In this study, anatase TiO2 nano sol (TNS, TiO2 Nano-Sol) was synthesized via a simple sol-gel method under low-temperature and ambient pressure conditions using TiOCl2 as a precursor. The structural and photocatalytic properties of the TNS were systematically investigated as a function of reaction time. X-ray diffraction (XRD) confirmed the formation of the anatase crystal structure as the reaction time increased, while field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) analyses verified the uniform formation of fine anatase nanoparticles, averaging less than 10 nm in size. The synthesized TNS sol enabled the fabrication of transparent TiO2 coatings that retained over 76 % transmittance in the visible light range, as verified by UV-Vis spectroscopy. Photocatalytic activity was evaluated through methylene blue (MB) degradation experiments, which showed that degradation efficiency was enhanced with longer reaction times. Notably, the TNS-48 exhibited superior photocatalytic degradation performance, being approximately three times higher than that of TNS-1 and about twice that of the commercial P25. This study demonstrates that the TNS sol synthesized through a simple sol-gel process can achieve high transparency and excellent photocatalytic properties without requiring hightemperature and high-pressure synthesis. It is expected to be applicable in various photocatalytic fields, such as functional coatings and electrode materials.
In the present work, we address the new route for the green synthesis of manganese dioxide (MnO2) by an innovative method named the solution plasma process (SPP). The reaction mechanism of both colloidal and nanostructured MnO2 was investigated. Firstly, colloidal MnO2 was synthesized by plasma discharging in KMnO4 aqueous solution without any additives such as reducing agents, acids, or base chemicals. As a function of the discharge time, the purple color solution of MnO4 - (oxidation state +7) was changed to the brown color of MnO2 (oxidation state +4) and then light yellow of Mn2+ (oxidation state +2). Based on the UV-vis analysis we found the optimal discharging time for the synthesis of stable colloidal MnO2 and also reaction mechanism was verified by optical emission spectroscopy (OES) analysis. Secondly, MnO2 nanoparticles were synthesized by SPP with a small amount of reducing sugar. The precipitation of brown color was observed after 8 min of plasma discharge and then completely separated into colorless solution and precipitation. It was confirmed layered type of nanoporous birnessite- MnO2 by X-ray powder diffraction (XRD), fourier-transform infrared spectroscopy (FT-IR), and electron microscopes. The most important merits of this approach are environmentally friendly process within a short time compared to the conventional method. Moreover, the morphology and the microstructure could be controllable by discharge conditions for the appropriate potential applications, such as secondary batteries, supercapacitors, adsorbents, and catalysts.
Recently, research on MAX phase materials has been actively conducted. M of MAX phase is made of early transition metal element, A is A-group (IIIA or IVA) element, and X is Carbon or Nitrogen. It has the chemical formula of MnAXn-1, and is called the 211, 312, and 413 groups according to the indices(n=1,2,3). MXene material is characterized by having a layered structure of 2D structure like graphene by etching the element corresponding to A-gruop in the MAX phase. So far, MXene materials have been reported to be applied in various fields. In particular, research is being actively conducted as anode material for Li secondary batteries, electromagnetic wave shielding material, and hydrogen storage alloy material. In the pulse energization active sintering method, the surface of the powder particles is cleaned and activated more easily than the conventional electrical sintering process and material transfers at both the macro and micro level, so that a high-quality sintered body can be obtained at low temperature and fast time. In this study, the MAX phase was synthesized in a short time by using a pulse current active sintering apparatus, and the MXene material was prepared from the synthesized MAX phase and the structure was analyzed.
Tungsten carbide is widely used in carbide tools. However, its production process generates a significant number of end-of-life products and by-products. Therefore, it is necessary to develop efficient recycling methods and investigate the remanufacturing of tungsten carbide using recycled materials. Herein, we have recovered 99.9% of the tungsten in cemented carbide hard scrap as tungsten oxide via an alkali leaching process. Subsequently, using the recovered tungsten oxide as a starting material, tungsten carbide has been produced by employing a self-propagating high-temperature synthesis (SHS) method. SHS is advantageous as it reduces the reaction time and is energy-efficient. Tungsten carbide with a carbon content of 6.18 wt % and a particle size of 116 nm has been successfully synthesized by optimizing the SHS process parameters, pulverization, and mixing. In this study, a series of processes for the highefficiency recycling and quality improvement of tungsten-based materials have been developed.
In this study, (GaN)1-x(ZnO)x solid solution nanoparticles with a high zinc content are prepared by ultrasonic spray pyrolysis and subsequent nitridation. The structure and morphology of the samples are investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The characterization results show a phase transition from the Zn and Ga-based oxides (ZnO or ZnGa2O4) to a (GaN)1-x (ZnO)x solid solution under an NH3 atmosphere. The effect of the precursor solution concentration and nitridation temperature on the final products are systematically investigated to obtain (GaN)1-x(ZnO)x nanoparticles with a high Zn concentration. It is confirmed that the powder synthesized from the solution in which the ratio of Zn and Ga was set to 0.8:0.2, as the initial precursor composition was composed of about 0.8-mole fraction of Zn, similar to the initially set one, through nitriding treatment at 700oC. Besides, the synthesized nanoparticles exhibited the typical XRD pattern of (GaN)1-x(ZnO)x, and a strong absorption of visible light with a bandgap energy of approximately 2.78 eV, confirming their potential use as a hydrogen production photocatalyst.
Continuous synthesis of high-crystalline carbon nanotubes (CNTs) is achieved by reconfiguring the injection part in the reactor that is used in the floating catalyst chemical vapor deposition (FC-CVD) process. The degree of gas mixing is divided into three cases by adjusting the configuration of the injection part: Case 1: most-delayed gas mixing (reference experiment), Case 2: earlier gas mixing than Case 1, Case 3: earliest gas mixing. The optimal synthesis condition is obtained using design of experiment (DOE) in the design of Case 1, and then is applied to the other cases to compare the synthesis results. In all cases, the experiments are performed by varying the timing of gas mixing while keeping the synthesis conditions constant. Production rate (Case 1: 0.63 mg/min, Case 2: 0.68 mg/min, Case 3: 1.29 mg/min) and carbon content (Case 1: 39.6 wt%, Case 2: 57.1 wt%, Case 3: 71.6 wt%) increase as the gas-mixing level increases. The amount of by-products decreases stepwise as the gas-mixing level increases. The IG/ID ratio increases by a factor of 7 from 10.3 (Case 1) to 71.7 (Case 3) as the gas-mixing level increases; a high ratio indicates high-crystalline CNTs. The radial breathing mode (RBM) peak of Raman spectrograph is the narrowest and sharpest in Case 3; this result suggests that the diameter of the synthesized CNTs is the most uniform in Case 3. This study demonstrates the importance of configuration of the injection part of the reactor for CNT synthesis using FC-CVD.
3 mol% yttria-doped stabilized zirconia (3YSZ) is synthesized by a solvothermal process, and its characteristics are investigated using various methods. Also, the dispersibility of synthesized 3YSZ nanoparticles is observed with the species of surface modifier. The 3YSZ nano sol prepared with an optimum condition is employed in prism coating and its properties are evaluated. The synthesized 3YSZ nanoparticles show a globular shape with about 10 to 20 nm crystallite size. The mixed phases with the nano sol show a high specific surface of 178 m2/g. The prism sheet coated with the 3YSZ nano sol present an excellent refractive index, transmittance, and luminance; refractive index is 1.603, transmittance is 90.2 %, and luminance of coating film is improved by 5.9 % compared to that of the film without 3YSZ nano sol. It is verified that the surface modified 3YSZ is suitable as the prism sheet for optical displays.
SiC is a material with excellent strength, heat resistance, and corrosion resistance. It is generally used as a material for SiC invertors, semiconductor susceptors, edge rings, MOCVD susceptors, and mechanical bearings. Recently, SiC single crystals for LED are expected to be a new market application. In addition, SiC is also used as a heating element applied directly to electrical energy. Research in this study has focused on the manufacture of heating elements that can raise the temperature in a short time by irradiating SiC-I2 with microwaves with polarization difference, instead of applying electric energy directly to increase the convenience and efficiency. In this experiment, Polydimethylsilane (PDMS) with 1,2 wt% of iodine is synthesized under high temperature and pressure using an autoclave. The synthesized Polycarbosilane (PCS) is heat treated in an argon gas atmosphere after curing process. The experimental results obtain resonance peaks using FT-IR and UV-Visible, and the crystal structure is measured by XRD. Also, the heat-generating characteristics are determined in the frequency band of 2.45 GHz after heat treatment in an air atmosphere furnace.
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 m2/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.
Porous Cu-14 wt% Co with aligned pores is produced by a freeze drying and sintering process. Unidirectional freezing of camphene slurry with CuO-Co3O4 powders is conducted, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The dried bodies are hydrogen-reduced at 500oC and sintered at 800oC for 1 h. The reduction behavior of the CuO-Co3O4 powder mixture is analyzed using a temperature-programmed reduction method in an Ar-10% H2 atmosphere. The sintered bodies show large and aligned parallel pores in the camphene growth direction. In addition, small pores are distributed around the internal walls of the large pores. The size and fraction of the pores decrease as the amount of solid powder added to the slurry increases. The change in pore characteristics according to the amount of the mixed powder is interpreted to be due to the rearrangement and accumulation behavior of the solid particles in the freezing process of the slurry.
정삼투 공정에 유용한 유도용질로서 diethyl malonate를 사용한 citrate 계열의 유기 화합물을 합성하였다. 최종적으로 얻은 potassium pentane-1,3,3,5-tetracarboxylate는 1H-NMR과 13C-NMR을 통하여 확인하였다. 유도용질의 물성을 확인 하기 위해 삼투압, 용해도, 수투과도, 역염 투과도를 측정하였다. 합성한 유도용액을 사용하여 정삼투 공정을 진행한 결과, 동일한 citrate 계열인 trisodium citrate 및 tripotassium citrate보다 높은 수투과량을 나타내었으며 염의 역확산 정도는 NaCl에 비하여 매우 낮은 값을 나타내었다. 합성된 유도용질의 삼투압은 NaCl보다 약 25% 낮았으나 물에 대한 용해도는 NaCl의 8.8 배인 317 g/100 g water의 값을 나타내었다. 정삼투 종료 후 유도용질의 회수를 위해 상용화된 나노여과막을 사용하였고, 낮은 압력에서 효율적으로 회수가 가능하였다.
Current synthesis processes for titanium dioxide (TiO2) nanoparticles require expensive precursors or templates as well as complex steps and long reaction times. In addition, these processes produce highly agglomerated nanoparticles. In this study, we demonstrate a simple and continuous approach to synthesize TiO2 nanoparticles by a salt-assisted ultrasonic spray pyrolysis method. We also investigate the effect of salt content in a precursor solution on the morphology and size of synthesized products. The synthesized TiO2 nanoparticles are systematically characterized by X-ray diffraction, transmission electron micrograph, and UV-Vis spectroscopy. These nanoparticles appear to have a single anatase phase and a uniform particle-size distribution with an average particle size of approximately 10 nm. By extrapolating the plots of the transformed Kubelka-Munk function versus the absorbed light energy, we determine that the energy band gap of the synthesized TiO2 nanoparticles is 3.25 eV
This paper examines a simple one-step and catalyst-free method for synthesizing carbon nanoparticles from aliphatic alcohols and n-hexane with linear molecule formations by using a stable solution plasma process with a bipolar pulse and an external resistor. When the external resistor is adopted, it is observed that the current spikes are dramatically decreased, which induced production of a more stable discharge. Six aliphatic linear alcohols (methanol- hexanol) containing carbon with oxygen sources are studied as possible precursors for the massive production of carbon nanoparticles. Additional study is also carried out with the use of n-hexane containing many carbons without an oxygen source in order to enhance the formation of carbon nanoparticles and to eliminate unwanted oxygen effects. The obtained carbon nanoparticles are characterized with field emission-scanning electron microscopy, energy dispersive X-ray spectroscopy, and Raman spectroscopy. The results show that with increasing carbon ratios in alcohol content, the synthesis rate of carbon nanoparticles is increased, whereas the size of the carbon nanoparticles is decreased. Moreover, the degree of graphitization of the carbon nanoparticles synthesized from 1-hexanol and n-hexane with a high carbon (C)/oxygen (O) ratio and low or no oxygen is observed to be greater than that of the carbon nanoparticles synthesized from the corresponding materials with a low C/O ratio.
Despite numerous advances in the preparation and use of GaN, and many leading-edge applications in lighting technologies, the preparation of high-quality GaN powder remains a challenge. Ammonolytic preparations of polycrystalline GaN have been studied using various precursors, but all were time-consuming and required high temperatures. In this study, an efficient and low-temperature method to synthesize high-purity hexagonal GaN powder is developed using sub-micron Ga2O3 powder as a starting material. The sub-micron Ga2O3 powder was prepared by an ultrasonic spray pyrolysis process. The GaN powder is synthesized from the sub-micron Ga2O3 powder through a nitridation treatment in an NH3 flow at 800℃. The characteristics of the synthesized powder are systematically examined by X-ray diffraction, scanning and transmission electron microscopy, and UV-vis spectrophotometer.
정삼투 공정에 유용한 유도용질로서 n-nitrilotris(methylene) phosphonic acid (NTPA) 염을 합성하였다. NTPA에 첨가하는 KOH의 함량을 변화시켜 NTPA-4K, NTPA-5K, NTPA-6K 세 종류의 유도용질을 합성하고 1H-NMR, 13C-NMR을 통하여 확인하였다. 유도용질의 물성을 확인하기 위해 삼투압, 점도, 수투과도, 역염 투과도를 측정하였다. 정삼투 공정에서는 증류수를 유입용액으로 사용하고 0.5 M의 유도용액으로 실험한 결과 각각 수투과도는 35.8, 38.8, 42.2 LMH를 나타내고 5.4, 6.9, 7.4 gMH의 역염 투과도를 나타내었다. 이는 기존의 NaCl 유도용액보다 높은 수투과도와 훨씬 낮은 역염 투과도를 확인 하였다. 정삼투 공정 후 묽어진 유도용질의 회수를 위해 나노여과 방식으로 상용막을 사용하여 제거율을 측정한 결과 90% 이상의 높은 성능을 확인하였다.
Using a high pressure homonizer, we report on the electrochemical performance of Li4Ti5O12(LTO) particles manufactured as anode active material for lithium ion battery. High-pressure synthesis processing is performed under conditions in which the mole fraction of Li/Ti is 0.9, the synthesis pressure is 2,000 bar and the numbers of passings-through are 5, 7 and 10. The observed X-ray diffraction patterns show that pure LTO is manufactured when the number of passings-through is 10. It is found from scanning electron microscopy analysis that the average size of synthesized particles decreases as the number of passings-through increases. LiCoO2-based active cathode materials are used to fabricate several coin half/full cells and their battery characteristics such as lifetime, rate capability and charge transfer resistance are then estimated, revealing quite good electrochemical performance of the LTO particles as an effective anode active material for lithium secondary batteries.
Boron nitride nanotubes (BNNTs) are receiving great attention because of their unusual material properties, such as high thermal conductivity, mechanical strength, and electrical resistance. However, high-throughput and highefficiency synthesis of BNNTs has been hindered due to the high boiling point of boron (~ 4000℃) and weak interaction between boron and nitrogen. Although, hydrogen-catalyzed plasma synthesis has shown potential for scalable synthesis of BNNTs, the direct use of H2 gas as a precursor material is not strongly recommended, as it is extremely flammable. In the present study, BNNTs have been synthesized using radio-frequency inductively coupled thermal plasma (RF-ITP) catalyzed by solid-state ammonium chloride (NH4Cl), a safe catalyst materials for BNNT synthesis. Similar to BNNTs synthesized from h-BN (hexagonal boron nitride) + H2, successful fabrication of BNNTs synthesized from h-BN+NH4Cl is confirmed by their sheet-like properties, FE-SEM images, and XRD analysis. In addition, improved dispersion properties in aqueous solution are found in BNNTs synthesized from h-BN +NH4Cl.
Alane(aluminum trihydride, AlH3)으로 명명되는 고에너지 물질인 삼수소알루미늄은 수소저장 물질로서 뿐만 아니라 우주항공분야의 고체 추진제나 방위산업의 화약제조용으로도 사용될 수 있다. 본 연구는 습식공정을 통하여 합성하고, 에테르를 세밀하게 분리하는 결정화 공정을 통하여 최종 수소화물을 추출하였다. 결정화 공정에서 삼수소알루미늄-에테레이트(AlH3·(C2H5)2O)가 alane으로 상변이하면서 입자가 성장하고, 85℃에서 2 시간의 결정화 시간이 이루어졌을 때 가장 안정된 결정상이 나타나는 모습을 확인하였다. 최종적으로 추출된 고체상 삼수소알루미늄은 막대모양의 γ-형태가 가장 많은 양을 차지하는 것으로 나타났으며, 크기는 50-100 μm 수준이었다
Cost-effective functional phosphor nanoparticles are prepared by introducing low-cost SiO2 spheres to rareearth phosphor (YVO4:Eu3+, YVO4:Er3+, and YVO4:Nd3+) shells using a sol-gel synthetic method. These functional nanoparticles are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy, and general photoluminescence spectra. The SiO2 sphere occupying the interior of the conventional phosphor is advantageous in significantly reducing the cost of expensive rare-earth phosphor nanoparticles. The sol-gel process facilitates the core–shell structure formation; the rare-earth shell phosphor has strong interactions with chelating agents on the surfaces of SiO2 nanoparticles and thus forms layers of several nanometers in thickness. The photoluminescence wavelength is simply tuned by replacing the active materials of Eu3+, Er3+, and Nd3+. Moreover, the photoluminescent properties of the core–shell nanoparticles can be optimized by manipulating the specific contents of active materials in the phosphors. Our simple approach substitutes low-cost SiO2 for expensive rare-earth-based phosphor materials to realize cost-effective phosphor nanoparticles for various applications.