• Journal of Conservation Science
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• v.36 no.3
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• pp.162-177
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• 2020

Research was conducted to characterize the copper production and smelting process with 11 copper smelting by-products (copper slag and copper crucible) excavated from the NA and LA areas at the Gwanbuk-ri archeological site in Buyeo. Scanning electron microscopy-energy dispersive spectroscopy, wavelength dispersive X-ray fluorescence, X-ray diffraction, and Raman microspectroscopy were employed in the analysis. The research results reveal that the copper slag from Gwanbuk-ri contained silicate oxide, magnetite, fayalite, and delafossite, which are typical characteristics of crucible slag and refined slag. The outward appearance and microstructure of the slag were grouped as follows: 1. glassy matrix + Cu prill, 2. glassy matrix + Cu prill + magnetite, 3. silicate mineral matrix + Cu prill, 4. crystalline (delafossite and magnetite) + amorphous (Cu prill), 5. magnetite + fayalite, and 6. slag from slag. The copper slags from Guanbuk-ri were found to contain residues of impurities such as SiO₂, Al₂O₃, CaO, SO₄, P₂O₅, Ag₂O, and Sb₂O₃ in their microstructure, and, in some cases, it was confirmed that copper, tin and lead are alloys. These results indicate that refining of intermediate copper(including impurities) and refining of alloys of copper(including impurities) - tin and refining of copper(including impurities) - tin - lead took place during the copper production process at Gwanbuk-ri, Buyeo.

• 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.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.08a
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• pp.351-352
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• 2011

그래핀(Graphene)은 2차원 평면구조의 $sp^2$ 탄소 결합으로 이루어진 물질이다. 일반적으로 그래핀은 탄소 원자 한층 정도의 얇은 두께를 가지면서 강철의 100배 이상 높은 강도, 다이아몬드보다 2배 이상 뛰어난 열 전도성, 그리고 규소보다 100배 이상 빠른 전자이동도 등의 매우 우수한 특성을 지닌다. 그래핀을 합성하거나 얻는 방법에는, 기계적 박리법(Micro mechanical exfoliation), 산화흑연(graphite oxide)을 이용한 reduced graphene oxide(RGO)방법과 탄화 규소(SiC)를 이용한 epitaxial growth 방법 등이 있지만, 대 면적화가 어렵거나 구조적 결함이 큰 문제점이 있다. 반면, 탄화수소(hydrocarbon)를 탄소 공급원으로 하는 열화학 기상 증착법(Thermal chemical vapor deposition, TCVD)은 구조적 결함이 상대적으로 적으면서 대 면적화가 가능하다는 이점 때문에 최근 가장 많이 이용되고 있는 방법이다. TCVD를 이용, 니켈, 몰리브덴, 금, 코발트 등의 금속에서 그래핀 합성연구가 보고되었지만, 대부분 수 층(fewlayer)의 그래핀이 합성되었다. 하지만, 구리 촉매를 이용하는 것이 단층 그래핀 합성에 매우 효율적이라는 연구결과가 보고되었다. 구리의 경우, 낮은 탄소융해도(solubility of carbon) 때문에 표면에서 self limiting 과정을 통하여 단층 그래핀이 합성된다. 그러나 단층 그래핀 일지라도 면저항(sheet resistance)이 매우 높고, 이론적 계산값에 비해 전자이동도(electron mobility)가 낮게 측정된다. 이러한 원인은 구조적 결함에서 기인된 것으로써 산업으로의 응용을 어렵게 만들기 때문에 양질의 단층 그래핀 합성연구는 필수적이다[1,2]. 본 연구에서는 TCVD를 이용하여 구리 포일(25 ${\mu}m$, Alfa Aeser) 위에 메탄가스를 탄소공급원으로 하여 수소를 함께 주입하고, 메탄가스의 양과 합성시간, 열처리 시간을 조절하면서 균일한 단층 그래핀을 합성하였다. 합성된 그래핀을 $SiO_2$ (300 nm)기판위에 전사(transfer)후 라만 분광법(raman spectroscopy)과 광학 현미경(optical microscope)을 통하여 분석하였다. 그 결과, 열처리 시간이 증가할수록 촉매로 사용된 구리 포일의 grain size가 커짐을 확인하였으며, 구리 포일 위에 합성된 그래핀의 grain size는, 구리 포일의 grain size에 의존하여 커짐을 확인하였다. 또한 동일한 grain 내의 그래핀은 균일한 층으로 합성되었다. 이는 기계적 박리법, RGO 방법, epitaxial growth 방법으로 얻은 그래핀과 비교하여 매우 뛰어난 결정성을 지님이 확인되었다. 본 연구를 통하여 면적이 넓으면서도 결정성이 매우 뛰어난 양질의 단층 그래핀 합성 방법을 확립하였다.

• Korean Chemical Engineering Research
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• v.46 no.6
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• pp.1095-1099
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• 2008

In this study, we investigated that hydrate formation and phase behavior of the $THF+H_2$ binary clathrate hydrates. In order to confirm the binary clathrate hydrate formation we employed the Raman and NMR spectroscopies that are known to be quite powerful tools, particularly for examining the cage occupancy pattern of guest molecules. In addition, we traced the P-T profiles from clathrate hydrate formation and dissociation process, which made it possible for the resulting phase equilibrium boundary to be clearly established. In the binary clathrate hydrate matrix we further identified that the relatively large THF molecules can only occupy the large $5^{12}6^4$ cavities, while the small $H_2$ molecules are entrapped in the empty $5^{12}$ cavities in structure-II, making the hydrate to be stable above 273 K even at relatively low pressure condition. Considering that pure $H_2$ hydrate can be produced at the extreme pressures higher that 1,000 bar, we can conclude that the water-soluble second guest inclusion induces $H_2$ storage and transportation to be readily achievable under much milder conditions.

• Clean Technology
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• v.26 no.2
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• pp.131-136
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• 2020

Biomass bamboo charcoal is utilized as anode for lithium-ion battery in an effort to find an alternative to conventional resources such as cokes and petroleum pitches. The amorphous phase of the bamboo charcoal is partially converted to graphite through a low temperature graphitization process with iron oxide nanoparticle catalyst impregnated into the bamboo charcoal. An optimum catalysis amount for the graphitization is determined based on the characterization results of TEM, Raman spectroscopy, and XRD. It is found that the graphitization occurs surrounding the surface of the catalysis, and large pores are formed after the removal of the catalysis. The formation of the large pores increases the pore volume and, as a result, reduces the surface area of the graphitized bamboo charcoal. The partial graphitization of the pristine bamboo charcoal improves the discharge capacity and coulombic efficiency compared to the pristine counterpart. However, the discharge capacity of the graphitized charcoal at elevated current density is decreased due to the reduced surface area. These results indicate that the size of the catalysis formed in in-situ graphitization is a critical parameter to determine the battery performance and thus should be tuned as small as one of the pristine charcoal to retain the surface area and eventually improve the discharge capacity at high current density.

• Korean Journal of Crystallography
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• v.13 no.3_4
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• pp.165-171
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• 2002

Single phase $Pb(Fe_{1/2}Ta_{1/2})O_3$, ceramics were successfully synthesized from the powders prepared by solid state reaction (sintering temperature: $1100^{\circ}C$, density: $9.3g/cm^3$, average grain size: $5.1{\pm}1.2mm$, space group: Pm3m). Their dielectric properties measured at $-150{\sim}50^{\circ}C$ showed the maximum relative dielectric constant of 31000 at $-41^{\circ}C$. 1 kHz, and typical relaxor ferroelectrics characteristics such as diffuse phase transition and dielectric relaxation phenomena. However, the diffuseness of phase transition decreased and the dielectric properties became more normal ferroelectrics as the time of annealing at $1000^{\circ}C$ increased. By using Raman spectroscopy, it was revealed that the $Fe^{3+}$ and $Ta^{5+}$ ions in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, are stoichiometrically 1 : 1 ordered within the short-range that can not be probed even by transmission electron microscopy, and this stoichiometric 1 : 1 ordering is enhanced by the annealing. The relaxor ferroelectric characteristics in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, could be correlated with the stoichiometric 1 : 1 short-range ordering of B-site cations, and the decrease of relaxor ferroelectric characteristics in the annealed $Pb(Fe_{1/2}Ta_{1/2})O_3$ could be correlated with the enhanced stoichiometric 1 : 1 short-range ordering of B-site cations.

• Restorative Dentistry and Endodontics
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• v.35 no.5
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• pp.321-334
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• 2010

Objectives: The purpose of this study is to evaluate bonding efficacy by means of measuring the effect of remained solvent on Degree of conversion(DC) and ${\mu}TBS$ and FE-SEM examination. Materials and Methods: Two 2-step total etching adhesives and two single-step self etching adhesives were used in this study. First, volume weight loss of 4 dentin adhesives were measured using weighting machine in process of time in normal conditions and calculate degree of evaporation (DE). Reaction/reference intensity ratio were measured using micro-Raman spectroscopy and calculate DC according to DE. Then 2 experimental groups were prepared according to air-drying methods (under, over) and control group was prepared to manufacturer's instruction. Total 12 groups were evaluated by means of micro tensile bond strength and FE-SEM examination. Results: Degree of evaporation (DE) was increased as time elapsed but different features were observed according to the kind of solvents. Acetone based adhesive showed higher DE than ethanol and butanol based adhesive. Degree of conversion (DC) was increased according to DE except for $S^3$ bond. In ${\mu}TBS$ evaluation, bond strength was increased by additional air-drying. Large gaps and droplets were observed in acetone based adhesives by FE-SEM pictures. Conclusions: Additional air-drying is recommended for single-step self etching adhesive but careful consideration is required for 2-step total etching adhesive because of oxygen inhibition layer. Evaporation method is carefully chose and applied according to the solvent type.

• Journal of the Institute of Electronics and Information Engineers
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• v.53 no.3
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• pp.124-131
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• 2016

Baseline correction is very important due to influence on performance of spectral analysis in application of spectroscopy. Baseline is often estimated by parameter selection using visual inspection on analyte spectrum. It is a highly subjective procedure and can be tedious work especially with a large number of data. For these reasons, it is an objective and automatic procedure is necessary to select optimal parameter value for baseline correction. Asymmetrically reweighted penalized least squares (arPLS) based on penalized least squares was proposed for baseline correction in our previous study. The method uses a new weighting scheme based on the generalized logistic function. In this study, we present an automatic selection of optimal parameter for baseline correction using arPLS. The method computes fitness and smoothness values of fitted baseline within available range of parameters and then selects optimal parameter when the sum of normalized fitness and smoothness gets minimum. According to the experimental results using simulated data with varying baselines, sloping, curved and doubly curved baseline, and real Raman spectra, we confirmed that the proposed method can be effectively applied to optimal parameter selection for baseline correction using arPLS.

• Journal of the Korea institute for structural maintenance and inspection
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• v.23 no.2
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• pp.130-134
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• 2019

In this paper, a laser-based non-contact load cell is newly developed for measuring forces in prestressed concrete tendons. First, alumina particles have been sprayed onto an empty load cell which has no strain gauges on it, and the layer has been used as a passive stress sensor. Then, the spectral shifts in fluorescence spectroscopy have been measured using a laser-based spectroscopic system under various force levels, and it has been found that the relation of applied force and spectral shift is linear in a lab-scale test. To validate the field applicability of the customized load cell, a full-scale prestressed concrete specimen has been constructed in a yard. During the field test, it was, however, found that the coating surface has irregular stress distribution. Therefore, the location of a probe has to be fixed onto the customized load cell for using the coating layer as a passive stress sensor. So, a prototype customized load cell has been manufactured, which consists of a probe mount on its casing. Then, by performing lab-scale uniaxial compression tests with the prototype load cell, a linear relation between compression stress and spectrum shift at a specific point where laser light had been illuminated has been detected. Thus, it has a high possibility to use the prototype load cell as a force sensor of prestressed concrete tendons.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.3
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• pp.103-111
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• 2021

Hexagonal shape Si crystals were grown by the mixed-source hydride vapor phase epitaxy (HVPE) method of mixing solid materials such as Si, Al and Ga. In the newly designed atmospheric pressure mixed-source HVPE method, nuclei are formed by the interaction between GaCl_n, AlCl_n and SiCl_n gases at a high temperature of 1200℃. In addition, it is designed to generate a precursor gas with a high partial pressure due to the rapid reaction of Si and HCl gas. The properties of hexagonal Si crystals were investigated through scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), high-resolution X-ray diffraction (HR-XRD), and Raman spectrum. From these results, it is expected to be applied as a new material in the Si industry.