• Economic and Environmental Geology
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• v.37 no.3
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• pp.303-309
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• 2004

Pyrochlores were known as promising materials for the immobilization of radioactive actinide. Accordingly, we synthesized pyrochlores with Gd$_2$Ti$_2$$O_7$ and Gd$_2$Zr$_2$$O_7$compositions by sintering method, and studied its properties and phase relations in Gd-Ti-O and Gd-Zr-O system. The mixed powders were pressed into pellets under 200-400 kgf/cm$^2$ at room temperature. and then sintered at 1000-1$600^{\circ}C$ for 0.5-40 hours. The synthesized samples were analyzed and were identified with XRD and SEM/EDS analyses. The optimal synthetic conditions of pyrochlores with Gd$_2$Ti$_2$$O_7$composition were at 140$0^{\circ}C$/0.5hrs, 130$0^{\circ}C$/3hrs and 120$0^{\circ}C$/20hrs. Its chemical composition was $Gd_{2.0-2.1}$$Ti_{1.9-2.0}$$O_7$ and similar to the stoichiometric composition without any relationship in temperature and atmosphere. The optimal synthetic conditions of pyrochlores with $Gd_{2}$$Zr_{2}$$O_7$composition were at 155$0^{\circ}C$/40hrs and 1$600^{\circ}C$/30hrs. The compositions of pyrochlore synthesized from these optimal conditions were irregular with $Gd_{1.5-2.4}$$Zr_{1.7-2.4}$$O_7$. Such heterogeneity indicates that the reaction rate of pyrochlore with Gd$_2$Zr$_2$$O_7$composition is very low, and then its equilibrium state could not be attained even for 40 hours which was the longest sintering time in this research.

• Economic and Environmental Geology
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• v.49 no.1
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• pp.13-22
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• 2016

The objectives of this study were to recover silica and iron oxides and $CO_2$ sequestration using serpentine via various acid dissolution and pH swing processes. Serpentine collected from Guhang-myeon in S. Korea were mainly composed of antigorite and magnetite consisting of $SiO_2$ (45.3 wt.%), MgO (41.3 wt.%), $Fe_2O_3$ (12.2 wt.%). Serpentine pulverized ($${\leq_-}75{\mu}m$$) and then dissolved in 3 different acids, HCl, $H_2SO_4$, $HNO_3$. Residues treated with acidic solution were recovered from the solution (step 1). And then the residual solution containing dissolved serpentine was titrated using $NH_4OH$. And pH of the solution increased up to pH=8.6 to obtain reddish precipitates (step 2). After recovery of the precipitates, the residual solution reacted with $CO_2$ and then pH increased up to pH=9.5 to precipitate white materials (step 3). The mineralogical characteristics of the original sample and harvested precipitates were examined by XRD, and TEM-EDS analyses. ICP-AES analysis was also used to investigate solution chemistry. The dissolved ions were Mg, Si, and Fe. The antigorite became noncrystralline silica after acid treatment (step 1). The precipitate at pH=8.6 was mainly amorphous iron oxide, of which size ranged from 2 to 10 nm and mainly consisting of Fe, O, and Si (step 2). At pH=9.5, nesquehonite [$Mg(HCO_3)(OH){\cdot}2(H_2O)$] and lasfordite [$MgCO_3{\cdot}H_2O$] were formed after reaction with $CO_2$ (step 3). The size of carbonated minerals was ranged from 1 to $6{\mu}m$. These results indicated that the acid treatment of serpentine and pH swing processes for the serpentine can be used for synthesis of other materials such as silica, iron oxides and magnesium carbonate. Also, This process may be useful for the precursor synthesis and $CO_2$ sequestration via mineral carbonation.

• Korean Journal of Heritage: History & Science
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• v.44 no.3
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• pp.112-131
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• 2011

This article reports the results of scientific analysis using SEM-EDX, XRD, TG/DTA, performed on 5 green glaze samples of the brick and roofing tile excavated from the Sacheonwang temple site in Gyeongju in order to verify the chemical compositions and melting temperature. The glaze samples on 2 clay statues have similar chemical composition (PbO 74~81%, $SiO_2$ 14~18%) and melting temperature range ($970{\sim}1070^{\circ}C$), whereas the 2 tiles of goblin's face and 1 rhomb brick have different characteristics. Sample SC 003 (made of PbO 63~67%, $SiO_2$ 25~28%), one of the tiles of goblin's face, shows low melting temperature range (below $970^{\circ}C$), and sample SC 004 (composed of PbO 64~70%, $SiO_2$ 19~25% and melting point $970{\sim}1070^{\circ}C$), the other tile of goblin's face, shows different chemical characteristics compared with 2 clay statues. The green glaze on rhomb brick shows different composition compared with all the others from Sacheonwang temple site in that it does not show any impurity elements other than the main components (PbO 87~88%, $SiO_2$ 12~13%) with very low melting temperature range ($750{\sim}770^{\circ}C$). Surprizingly, the chemical and optical characteristics of this green-glaze on rhomb brick are very similar to that on the bricks from Yeongmyo temple site, Gyeongju. The above results indicate that raw material and manufacturing method are not same for 5 green-glaze samples from Sacheonwang temple site and therefore suggests that further study on the provenance of raw material such as lead isotope analysis is necessary. Our work will provide basic data for future reproduction study of green glazed brick of Sacheonwang temple site, Gyeongju and will also serve as a reference data for the study of raw material and manufacturing method of green glaze from other sites of cultural assets.

• Applied Chemistry for Engineering
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• v.32 no.1
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• pp.117-123
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• 2021

In this study, the composite was prepared by mixing SiOx, soft carbon, and carbon black and the electrochemical properties of lithium ion battery were investigated. The content of SiOx added to improve the capacity of the soft carbon anode material was varied to 0, 6, 8, 10, 20 wt%, and carbon black was added as a structural stabilizer for reducing the volume expansion of SiOx. The physical properties of prepared CB/SiOx/C composite were investigated through XRD, SEM, EDS and powder resistance analysis. In addition, the electrochemical properties of prepared composite were observed through the charge/discharge capacity, rate and impedance analysis of the lithium ion battery. The prepared CB/SiOx/C composite had an inner cavity capable of mitigating the volume expansion of SiOx by adding carbon black. The formed internal cavity showed a low initial efficiency when the SiOx content was less than 8 wt%, and low cycle stability when the content of SiOx was less than 20 wt%. The CB/SiOx/C composite containing 10 wt% of SiOx showed an initial discharge capacity of 537 mAh/g, a capacity retention rate of 88%, and a rate of 79 at 2C/0.1C. SiOx was added to improve the capacity of the soft carbon anode material, and carbon black was added as a structural stabilizer to buffer the volume change of SiOx. In order to use the CB/SiOx/C composite as a high-efficiency anode material, the mechanism of the optimal SiOx and the use of carbon black as a structural stabilizer was discussed.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.1
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• pp.8-15
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• 2021

TiO2 has been used in various fields such as solar cells, dental implants, and photocatalysis, because it has high physical and chemical stability and is harmless to the body. TiO2 nanofibers which have a large specific surface area also show a good reactivity in bio-friendly products and excellent photocatalysis in air and water purification. To fabricate TiO2 nanofibers, an electrospinning method was used. To observe the diameter of TiO2 nanofibers with fabrication variables, the fabrication variables was divided into precursor composition variables and process variables and microstructure was analyzed. The concentrations of PVP (Polyvinylpyrrolidone) and TTIP (Titanium(IV) isopropoxide) were selected as precursor composition variables, and inflow velocity and voltage were also selected as process variables. Microstructure and crystal structure of TiO2 nanofibers were analyzed using FE-SEM (Field emission scanning electron microscope) and XRD (X-ray diffraction), respectively. As-spun TiO2 nanofibers with an average diameter of about 0.27 ㎛ to 1.31 ㎛ were transformed to anatase TiO2 nanofibers with an average diameter of about 0.22 ㎛ to 0.78 ㎛ after heat treatment of 3 hours at 450℃. Anatase TiO2 nanofibers with an average diameter of 0.22 ㎛ can be expected to improve the photocatalytic properties by increasing the specific surface area. To change the average diameter of TiO2 nanofibers, the control of precursor composition variables such as concentrations of PVP and TTIP is more efficient than the control of electrospinning process variables such as inflow velocity and voltage.

• Clean Technology
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• v.30 no.2
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• pp.134-144
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• 2024

In this study, the mechanical stability of red mud was improved for its commercial use as a catalyst to effectively decompose HFC-134a, one of the seven major greenhouse gases. Red mud is an industrial waste discharged from aluminum production, but it can be used for the decomposition of HFC-134a. Red mud can be manufactured into a catalyst via the crushing-preparative-compression molding-firing process, and it is possible to improve the catalyst performance and secure mechanical stability through calcination. In order to determine the optimal heat treatment conditions, pellet-shaped compressed red mud samples were calcined at 300, 600, 800 ℃ using a muffle furnace for 5 hours. The mechanical stability was confirmed by the weight loss rate before and after ultra-sonication after the catalyst was immersed in distilled water. The catalyst calcined at 800 ℃ (RM 800) was found to have the best mechanical stability as well as the most catalytic activity. The catalyst performance and durability tests that were performed for 100 hours using the RM 800 catalyst showed thatmore than 99% of 1 mol% HFC-134a was degraded at 650 ℃, and no degradation in catalytic activity was observed. XRD analysis showed tri-calcium aluminate and gehlenite crystalline phases, which enhance mechanical strength and catalytic activity due to the interaction of Ca, Si, and Al after heat treatment at 800 ℃. SEM/EDS analysis of the durability tested catalysts showed no losses in active substances or shape changes due to HFC-134a abasement. Through this research, it is expected that red mud can be commercialized as a catalyst for waste refrigerant treatment due to its high economic feasibility, high decomposition efficiency and mechanical stability.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.34 no.4
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• pp.109-116
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• 2024

β-Ga₂O₃ is a representative ultra-wide bandgap (UWBG) semiconductor that has attracted much attention for power device applications due to its wide-bandgap of 4.9 eV and high-breakdown voltage of 8 MV/cm. In addition, because solution growth is possible, it has advantages such as fast growth rate and lower production cost compared to SiC and GaN [1-2]. In this study, we have successfully grown Si-doped 10 mm thick Si-doped β-Ga₂O₃ single crystals by the EFG (Edge-defined Film-fed Growth) method. The growth direction and growth principal plane were set to [010] / (010), respectively, and the growth speed was 7~20 mm/h. The as-grown β-Ga₂O₃ single crystal was cut into various crystal planes (001, 100, ${\bar{2}}01$) and off-angles (1^o, 3^o, 4^o), and then surface processed. After processed, the homoepitaxial layer was grown on the epi-ready substrate using the HVPE (Halide vapor phase epitaxy) method. The processed samples and the epi-layer grown samples were analyzed by XRD, AFM, OM, and Etching to compare the surface properties according to the crystal plane and off-angle.

• Journal of the Korean Vacuum Society
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• v.18 no.2
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• pp.141-146
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• 2009

PLZT ferroelectric thin films were deposited on Pt/Ti/$SiO_2$/Si substrate with $TiO_2$ buffer layer in between by rf magnetron sputtering method. In order to investigate the effect of Ar/$O_2$ partial pressure ratio on the ferroelectric properties of PLZT thin films, PLZT thin films were deposited at various Ar/$O_2$ partial pressure ratio ; 27/1.5 seem, 23/5.5 seem, 21/7.5 seem and 19/9.5 seem. The crystallinities of PLZT thin films were analyzed by XRD. The surface morphology was observed using FE-SEM. The P-E hysteresis loops, the remanent polarization characteristics and the leakage current characteristics were obtained using a Precision LC. The crystallinity and elaborateness of PLZT thin films were decreased as increasing the oxygen partial pressure ratio. And preferred orientation of PLZT thin films changed from (110) plane to (111) plane. The oxygen partial pressure ratio affects the thin film surface morphology and the ferroelectric properties.

• Journal of the Mineralogical Society of Korea
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• v.27 no.1
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• pp.53-62
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• 2014

In order to remove Fe impurity from low-grade pyrophyllite ore, the effect of certain variables such as particle size, concentration of sulfuric acid, amount of ammonium sulfate, added hydrogen peroxide, and temperature were studied. The euhedral cubic pyrites were observed in the low-grade pyrophyllite ore by reflected light microscopy, and quartz and dickite were identified in the sample by XRD analysis. The results of the Fe removal experiments showed that the best Fe removal parameters were when the particle size was at -325 mesh, the addition of $H_2SO_4$, $(NH_4)_2SO_4$ and $H_2O_2$ was at a 2.0 M, 10.0 g/l, and 3.0 M concentration, respectively, and at a $70^{\circ}C$ leaching temperature. In the dissolution kinetics analysis, the dissolution of Fe from the pyrite surface was a controlled chemical reaction, and the Fe dissolution reaction was proportioned to 0.066/R, $[H_2SO_4]^{1.156}$, $[(NH_4)_2SO_4]^{0.745}$, $[H_2O_2]^{0.428}$.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.185-185
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• 2012

중공 발광 나노 물질은 특유의 구조적 특성(낮은 밀도, 높은 비표면적, 다공성 물질, 낮은 열팽창계수 등)과 광학적 성질을 이용하여 디스플레이 패널, 광결정, 약물전달체, 바이오 이미징 라벨 등의 다양한 적용이 가능하다. 이러한 적용에 있어 균일한 크기와 형태의 중공 입자는 필수 조건으로 여겨진다. 지금까지 합성된 중공 발광 입자에는 BaMgAl10O17 : Eu2+-Nd3+, Gd2O3 : Eu3+, $EuPO_4{\cdot}H_2O$과 같은 것들이 있으나 크기 조절이 어렵고, 그 균일성이 확보되지 못하였다. 균일한 크기의 중공 발광 입자를 만들기 위해 SiO2나 emulsion을 템플릿으로 이용하여 황화카드뮴, 카드뮴 셀레나이드 중공 입자를 합성한 예가 있으나, 양자점의 독성으로 인하여 바이오분야 응용에는 적합하지 않다. YAG는 모체로써 형광체에서 가장 많이 이용되는 물질로, 화학적 안정성과 낮은 독성, 높은 양자 효율 등 많은 장점을 갖고 있다. 특히 세륨이 도핑된 YAG형광체의 경우 WLED, 신틸레이터, 바이오산업에 적용이 가능하다. 그러나 지금까지 중공 YAG:Ce3+형광체를 합성한 예가 없었다. 본 연구에서는 단분산 수화 알루미늄 (Al(OH)3) 입자 위에 세륨이 도핑 된 이트륨 베이직 카보네이트 ($Y(OH)CO_3$)를 균일하게 코팅한 후 열처리를 하여 균일한 크기의 Y3Al5O12:Ce3+(YAG) 중공 입자를 합성하였다. 열처리 온도에 따른 고분해능 투과 전자 현미경(HRTEM), X-선 회절(XRD), 고분해능 에너지 분광법(HREDX) 분석결과, 중공 YAG: Ce3+입자는 Kirkendall 효과에 의해 형성됨을 확인하였다. 전계방사형 주사 전자 현미경(FE-SEM) 측정을 통해, 열처리 후에도 입자의 크기와 형태가 균일함을 확인하였으며, 공초점 현미경 관찰을 통해 중공 형태를 명확히 확인 할 수 있었다. Photoluminescence (PL) 분광법과 형광 수명 이미징 현미경(FLIM)을 이용한 광 특성 분석결과, 합성된 입자는 400-500 nm에서 흡수 파장 (456 nm에서 최대 강도)과 500-700 nm 범위의 발광 파장(544 nm에서 최대 강도)을 나타냈고, 상용 YAG: Ce3+(70 ns)에 준하는 74 ns의 잔광 시간(decay time)이 측정되었다. 단분산 수화 알루미늄 입자의 크기를 조절하여 최종 합성된 YAG: Ce3+의 크기를 조절할 수 있었다. 지름 약 600 nm의 Al(OH)3를 사용한 경우, $1,300^{\circ}C$에서 열처리를 한 후 평균 지름 590 nm의 중공입자를 합성하였고, 약 170 nm의 Al(OH)3를 이용하여, 더 낮은 온도인 $1,100^{\circ}C$에서의 열처리를 통해 평균지름 140 nm의 중공 YAG: Ce3+입자를 합성하였다. 본 연구를 통하여 합성된 균일한 크기의 YAG 중공입자는 LED와 같은 광전변환 소자 및 다기능성 바이오 이미징 등의 나노바이오 소자 분야에 활용될 수 있음이 기대된다.