mineral acids were tested to comprehensively study and optimize the leaching parameters such as acidity, pulp density, temperature and time. The most effective leaching of Ga and In was observed for a boiling 4 M HCl solution vigorously stirred at 400 rpm. Phase transformation of GaN into gallium oxide by heat treatment also improved the leaching efficiency of Ga. Subsequently high purity Ga and In can be recovered by series of hydro processes.
Nowadays, research and development on quantum dot have been intensively and comprehensively pursued worldwide in proportion to concurrent breakthrough in the field of nanotechnology. At present, quantum dot technology forms the main interdisciplinary basis of energy, biological and photoelectric devices. More specifically, quantum dot semiconductor is quite noteworthy for its sub-micro size and possibility of photonic frequency modulation capability by controlling its size, which has not been possible with conventionally fabricated bulk or thin film devices. This could lead to realization of novel high performance devices. To further understand related background knowledge of semiconductor quantum dot at somewhat extensive level, a review paper is presently drafted to introduce basics of (semiconductor) quantum dot, its properties, applications, and present and future market trend and prospect.
현재 국내 디스플레이 생산과 수요의 꾸준한 증가 추세와 전자 제품의 짧은 순환주기를 고려하였을 때 향후 폐디스플레이의 발생량은 급증할 것으로 예측 되며, 2020년에 약 75만 t이 발생할 것으로 예상되고 있다. 하지만, 국내 폐디스플레이 재활용 기술은 선진국에 비해 매우 미비하며, 대부분 수작업을 통해 금속류만 회수하여 재활용 하고 있는 실정이다. 특히, 제조사에 따라 디스플레이의 부품 구성 및 설계가 다양하여 해체・분리에 가장 많은 시간이 소비되며, 이는 작업 효율 감소 문제로 이어지게 된다. 본 연구에서는 폐디스플레이 재활용 공정효율 향상을 위한 체계적인 폐디스플레이 해체・분리 시스템을 구축하고자 하였으며, 개발 시스템은 오토 로딩 시스템, 스마트 비전 인식 시스템, 폐디스플레이 해체・분리 시스템, CCFL 자동무인화 처리 시스템으로 구성된다. 오토 로딩 시스템의 경우 기존 수작업에 의존하던 폐디스플레이 적재작업을 자동화함으로써 작업자의 작업 환경을 개선함과 동시에 공정의 효율을 증대 시키는 효과를 얻을 수 있다. 스마트 비전 인식 시스템의 경우 작업자의 경험에 의존한 다양한 폐디스플레이의 해체・분리 공정을 개선하기 위해 도입하였으며, 작업자에게 페디스플레이가 공급되기 전 자동으로 폐디스플레이의 정보를 확인하고 작업자에게 해체작업 정보를 제공함으로써 작업자의 경험차이에서 발생되는 문제를 해결하고자 하였다. 또한, 기존에 한명의 작업자가 하나의 폐디스플레이 전체를 해체・분리하는 방식을 다수의 작업대를 설계하여 세분화 및 단순화 하였으며, 작업자 간의 폐디스플레의 이송이 원활하도록 병렬구조 이송 라인 설계 등 작업 효율 증대를 위한 해체・분리 작업 시스템을 개발 하였다. 마지막으로 기존 수작업 공정에서 작업자에게 수은과 같은 유해물질을 직접적으로 노출시키는 CCFL 처리 공정은 무인 자동화함으로써 수은으로 인한 문제를 해결하였다. 이렇게 개발된 시스템은 기존에 수작업만을 사용했던 공정에 자동화 시스템을 적용함으로써 작업 효율 증대, 작업 환경 개선 등의 효과를 기대할 수 있을 것이다.
갈륨은 뛰어난 특성을 가지는 반도체 재료지만, 정광이 거의 존재하지 않는 희소원소이며, 주로 알루미늄이나 아연 제련 등의 부산물로서 얻을 수 있고, 주로 화합물 반도체(compound semiconductor)에 사용되고 있다. 화합물 반도체는 갈륨비소(gallium arsenide, GaAs), 갈륨인(GaP) 등이 있으며, 발광 다이오드(light emitting diode, LED), IC 등에 이용되고 있다. 이러한 화합물 반도체(GaAs, GaP 등)를 습식으로 분리, 농축하는 일반적인 방법으로는 이온교환법(ion exchange method), 용매추출법(solvent extraction method), 산-중화법 등이 있다. 이온교환법은 갈륨을 포함한 용액을 적정한 pH의 영역에서 킬레이트 이온교환 수지를 사용하여 흡착한 후, 탈기하여 갈륨 수용액으로 회수한 후, 전해채취를 통하여 갈륨을 회수하는 방법이며, 용매추출법은 유기용매에 카르본산계 또는 인산계 킬레이트 추출제를 포함한 유기상을 사용하여 수용액의 pH를 조정한 후, 갈륨을 선택적으로 추출하여 분리․농축한 후, 전해채취를 통하여 갈륨을 회수하는 방법이다. 산-중화법은 강산으로 침출해 중화를 거친 후, 알칼리 용해하여 비소와 인을 동시에 석출시키는 정액에 의해서 농축 분리하고 알칼리 용액으로 갈륨을 재용해하여 전해채취를 통해 갈륨을 회수하는 방법이다. 이온교환법과 용매추출법은 고비용과 작업의 안정성 및 환경오염 측면에서 문제점이 있으며, 산-중화법은 산과 알칼리가 다량 소비되는 단점이 있다. 따라서, 본 연구에서는 GaAs를 알칼리 용액에 산화제를 투입하여 고액농도(pulp density)에 따라 갈륨과 비소를 용해한 후, 알칼리 용해액에 알칼리 토금속 화합물(alkaline earth metals)을 첨가하고, 고액분리하여 갈륨을 용해한 용액과 비소와 알칼리 토금속의 화합물의 고체를 분리하였다. 분리된 갈륨용액은 전해채취를 통하여 갈륨으로 석출시켜 회수하는 습식제련 공정 연구를 수행하였다.
액정 디스플레이는 가벼운 무게, 작은 부피, 낮은 비용, 낮은 전력 소비 등의 이유로 PC 모니터, 노트북, 태블릿 등 광범위한 분야에서 사용되며 원료 사용량이 증가하게 되었다. 우수한 광전자 특성으로 인하여 액정 디스플레이에서 투명 전도 산화물 박막으로 indium-tin-oxide(ITO)가 사용된다. ITO는 90 wt%의 In2O3와 10 wt%의 SnO2로 이루어져 있으며 전세계 인듐 소비량의 84%는 액정 디스플레이 제조시 ITO를 형성하는데 사용된다. 일반적으로 3-8년인 액정 디스플레이의 수명을 고려하면, LCD의 폐기물은 재활용을 통하여 인듐을 생산 할 수 있는 잠재적인 대체 자원이다. 액정 디스플레이 재활용을 통하여 소각 또는 매립되는 폐기물로 인한 환경오염을 방지 할 수 있으며 또한 폐기물 내 인듐과 같은 유가금속을 재활용 하여 부가가치를 창출 할 수 있어 폐 액정디스플레이 재활용은 도시 광산 분야의 중요한 연구의 분야이다. 본 연구기관에서는 수명이 다한 사용 후 LCD TV를 해체/분리하여 액정패널, 인쇄회로기판, 냉음극관, 플라스틱케이스, 금속류 등으로 분해 하는 공정을 개발하였다. 해체/분리 공정을 통해 분리된 액정패널은 기계적으로 파쇄를 하여 유리 입자사이즈를 작게 하여 이 후 금속 회수를 용이하게 하였다. 본 연구에서는 파쇄 된 액정 디스플레이 유리에서 인듐을 회수하기 위하여 산을 이용하여 용출을 하였다. 가능한 용출 변수를 실험을 통하여 최적화 하였다. 액정 디스플레이에 인듐 함유량이 매우 낮아 특별히 고안된 방법을 이용하여 침출 용액을 농축하였으며 최적의 조건에서 인듐이 완전히 용출되는 것을 확인 할 수 있었다. 또한, 인듐 외 다른 금속에 대한 용출을 최소화 하였다.
파우더 파운데이션은 사용이 간편하고 수정화장이 용이하여 고객들이 많이 사용하고 있으며, 파우더 파운데이션을 만드는 방법은 건식방식, 소성방식, 그리고 습식방법으로 크게 분류할 수가 있다. 이중 습식방법은 이미 잘 알려진 바와 같이 back injection 방법과 front injection 방법이 있으며, 본 논문에서는 front injection 방법을 사용해 실험을 진행하였다. 실험결과 용매의 종류에 따른 경도 변화를 살펴보면 휘발성 실리콘이나 탄화수소계 휘발성 물질을 이용할 때 보다 정제수를 이용할 때 경도가 높게 나타났으며, 사용감 측면에서는 물보다는 탄화수소계 휘발성 물질과 휘발성 실리콘 등을 사용했을 때, 고객 선호도가 높게 나타났다. 또한 코팅물질 변화에 따른 경도 변화로는 아미노산계 코팅물질을 사용하였을 대 경도가 상승하는 효과를 나타냈으며, 실리콘 코팅 물질을 사용했을 때 경도 상승효과가 미비한 것으로 나타났다. 이러한 결과를 토대로 각 대상 고객에 맞는 처방을 개발하고자 할 때 사용감과 경도의 상관관계를 알고, 처방설계에 이용한다면 고객이 원하는 사용감에 한발 더 접근할 수 있으리라 생각된다.