• Applied Chemistry for Engineering
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• v.22 no.6
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• pp.685-690
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• 2011

In this study, a solvothermal reaction to prepare nanocrystalline titania was carried out using $TiCl_4$ and mixed solvents of alcohol and water. The effects of the type and the composition of alcohol on the crystal structure and agglomeration of final $TiO_2$ products were investigated. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscopy (SEM). In the solvothermal reaction using the n-butanol solutions with different volume ratios of n-butanol/water (100/0, 75/25, 50/50, 25/75, 0/100), the extent of agglomeration of obtained rutile $TiO_2$ was found to change with the volume ratio of n-butanol/water, and the n-butanol/water ratio of 75/25 revealed the best result for the preparation of well-dispersed nanocrystalline $TiO_2$ powders. The crystal phase of $TiO_2$ prepared through the solvothermal reaction changed with the type of alcohol in solvent (alcohol/water = 75/25). $TiO_2$ products obtained with the aqueous solutions of methanol, ethanol and isopropanol have an anatase phase, while that with n-butanol has a rutile phase. The results showed that, in the solvothermal reaction using both $TiCl_4$ as a starting material and the alcohol-water mixed solvents without any other additive, the enhancement of dispersion and control of crystal structure of $TiO_2$ products can be feasible by simply varying the composition and type of alcohol in the mixed solvents.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.239-240
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• 2008

As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.284-284
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• 2016

Topological insulator (TI) is a bulk-insulating material with topologically protected Dirac surface states in the band gap. In particular, $Bi_2Se_3$ attracted great attention as a model three-dimensional TI due to its simple electronic structure of the surface states in a relatively large band gap (~0.3 eV). However, experimental efforts using $Bi_2Se_3$ have been difficult due to the abundance of structural defects, which frequently results in the bulk conduction being dominant over the surface conduction in transport due to the bulk doping effects of the defect sites. One promising approach in avoiding this problem is to reduce the structural defects by heteroepitaxially grow $Bi_2Se_3$ on a substrate with a compatible lattice structure, while also preventing surface degradation by encapsulating the pristine interface between $Bi_2Se_3$ and the substrate in a clean growth environment. A particularly promising choice of substrate for the heteroepitaxial growth is hexagonal boron nitride (h-BN), which has the same two-dimensional (2D) van der Waals (vdW) layered structure and hexagonal lattice symmetry as $Bi_2Se_3$. Moreover, since h-BN is a dielectric insulator with a large bandgap energy of 5.97 eV and chemically inert surfaces, it is well suited as a substrate for high mobility electronic transport studies of vdW material systems. Here we report the heteroepitaxial growth and characterization of high quality topological insulator $Bi_2Se_3$ thin films prepared on h-BN layers. Especially, we used molecular beam epitaxy to achieve high quality TI thin films with extremely low defect concentrations and an ideal interface between the films and substrates. To optimize the morphology and microstructural quality of the films, a two-step growth was performed on h-BN layers transferred on transmission electron microscopy (TEM) compatible substrates. The resulting $Bi_2Se_3$ thin films were highly crystalline with atomically smooth terraces over a large area, and the $Bi_2Se_3$ and h-BN exhibited a clear heteroepitaxial relationship with an atomically abrupt and clean interface, as examined by high-resolution TEM. Magnetotransport characterizations revealed that this interface supports a high quality topological surface state devoid of bulk contribution, as evidenced by Hall, Shubnikov-de Haas, and weak anti-localization measurements. We believe that the experimental scheme demonstrated in this talk can serve as a promising method for the preparation of high quality TI thin films as well as many other heterostructures based on 2D vdW layered materials.

• Microbiology and Biotechnology Letters
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• v.48 no.2
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• pp.205-214
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• 2020

Cyanobacteria are microorganisms which have important roles in the nitrogen cycle due to their ability to fix nitrogen in water and soil ecosystems. They also produce valuable materials that may be used in various industries. However, some species of cyanobacteria may limit the use of water resources by causing harmful algal blooms in water ecosystems. Many culture collection depositories provide cyanobacterial strains for research, but their systematic preservation is not well-developed in Korea. In this study, we developed a method for the cryopreservation of the cyanobacteria Trichormus variabilis (syn. Anabaena variabilis), using alginate microcapsules. Two approaches were used for the experiments and their outputs were compared. One of the methods involved the cryopreservation of cells using only a cryoprotectant and the other used the cryoprotectant within microcapsules. After cryopreservation for 35 days, cells preserved with both methods were successfully regenerated from the initial 1.0 × 10⁵ cells/ml to a final concentration of 6.7 × 10⁶ cells/ml and 1.1 × 10⁷ cells/ml. Irregular T. variabilis shapes were found after 14 days of regeneration. T. variabilis internal structures were observed by transmission electron microscopy (TEM), revealing that lipid droplets were reduced after cryopreservation. The expression of the mreB gene, known to be related to cell morphology, was downregulated (54.7%) after cryopreservation. Cryopreservation using cryoprotectant alone or with microcapsules is expected to be applicable to other filamentous cyanobacteria in the future.

• Applied Microscopy
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• v.41 no.4
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• pp.277-284
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• 2011

This study was conducted to determine the antiseptic effect of stabilized chlorine dioxide (S-$ClO_2$) on muscle tissue of rats. Skeletal muscle of 8-week old Sprague-Dawley rats was used. Light and transmission electron microscopic findings were observed in the control group, which was not treated with stabilized chlorine dioxide, and in the experimental group, which was treated with a stabilized chlorine dioxide powder in aqueous solution. According to the LM and TEM observations, the day 1 control group showed the initiation of endomysium collapse resulting in an unclear boundary of muscle fibers, and partial collapse of the mitochondrial membranes. All endomysium had collapsed, and bacteria were observed among muscle fibers in the day 2 and later groups. Shapes of muscles were not distinguishable in day 3 or later groups. In contrast, the day 1 and 3 experimental groups revealed detailed structure of typical muscles, but partial collapse of the mitochondrial membranes was observed in the day 3 and later groups. Subsequently, connective tissues collapsed and structures in the shape of concentric circles were observed. In summary, the day 1 control group showed the initial collapse of tissues, and shapes were not distinguishable in the day 3 and later groups because most of the tissues had collapsed. In contrast, the day 3 experimental group showed partial collapse, but the overall shapes of muscles were maintained as time went on, confirming the antiseptic effect of stabilized chlorine dioxide on muscles.

• Journal of Korean Society of Environmental Engineers
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• v.34 no.5
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• pp.345-350
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• 2012

To investigate the exposure and health risk assessment for the residents near the D-asbestos mine in Chungbuk, Korea. We analyzed asbestos in the 20 ambient air and 23 activity based samples near the mine. The airborne sample results are showed that 8 of 20 samples ranged between 0.0025 to 0.0029 f/cc (fiber per cubic centimeter) and the others were below the detection limit by phase contrast microscopy (PCM). In addition, asbestos fibers were under the detection limit or not being by transmission electron microscopy (TEM). Based on interview and survey targeting the local residents, we made the activity based sampling (ABS) scenarios fit to the conditions of field. At the same time, we calculated the excess lifetime cancer risk (ELCR) of these ABS scenarios according to the ELCR average value and 95% upper confidence limit (UCL). At the case of weed whacking, soil digging and sweeping yard scenario, 95% UCL of ELCR exceeded the $1{\times}10^{-4}$, acceptable risk range for exposure. Based on our study results, it is necessary safety measures such as risk communication, abatement or management of naturally occurring asbestos (NOA).

• Journal of the Korean Magnetics Society
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• v.17 no.3
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• pp.120-123
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• 2007

The typical double-barrier magnetic tunnel junction (DMTJ) structure examined in this paper consists of a Ta 45/Ru 9.5/IrMn 10/CoFe7/$AlO_x$/free layer/AlO/CoFe 7/IrMn 10/Ru 60 (nm). The free layer consists of an $Ni_{16}Fe_{62}Si_8B_{14}$ 7 nm, $Co_{90}Fe_{10}$ (fcc) 7 nm, or CoFe $t_1$/NiFeSiB $t_2$/CoFe $t_1$ layer in which the thicknesses $t_1$ and $t_2$ are varied. The DMTJ with an NiFeSiB-free layer had a tunneling magnetoresistance (TMR) of 28%, an area-resistance product (RA) of $86\;k{\Omega}{\mu}m^2$, a coercivity ($H_c$) of 11 Oe, and an interlayer coupling field ($H_i$) of 20 Oe. To improve the TMR ratio and RA, a DMTJ comprising an amorphous NiFeSiB layer that could partially substitute for the CoFe free layer was investigated. This hybrid DMTJ had a TMR of 30%, an RA of $68\;k{\Omega}{\mu}m^2$, and a of 11 Oe, but an increased of 37 Oe. We confirmed by atomic force microscopy and transmission electron microscopy that increased as the thickness of NiFeSiB decreased. When the amorphous NiFeSiB layer was thick, it was effective in retarding the columnar growth which usually induces a wavy interface. However, if the NiFeSiB layer was thin, the roughness was increased and became large because of the magnetostatic $N{\acute{e}}el$ coupling.

• Journal of Life Science
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• v.19 no.6
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• pp.770-780
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• 2009

A new photosensitizer, 9-Hydroxypheophorbide-a (9-HpbD-a), was derived from Spirulina platensis. We conducted a series of experiments, in vitro and in vivo, to evaluate the anticancer effect and mechanism of photodynamic therapy using 9-HpbD-a and 660 nm diode lasers on a squamous carcinoma cell line. We studied the cytotoxic effects of pheophytin-a, 9-HpbD-a, 9-HpbD-a red and 660 nm diode lasers in a human head and neck cancer cell line (SNU-1041). Cell growth inhibition was determined by using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) reduction assay. The effects of 9-HpbD was higher than those of 9-HpbD-a red or pheophytin-a in PDT. We then tested the cytotoxic effects of 9-hydroxypheophorbide-a (9-HpbD-a) in vitro. The cultured SNU-I041 cells were treated with serial concentrations of 9-HpbD-a followed by various energy doses (0, 0.1, 0.5, 3.2 J/$cm^{2}$) and by various interval times (0, 3, 6, 9, 12 hr) until laser irradiation, then MTT assay was applied to measure the relative inhibitory effects of photodynamic therapy (PDT). Optimal laser irradiation time was 30 minutes and the cytotoxic effects according to incubation time after 9-HpbD-a treatment increased until 6 hours, after which it then showed no increase. To observe the cell death mechanism after PDT, SUN-I041 cells were stained by Hoechst 33342 and propidium iodide after PDT, and observed under transmission electron microscopy (TEM). The principal mechanism of PDT at a low dose of 9-HpbD-a was apoptosis, and at a high dose of 9-HpbD-a it was necrosis. PDT effects were also observed in a xenografted nude mouse model. Group I (no 9-HpbD-a, no laser irradiation) and Group II (9-HpbD-a injection only) showed no response (4/4, 100%), and Group III (laser irradiation only) showed recurrence (1/4,25%) or no response (3/4, 75 %). Group IV (9-HpbD-a + laser irradiation) showed complete response (10/16, 62.5%), recurrence (4/16, 25%) or no response (2/16, 12.5%). Group IV showed a significant remission rate compared to other groups (p<0.05). These results suggest that 9-HpbD-a is a promising photosensitizer for the future and that further studies on biodistribution, toxicity and mechanism of action would be needed to use 9-HpbD-a as a photosensitizer in the clinical setting.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.3
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• pp.115-120
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• 2016

$CeO_2$ is used as a co-catalyst with $TiO_2$ to improve the catalytic activity of $MnO_x$ and characterization of nano-sized powder is identified with de-NOx efficiency. A comparison between $MnO_x-CeO_2/TiO_2$ and single $CeO_2$ was conducted in terms of microstructural analysis to observe the behavior of $CeO_2$ in the ternary catalyst. The $MnO_x-CeO_2/TiO_2$ catalyst was synthesized by sol-gel method and the average particle size of the single $CeO_2$ is about $285{\mu}m$ due to the low thermal stability, whereas the particle size $MnO_x-CeO_2/TiO_2$ is about 130 nm. The strong interaction between Ce and Ti was identified through the EDS mapping by transmission electron microscopy (TEM). The improvement about 20 % of $de-NO_x$ efficiency is observed in the low-temperature ($150^{\circ}C{\sim}250^{\circ}C$) and vigorous oxygen exchange by well-dispersed $CeO_2$ is the reason of catalytic activity improvement.