• Journal of the Korean Ceramic Society
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• v.40 no.12
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• pp.1202-1207
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• 2003

Using a recently developed Hybric Plasma-Particle Accelerating Impact Deposition (HP-PAID) process, synthesis of nanostructured silicon coatings has been investigated by injecting vapor-phase TEOS (tetraethosysilane, (C$_2$H$\_$5/O)$_4$Si) into an Ar hybrid plasma. The plasma jet with reactants was expanded through nozzle into a deposition chamber, with the pressure dropping from 700 to 10 torr. Ultrafine particles accelerated in the free jet downstream of the nozzle, deposited by an inertial impaction onto a temperature controlled substrate. By using this process, nanostructured amorphous silicon coatings with grain size smaller than 10 nm could be synthesized. These samples were annealed in an Ar and crystallized at 900$^{\circ}C$ for 30 min. TEM analysis showed that the annealed coatings were also composed of nanoparticles smaller than 10 nm, which showed a good consistency that the average grain size of 7 nm was also estimated from a peak shift of 2.39 cm$\^$-1/ and Full Width at Half Maximum (FWHM) 5.92 cm$\^$-1/ of Raman analysis. The noteworthy is that a strong PL peak at 398 nm was also obtained for this sample, which indicates that the deposited coatings also contained 3∼4 nm nanostructured grains.

• Korean Journal of Materials Research
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• v.8 no.9
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• pp.813-818
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• 1998

Ultrafine powders of $\textrm{In}_{2}\textrm{O}_{3}$-doped $\textrm{SnO}_{2}$ were synthesized by a coprecipitation method and the effects of pH value and the amount of In2Q addition on particle size were investigated. The influence of pH value on particle size could be negligible, whereas the amount of $\textrm{In}_{2}\textrm{O}_{3}$ has influenced on particle size and specific surface area. The gas sensitivity to hydrocarbOn($\textrm{C}_{3}\textrm{H}_{8}$, $\textrm{C}_{4}\textrm{H}_{10}$) increased with $\textrm{In}_{2}\textrm{O}_{3}$ addition and reached a maximum at 3wt.% addition. From the results of impedance analysis and I-V characteristics. it was showed that the agglomeration structure of particles and the boundaries between agglomerates were the important factors to determine the gas sensing mechanism.

• Korean Journal of Materials Research
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• v.4 no.3
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• pp.319-328
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• 1994

Aluminium and titanium precursors containing $\beta$-diketonate ligands were used for the synthesis of polymeric sols of alumina and titania by sol-gel methods. To prepare polymeric sols by solgel processing, we synthesized modified precursors having chelating organic ligands. With these precursors it was found to be possible to control both hydrolysis and polycondensation reaction rates which resulted in ultrafine particles few nms of average size. The optimum molar ratio of acid to alkoxide for alumina sol was 0.3-0.4 and that of water to alkoxide &as 1. On the other hand, the corresponding ratios for titania sol were found be 0.25-0.20 and 1 respectively. Dynamic light scattering measurements indicated that the average particle size in both sols was in the order of few nms. SEM photographs were taken to observe crack-free and smooth surfaces of coated membranes after sintering at $450^{\circ}C$. Alumina coated membrane on a slide glass had about 4-4.5$\mu \textrm{m}$, thickness and titania coated one had 2-2.5$\mu \textrm{m}$, thickness. And according to TEM photographs, the grain size of titania was smaller than 30nm and that of alumina was in the range of few $\AA$s to 2nms. An X-ray diffraction study revealed that alumina was $\gamma$ phase and titania was anatase crystal.

• Analytical Science and Technology
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• v.32 no.6
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• pp.243-251
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• 2019

Microplastics (MP) are found in large quantities in the oceans, posing a major threat to the ecosystem. In Korea, MPs have been reported to be detected in sea salts. In order to analyze MPs, information on their composition, size, and shape is required. FT-IR microscopy is used frequently to measure sizes larger than 20 ㎛. Recently, however, Raman microscopy, which can analyze ultrafine plastics below 20 ㎛, has been applied extensively. In this study, 10.0 g samples of commercially available salts were dissolved and filtered through a 45 ㎛ mesh filter with a size of 25.4 mm × 25.4 mm. These filtered samples were then analyzed by both FT-IR microscopy and Raman microscopy. A total of four MPs, including three polyethylene (PE) of size 70-100 ㎛ and a polypropylene (PP) of size 170 ㎛, were detected by FT-IR microscopy, while 10 MPs, including nine PE of size 10-120 ㎛ and one polystyrene (PS) of size 40 ㎛, were detected by Raman microscopy. Approximately, 1,000 MPs/kg was estimated, which was almost two times higher than the previous reported levels (~550-681 particles/kg in sea salts); this is because Raman microscopy can detect much smaller MPs than FT-IR microscopy. A total of 113 particles were found using Raman microscopy: Carbon (35, 31.5 %), minerals (28, 25 %), and glass (16, 14.4 %) were dominant, forming around 70% of the total, but MPs (10, 8.8 %) and cellulose (5, 4.5 %) were also found. Raman microscopy has great potential as an accurate method for measuring MPs, as it can measure smaller size MPs than FT-IR microscopy. It also has a reduced sample preparation time.

• Korean Journal of Mineralogy and Petrology
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• v.34 no.1
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• pp.31-40
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• 2021

The hydrogen in nominally anhydrous mineral is known to be associated with lattice defects, but it also can exist in the form of water and hydroxyl groups on the large surface of the nanoscale particles. In this study, we investigate the effectiveness of 1H solid-state nuclear magnetic resonance (NMR) spectroscopy as a robust experimental method to quantify the hydrogen atomic environments of amorphous silica nanoparticles with varying relative humidity. Amorphous silica nanoparticles were packed into NMR rotors in a temperature-humidity controlled glove box, then stored in different atmospheric conditions with 25% and 70% relative humidity for 2~10 days until 1H NMR experiments, and a slight difference was observed in 1H NMR spectra. These results indicate that amount of hydrous species in the sample packed in the NMR rotor is rarely changed by the external atmosphere. The amount of hydrogen atom, especially the amount of physisorbed water may vary in the range of ~10% due to the temporal and spatial inhomogeneity of relative humidity in the glove box. The quantitative analysis of 1H NMR spectra shows that the amount of hydrogen atom in amorphous silica nanoparticles linearly increases as the relative humidity increases. These results imply that the sample sealing capability of the NMR rotor is sufficient to preserve the hydrous environments of samples, and is suitable for the quantitative measurement of water content of ultrafine nominally anhydrous minerals depending on the atmospheric relative humidity. We expect that 1H solid-state NMR method is suitable to investigate systematically the effect of surface area and crystallinity on the water content of diverse nano-sized nominally anhydrous minerals with varying relative humidity.