The production of tin oxide ($SnO_2$) microrods on iridium (Ir)-coated substrates was achieved through the thermal evaporation of Sn powders in which a sufficiently high $O_2$ partial pressure was employed. Scanning electron microscopy revealed that the product consisted of microrods with diameters that ranged from 0.9 to $40\;{\mu}m$. X-ray diffraction, high-resolution transmission electron microscopy, and selected area electron diffraction indicated that the microrods were $SnO_2$ with a rutile structure. As the microrod tips were free of metal particles, it was determined that the growth of $SnO_2$ microrods via the present route was dominated by a vapor-solid mechanism. The thickening of rod-like structures was related to the utilization of sufficiently high $O_2$ partial pressure during the synthesis process, whereas low $O_2$ partial pressure facilitated the production of thin rods.
Cho, Youngji;Yang, Jun-Mo;Lam, Do Van;Lee, Seung-Mo;Kim, Jae-Hyun;Han, Kwan-Young;Chang, Jiho
Applied Microscopy
/
v.44
no.4
/
pp.133-137
/
2014
We suggest a facile transmission electron microscopy (TEM) specimen preparation method for the direct (polymer-free) transfer of layer-area graphene from Cu substrates to a TEM grid. The standard (polymer-based) method and direct transfer method were by TEM, high-resolution TEM, and energy dispersive X-ray spectroscopy (EDS). The folds and crystalline particles were formed in a graphene specimen by the standard method, while the graphene specimen by the direct method with a new etchant solution exhibited clean and full coverage of the graphene surface, which reduced several wet chemical steps and accompanying mechanical stresses and avoided formation of the oxide metal.
Seyedahmadian, Masoud;Houshyarazar, Shadi;Amirshaghaghi, Ahmad
Bulletin of the Korean Chemical Society
/
v.34
no.2
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pp.622-628
/
2013
Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.
Supported catalysts are at the heart of manufacturing essential chemical, agricultural and pharmaceutical products. While the longevity of such systems is critically hinged on the durability of metal nanoparticles, the conventional deposition/dispersion techniques are difficult to enhance the stability of the metal nanoparticles due to the lack of control over the interaction between metal-support. Regarding this matter, ex-solution has begun to be recognized as one of the most promising methodologies to develop thermally and chemically robust nanoparticles. By dissolving desired catalysts as a cation form into a parent oxide, fine and uniformly distributed metal nano-catalysts can be subsequently grown in situ under reductive heat treatment, which is referred to ex-solution. Over the several years, ex-solved analog has resulted in tremendous progress in the chemical-electrochemical applications due to the exceptional robustness coupled with ease synthesis. Herein, we describe the ex-solution process in detail which therein introducing the unique characteristics of ex-solved particles that distinguish them from conventionally dispersed nanoparticles. We then go through the history of science regarding the ex-solution phenomena and summarize several major research achievements which embrace the ex-solved nanoparticles to markedly promote the catalytic performances. In conclusion, we address the remaining challenges and the future perspectives of this rapidly growing field.
This study is the previous stage for the mass production technology development of the nano-sized tin oxide powder by the recycling of the wasted tin metal, and nano-sized tin oxide powder with the average particle size below 50 nm is prepared from the tin chloride solution by the spray pyrolysis process. As the reaction temperature increases from 800 to 850, the average particle size of the generated powder increases from 20 to 30 nm. As the reaction temperature increases to 900, the droplet type is composed of the particles with the average size of the 30 nm. while the average size of the independent particles increases up to $80{\sim}100$ nm and the surface microstructure becomes more solid. Until $900^{\circ}C$, as the reaction temperature increases, the XRD peak intensity increases, while the specific surface area decreases. When the reaction temperature increases to 950, most of the powder appears with the independent type and the average particle size decrease down to 70 nm. The XRD peak intensity greatly decreases and the specific surface area increases almost twice.
Proceedings of the Korean Vacuum Society Conference
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2012.02a
/
pp.100-101
/
2012
The plasma damage free and room temperature processedthin film deposition technology is essential for realization of various next generation organic microelectronic devices such as flexible AMOLED display, flexible OLED lighting, and organic photovoltaic cells because characteristics of fragile organic materials in the plasma process and low glass transition temperatures (Tg) of polymer substrate. In case of directly deposition of metal oxide thin films (including transparent conductive oxide (TCO) and amorphous oxide semiconductor (AOS)) on the organic layers, plasma damages against to the organic materials is fatal. This damage is believed to be originated mainly from high energy energetic particles during the sputtering process such as negative oxygen ions, reflected neutrals by reflection of plasma background gas at the target surface, sputtered atoms, bulk plasma ions, and secondary electrons. To solve this problem, we developed the NBAS (Neutral Beam Assisted Sputtering) process as a plasma damage free and room temperature processed sputtering technology. As a result, electro-optical properties of NBAS processed ITO thin film showed resistivity of $4.0{\times}10^{-4}{\Omega}{\cdot}m$ and high transmittance (>90% at 550 nm) with nano- crystalline structure at room temperature process. Furthermore, in the experiment result of directly deposition of TCO top anode on the inverted structure OLED cell, it is verified that NBAS TCO deposition process does not damages to the underlying organic layers. In case of deposition of transparent conductive oxide (TCO) thin film on the plastic polymer substrate, the room temperature processed sputtering coating of high quality TCO thin film is required. During the sputtering process with higher density plasma, the energetic particles contribute self supplying of activation & crystallization energy without any additional heating and post-annealing and forminga high quality TCO thin film. However, negative oxygen ions which generated from sputteringtarget surface by electron attachment are accelerated to high energy by induced cathode self-bias. Thus the high energy negative oxygen ions can lead to critical physical bombardment damages to forming oxide thin film and this effect does not recover in room temperature process without post thermal annealing. To salve the inherent limitation of plasma sputtering, we have been developed the Magnetic Field Shielded Sputtering (MFSS) process as the high quality oxide thin film deposition process at room temperature. The MFSS process is effectively eliminate or suppress the negative oxygen ions bombardment damage by the plasma limiter which composed permanent magnet array. As a result, electro-optical properties of MFSS processed ITO thin film (resistivity $3.9{\times}10^{-4}{\Omega}{\cdot}cm$, transmittance 95% at 550 nm) have approachedthose of a high temperature DC magnetron sputtering (DMS) ITO thin film were. Also, AOS (a-IGZO) TFTs fabricated by MFSS process without higher temperature post annealing showed very comparable electrical performance with those by DMS process with $400^{\circ}C$ post annealing. They are important to note that the bombardment of a negative oxygen ion which is accelerated by dc self-bias during rf sputtering could degrade the electrical performance of ITO electrodes and a-IGZO TFTs. Finally, we found that reduction of damage from the high energy negative oxygen ions bombardment drives improvement of crystalline structure in the ITO thin film and suppression of the sub-gab states in a-IGZO semiconductor thin film. For realization of organic flexible electronic devices based on plastic substrates, gas barrier coatings are required to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency flexible AMOLEDs needs an extremely low water vapor transition rate (WVTR) of $1{\times}10^{-6}gm^{-2}day^{-1}$. The key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required (under ${\sim}10^{-6}gm^{-2}day^{-1}$) is the suppression of nano-sized defect sites and gas diffusion pathways among the grain boundaries. For formation of high quality single inorganic gas barrier layer, we developed high density nano-structured Al2O3 single gas barrier layer usinga NBAS process. The NBAS process can continuously change crystalline structures from an amorphous phase to a nano- crystalline phase with various grain sizes in a single inorganic thin film. As a result, the water vapor transmission rates (WVTR) of the NBAS processed $Al_2O_3$ gas barrier film have improved order of magnitude compared with that of conventional $Al_2O_3$ layers made by the RF magnetron sputteringprocess under the same sputtering conditions; the WVTR of the NBAS processed $Al_2O_3$ gas barrier film was about $5{\times}10^{-6}g/m^2/day$ by just single layer.
Kim Cheol;Lim Jang-Seop;Jeon Young-Chan;Jeong Chang-Mo;Jeong Hee-Chan
The Journal of Korean Academy of Prosthodontics
/
v.43
no.5
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pp.599-610
/
2005
Purpose: The success of the bonding between electroformed gold and ceramic is dependent on the surface treatment of the pure gold coping. The purpose of this study was to evaluate the bonding strength between the electroformed gold and ceramic with varying surface treatment. Materials and methods: A total of 32 disks,8 were using conventional ceramometal alloy, 24 were using electroforming technique as recommended by manufacturer, were prepared. 24 electroformed disks were divided 3 groups according to surface treatment, i.e. 50 microns aluminium oxide sandblasting(GES-Sand), gold bonder treatment(GES-Bond) and $Rocatec^{TM}$ system(GES-Rocatec). For control group of conventional alloy 50 microns aluminium oxide treatment was done(V-Supragold). Energy dispersive x-ray analysis and scanning electron microscope image were observed. Using universal testing machine, shear bond strength and bonding failure mode at metal-porcelain interface were measured. Results and Conclusion: The following conclusions were drawn: 1. In the energy dispersive x-ray analysis, the Au was main component in electroformed gold(99.9wt%). After surface treatment, a little amount of $Al_2O_3(2.4wt%)$ were found in GES-Sand, and $SiO_2(4wt%)$ in GES-Bond. In GES-Rocatec, however, a large amount of $SiO_2(17.4wt%)$ were found. 2. In the scanning electron microscopy, similar pattern of surface irregu larities were observed in V-Supragold and GES-Sand. In GES-Bond, surface irregularities were increased and globular ceramic particles were observed. In GES-Rocatec, a large amount of silica particles attached to metal surface with increased surface irregularities were observed. 3. The mean shear bond strength values(MPa) in order were $22.9{\pm}3.7(V-Supragold),\;22.1{\pm}3.8(GES-Bond),\;20.1{\pm}2.8(GES-Rocatec)\;and\;13.0{\pm}1.4(GES-Sand)$. There was no significant difference between V-Supragold, GES-Bond, and GES-Rocatec. (P>0.05) 4. Most bonding failures modes were adhesive type in GES-Sand. However, in V-Supragold, GES-Bond and GES-Rocatec, cohesive and combination failures were commonly observed. From the result, with proper surface treatment method electroformed gold may have enough strength compare to conventional ceramometal alloy.
This paper presents analytical insights regarding into the occurrence of gold within organic matter, which is hosted by solid bitumen and closely associated with uranium ores in the Late Permian Kővágószőllős Sandstone Formation in Western Mecsek, South-West Hungary. The study utilizes a range of analytical techniques, including X-ray powder diffraction (XRPD) and wavelength dispersive X-ray fluorescence (WD-XRF) for comprehensive mineralogical and elemental analysis; organic petrography and electron microprobe analysis for characterizing organic matter; and an organic elemental analyzer for identifying organic compounds. A three-step sequential extraction method was used to liberate gold from organic matter and sulfide minerals, employing KOH, HCl, and aqua regia, followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) to quantify gold contents. The organic matter is identified as comprising two vitrinite types (telinite V1 and reworked V2) and three solid bitumen forms: nonfluorescing (B1) and fluorescing (B2) fillings within the V1, as well as homogenous pyrobitumen (PB) occupying narrow cracks and voids within globular quartz. Despite the samples exhibiting low total organic carbon content (<1 wt%), they display high sulfur content (up to 6 wt%) and the sequentially extracted noble metal content from the organic matter is found to total 7.45 ppm gold. The research findings suggest that organic matter plays crucial roles in ore mineralization processes. Organic matter acts as an active component in the migration of gold, uranium, and hydrocarbons within sulfur-rich hydrothermal fluids. Additionally, organic matter contributes to the entrapment and enrichment of gold in hetero-atomic organic fractions, forming metal-organic compounds. Moreover, uranium inclusions are observed as oxide/phosphate minerals within solid bitumen and associated vitrinite particles. These insights into the occurrence and distribution of gold within organic matter highlight substantial exploration potential, guiding additional research activities focused on organic matter within the Kővágószőllős Sandstone Formation at the Western Mecsek deposit.
A preparation process's conditions of aqueous sol which contains anatase-type nano titania particles with photocatalyic properties was established by using Yoldas process, so called, DCS(Destabilization of Colloidal Solution) process in this study. And crystal size change and phase transformation of titania particles in aqueous titania sol depending on reaction conditions was investigated by a light scattering method and XRD analysis of frozen dried powders, respectively. This sol with photo catalytic nano titania particles was used to the following hydrophilic hybrid coating film's fabrication and its properties was evaluated. Subsequently, for coating film using the above mentioned aqueous titania sol, non-aqueous titania sol was prepared without any chemical additives and its time stability according to aging time was investigate. By using the above mentioned aqueous titania sol and non-aqueous sol, a complex oxide coating sol for metal and ceramic substrate and a organic-inorganic hybrid coating sol for polymer substrate was prepared and it's hydrophilicity depending on UV irradiation conditions was evaluated. As a conclusions, the following results were obtained. (1)Aqueous titania sol The average particle size of titania in formed aqueous titania sol was distributed between 20$\sim$90nm range depending on reaction conditions. And the crystal phase of titania powders obtained by frozen drying method was changed from amorphous state to anatase and subsequently transformed to rutile crystal phase and it is attributed to concentration gradient in aqueous sol. (2)Non-aqueous titania sol Non-aqueous titania sol was prepared using methanol as a solvent and a little distilled water for hydrolysis and nitric acid as a catalyst were used. The obtained non-aqueous titania sol was stable at room temperature for 20 days. Additionally, non-aqueous titania sol with addition of chealating reagent such as acethylaceton and ethylene glycol prolonged the stability of sol by six months. (3)Complex sol and hybrid sol with super hydrophilicity The above mentioned aqueous titania sol as a main photocataylic component and non-aqueous titania sol as a binder for coating process was used to prepare a complex sol used for metal, ceramic and wood material substrate and also to prepare the organic-inorganic hybrid sol for polymer substrate such as polycarbonate and polyethylene, in which process APMS(3-Aminopropyltrimethoxysilane), GPTS(3-Glycidoxypropyl-trimethoxysilane) as a hydrophilic silane compound and HEMA(2-Hydroxyethyl methacrylate) as a forming network in hybrid coating film were used. The hybrid coating film such as prepared through this process showed a superhydrophilicity below 1$10^{\circ}$ depending on processing conditions and a pencil's hardness over 6 H.
Journal of the Korean Applied Science and Technology
/
v.34
no.1
/
pp.50-57
/
2017
Zinc oxide is, one of metal oxide semiconductor, harmless to human and environment-friendly. It has excellent chemical and thermal stability properties. Wurtzite-zinc oxide is a large band gap energy of 3.37 eV and high exciton binding energy of 60 meV. It can be applied to various fields, such as solar cells, degradation of the dye waste, the gas sensor. The photocatalytic activity of zinc oxide is varied according to the particle shape and change of crystallinity. Therefore, It is very important to specify the additives and the experimental variables. In this study, the zinc oxide were synthesized by using a microwave assisted hydrothermal synthesis. The precursor was used as the zinc nitrate, the pH value was controlled as 11 by NaOH. Surfactants are the ethanolamine, cetyltrimethylammonium bromide, sodium dodecyl sulfate, sorbitan monooleate was added by changing the concentration. The composite particles had the shape of a star-like, curcular cone, seed shape, flake-sphere. Physical and chemical properties of the obtained zinc oxide was characterized using x-ray diffractometer, field emission scanning electron microscopy, thermogravimetric analysis and optical properties was characterized using UV-visible spectroscopy, photoluminescence and raman spectroscopy.
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