• Title/Summary/Keyword: electron microscopy

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Characterization of Synthesized Carbonate and Sulfate Green Rusts: Formation Mechanisms and Physicochemical Properties (합성된 탄산염 및 황산염 그린 러스트의 형성 메커니즘과 이화학적 특성 규명)

  • Lee, Seon Yong;Choi, Su-Yeon;Chang, Bongsu;Lee, Young Jae
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.2
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    • pp.111-123
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    • 2022
  • Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO32-) and sulfate (SO42-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.

Interpretation of Firing Temperature and Thermal Deformation of Roof Tiles from Ancient Tombs of Seokchon-dong in Seoul, Korea (서울 석촌동 고분군 출토 기와의 소성온도와 열변형 특성 해석)

  • Jin, Hong Ju;Jang, Sungyoon;Lee, Myeong Seong
    • Economic and Environmental Geology
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    • v.54 no.6
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    • pp.671-687
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    • 2021
  • This study investigated the firing temperature and thermal deformation process of roof tiles excavated from the connected stone-mound tomb in Seokchon-dong, Seoul, based on mineralogical and physical properties. A large number of roof tiles were excavated from the tomb site and some roof tiles were deformed by heat and were fired in uneven conditions. The colors of original roof tiles and their cores are mostly yellowish-brown, with high water absorption over 12%, containing fine-grained textures and some minerals such as quartz, feldspars, amphibole, and mica. It is estimated that the original roof tiles were fired below 900℃ in oxidation condition, showing loose matrices and mica layers by scanning electron microscopy. However, deformed roof tiles have the uneven surface color of reddish-brown and bluish-gray, and those cross-sections have sandwich structures in which dense reddish-brown surface and porous grey core coexist. They contained mullite and hercynite, so it was estimated to have been fired over 1,000℃, with 0.81~11% water absorption. In some samples, bloating pores by overfiring were observed, which means that they were fired at more than 1,200℃. In addition, the refirng experiments that the original roof tile was fired between 800℃ and 1,200℃ were carried out to investigate the physical and mineralogical properties of roof tiles compared to deformed ones. As a result, the water absorption decreased rapidly and the mineral phase started to change over 1,000℃. As the temperature gradually rises, the matrices are partially melted and recrystallized, resulting in similar thermal characteristics of deformed roof tiles. Therefore, the roof tiles from ancient tombs in Seokchon-dong seem to experience the secondary high temperature of 1,000 to 1,200℃ under uneven firing conditions, resulting in deformation characteristics such as shape transformation and mineral phase transition. It is considered to have been related to cremation rituals at the tombs of Seockchon-dong during the Baekje period.

Phase Behavior Study of Fatty Acid Potassium Cream Soaps (지방산 칼륨 Cream Soaps 의 상거동 연구)

  • Noh, Min Joo;Yeo, Hye Lim;Lee, Ji Hyun;Park, Myeong Sam;Lee, Jun Bae;Yoon, Moung Seok
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.1
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    • pp.55-64
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    • 2022
  • The potassium cream soap with fatty acid called cleaning foam has a crystal gel structure, and unlike an emulsion system, it is weak to shear stress and shows characteristics that are easily separated under high temperature storage conditions. The crystal gel structure of cleansing foams is significantly influenced by the nature and proportion of fatty acids, degree of neutralization, and the nature and proportion of polyols. In order to investigate the effect of these parameters on the crystal gel structure, a ternary system consisting of water/KOH/fatty acid was investigated in this study. The investigation of differential scanning calorimeter (DSC) revealed that the eutectic point was found at the ratio of myristic acid (MA) : stearic acid (SA) = 3 : 1 and ternary systems were the most stable at the eutectic point. However, the increase in fatty acid content had little effect on stability. On the basis of viscosity and polarized optical microscopy (POM) measurements, the optimum degree of neutralization was found to be about 75%. The system was stable when the melting point (Tm) of the ternary system was higher than the storage temperature and the crystal phase was transferred to lamellar gel phase, but the increase in fatty acid content had little effect on stability. The addition of polyols to the ternary system played an important role in changing the Tm and causing phase transition. The structure of the cleansing foams were confirmed through cryogenic scanning electron microscope (Cryo-SEM), small and wide angle X-ray scattering (SAXS and WAXS) analysis. Since butylene glycol (BG), propylene glycol (PG), and dipropylene glycol (DPG) lowered the Tm and hindered the lamellar gel formation, they were unsuitable for the formation of stable cleansing foam. In contrast, glycerin, PEG-400, and sorbitol increased the Tm, and facilitated the formation of lamellar gel phase, which led to a stable ternary system. Glycerin was found to be the most optimal agent to prepare a cleansing foam with enhanced stability.

Behaviors of Soft Bangkok Clay behind Diaphragm Wall Under Unloading Compression Triaxial Test (삼축압축 하에서 지중연속벽 주변 방콕 연약 점토의 거동)

  • Le, Nghia Trong;Teparaksa, Wanchai;Mitachi, Toshiyuki;Kawaguchi, Takayuki
    • Journal of the Korean Geotechnical Society
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    • v.23 no.9
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    • pp.5-16
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    • 2007
  • The simple linear elastic-perfectly plastic model with soil parameters $s_u,\;E_u$ and n of undrained condition is usually applied to predict the displacement of a constructed diaphragm wall(DW) on soft soils during excavation. However, the application of this soil model for finite element analysis could not interpret the continued increment of the lateral displacement of the DW for the large and deep excavation area both during the elapsed time without activity of excavation and after finishing excavation. To study the characteristic behaviors of soil behind the DW during the periods without excavation, a series of tests on soft Bangkok clay samples are simulated in the same manner as stress condition of soil elements happening behind diaphragm wall by triaxial tests. Three kinds of triaxial tests are carried out in this research: $K_0$ consolidated undrained compression($CK_0U_C$) and $K_0$ consolidated drained/undrained unloading compression with periodic decrement of horizontal pressure($CK_0DUC$ and $CK_0UUC$). The study shows that the shear strength of series $CK_0DUC$ tests is equal to the residual strength of $CK_0UC$ tests. The Young's modulus determined at each decrement step of the horizontal pressure of soil specimen on $CK_0DUC$ tests decreases with increase in the deviator stress. In addition, the slope of Critical State Line of both $CK_0UC$ and $CK_0DUC$ tests is equal. Moreover, the axial and radial strain rates of each decrement of horizontal pressure step of $CK_0DUC$ tests are established with the function of time, a slope of critical state line and a ratio of deviator and mean effective stress. This study shows that the results of the unloading compression triaxial tests can be used to predict the diaphragm wall deflection during excavation.

Structural and functional characteristics of rock-boring clam Barnea manilensis (암석을 천공하는 돌맛조개(Barnea manilensis)의 구조 및 기능)

  • Ji Yeong Kim;Yun Jeon Ahn;Tae Jin Kim;Seung Min Won;Seung Won Lee;Jongwon Song;Jeongeun Bak
    • Korean Journal of Environmental Biology
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    • v.40 no.4
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    • pp.413-422
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    • 2022
  • Barnea manilensis is a bivalve which bores soft rocks, such as, limestone or mudstone in the low intertidal zone. They make burrows which have narrow entrances and wide interiors and live in these burrows for a lifetime. In this study, the morphology and the microstructure of the valve of rock-boring clam B. manilensis were observed using a stereoscopic microscope and FE-SEM, respectively. The chemical composition of specific part of the valve was assessed by energy dispersive X-ray spectroscopy (EDS) analysis. 3D modeling and structural dynamic analysis were used to simulate the boring behavior of B. manilensis. Microscopy results showed that the valve was asymmetric with plow-like spikes which were located on the anterior surface of the valve and were distributed in a specific direction. The anterior parts of the valve were thicker than the posterior parts. EDS results indicated that the valve mainly consisted of calcium carbonate, while metal elements, such as, Al, Si, Mn, Fe, and Mg were detected on the outer surface of the anterior spikes. It was assumed that the metal elements increased the strength of the valve, thus helping the B. manilensis to bore sediment. The simulation showed that spikes located on the anterior part of the valve received a load at all angles. It was suggested that the anterior part of the shell received the load while drilling rocks. The boring mechanism using the amorphous valve of B. manilensis is expected to be used as basic data to devise an efficient drilling mechanism.

Influence of a chemical additive on the reduction of highly concentrated ammonium nitrogen(NH4+-N) in pig wastewater (양돈 폐수로부터 고농도 암모니아성 질소의 감소를 위한 화학적 첨가제의 영향)

  • Su Ho Bae;Eun Kim;Keon Sang Ryoo
    • Korean Journal of Environmental Biology
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    • v.40 no.3
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    • pp.267-274
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    • 2022
  • Excess nitrogen (N) flowing from livestock manure to water systems poses a serious threat to the natural environment. Thus, livestock wastewater management has recently drawn attention to this related field. This study first attempted to obtain the optimal conditions for the further volatilization of NH3 gas generated from pig wastewater by adjusting the amount of injected magnesia (MgO). At 0.8 wt.% of MgO (by pig wastewater weight), the volatility rate of NH3 increased to 75.5% after a day of aeration compared to untreated samples (pig wastewater itself). This phenomenon was attributed to increases in the pH of pig wastewater as MgO dissolved in it, increasing the volatilization efficiency of NH3. The initial pH of pig wastewater was 8.4, and the pH was 9.2 when MgO was added up to 0.8 wt.%. Second, the residual ammonia nitrogen (NH4+-N) in pig wastewater was removed by precipitation in the form of struvite (NH4MgPO4·6H2O) by adjusting the pH after adding MgO and H3PO4. Struvite produced in the pig wastewater was identified by field emission scanning electron microscopy (FE-SEM) and X-ray diffraction (XRD) analysis. White precipitates began to form at pH 6, and the higher the pH, the lower the concentration of NH4+-N in pig wastewater. Of the total 86.1% of NH4+-N removed, 62.4% was achieved at pH 6, which was the highest removal rate. Furthermore, how struvite changes with pH was investigated. Under conditions of pH 11 or higher, the synthesized struvite was completely decomposed. The yield of struvite in the precipitate was determined to be between 68% and 84% through a variety of analyses.

Comparison of shear bond strength between various temporary prostheses resin blocks fabricated by subtractive and additive manufacturing methods bonded to self-curing reline resin (절삭 및 적층 가공법으로 제작한 임시 보철물 레진 블록과 재이 장용 자가중합 레진의 전단결합강도 비교)

  • Hyo-Min Ryu;Jin-Han Lee
    • The Journal of Korean Academy of Prosthodontics
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    • v.61 no.3
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    • pp.189-197
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    • 2023
  • Purpose. This study aimed to compare and evaluate the shear bond strength between various temporary prostheses resin blocks fabricated by subtractive and additive manufacturing methods bonded to self-curing reline resin. Materials and methods. The experimental groups were divided into 4 groups according to the manufacturing methods of the resin block specimens and each specimen was fabricated by subtractive manufacturing (SM), additive manufacturing stereolithography apparatus manufacturing (AMS), additive manufacturing digital light processing manufacturing (AMD) and conventional self-curing (CON). To bond the resin block specimens and self-curing resin, the reline resin was injected and polymerized into the same location of each resin block using a silicone mold. The shear bond strength was measured using a universal testing machine, and the surface of the adhesive interface was examined by scanning electron microscopy. To compare between groups, one-way ANOVA was done followed by Tukey post hoc test (α = 0.05). Results. The shear bond strength showed higher values in the order of CON, SM, AMS, and AMD group. There were significant differences between CON and AMS groups, as well as between CON and AMD groups. but there were no significant differences between CON and SM groups (P > .05). There were significant differences between SM and AMD groups, but there were no significant differences between SM and AMS groups. The AMS group was significantly different from the AMD group (P < .001). The most frequent failure mode was mixed failures in CON and AMS groups, and adhesive failures in SM and AMD groups. Conclusion. The shear bond strength of SM group showed lower but not significant bond strength compared to the CON group. The additive manufacturing method groups (AMS and AMD) showed significantly lower bond strength than the CON group, with the AMD group the lowest. There was also a significant difference between the AMD and SM group.

A study of the antifungal properties and flexural strength of 3D printed denture base resin containing titanium dioxide nanoparticles (이산화티타늄 나노입자를 함유한 3D 프린팅 의치상 레진의 항진균성 및 굽힘 강도에 대한 연구)

  • Seok-Won Yoon;Young-Eun Cho
    • The Journal of Korean Academy of Prosthodontics
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    • v.62 no.2
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    • pp.95-103
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    • 2024
  • Purpose. With the advancement of digital technology, 3D printing is being utilized in the fabrication of denture base. Nevertheless, increasing microbial adhesion to the surface of denture base has been reported as the disadvantage of 3D-printed denture base. The purpose of this study is to investigate the antifungal properties and flexural strength of 3D-printed denture base resin according to the different contents of titanium dioxide nanoparticles. Materials and methods. Titanium dioxide nanoparticles were mixed with the 3D printing resin at the ratios of 0.5, 1, 1.5, and 2 wt%. Twenty specimens per each group were printed in the form of cylindrical shape (diameter: 20 mm, height: 3 mm) to evaluate antifungal properties. Ten specimens from each group underwent polishing using autogrinder, while the remaining ten specimens did not. Candida albicans in hyphae form was inoculated onto each specimen, optical density and colony-forming unit were analyzed. The surface of the specimen was observed using scanning electron microscopy. To evaluate the flexural strength, twenty specimens per each group were 3D printed in the form of rectangular prism shape (length: 64 mm, height: 10 mm, width: 3 mm) and three-point bending tests were conducted using universal testing machine according to ISO 20795-1. Results. Colony-forming unit of C.albicans and optical density of culture medium showed no difference between non-polished groups, but decreased in the polished groups at concentration of 1, 1.5, 2 wt% titanium dioxide nanoparticles. Flexural strength increased with titanium dioxide nanoparticle at concentration of 0.5, 1, 1.5 wt%, but decreased at 2 wt% compared to 1.5 wt%. Conclusion. When 1.5 wt% of titanium dioxide nanoparticles were added to the 3D-printed denture base resin with polishing, antifungal properties were increased.

Preparation and Gas Permeation Performance of Pd-Ag-Cu Hydrogen Separation Membrane Using α-Al2O3 Support (α-Al2O3 지지체를 이용한 Pd-Ag-Cu 수소 분리막의 제조 및 기체투과 성능)

  • Sung Woo Han;Min Chang Shin;Xuelong Zhuang;Jae Yeon Hwang;Min Young Ko;Si Eun Kim;Chang Hoon Jung;Jung Hoon Park
    • Membrane Journal
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    • v.34 no.1
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    • pp.50-57
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    • 2024
  • In this experiment, Pd-Ag-Cu membrane was manufactured using electroless plating on an α-Al2O3 support. Pd, Ag and Cu were each coated on the surface of the support through electroless plating and heat treatment was performed for 18 h at 500℃ in H2 in the middle of electroless plating to form Pd alloy. The surface of the Pd-Ag-Cu membrane was observed through Scanning Electron Microscopy (SEM), and the thickness of the Pd membrane was measured to be 7.82 ㎛ and the thickness of the Pd-Ag-Cu membrane was measured to be 3.54 ㎛. Energy dispersive X-ray spectroscopy and X-ray diffraction analysis confirmed the formation of a Pd-Ag-Cu alloy with a composition of Pd-78wt%, Ag-8.81wt% and Cu-13.19wt%. The gas permeation experiment was conducted under the conditions of 350~450℃ and 1~4 bar in H2 single gas and H2/N2 mixed gas. The maximum H2 flux of the hydrogen separation membrane measured in H2 single gas is 74.16 ml/cm2·min at 450℃ and 4 bar for the Pd membrane and 113.64 ml/cm2·min at 450℃ and 4 bar for the Pd-Ag-Cu membrane. In the case of the separation factor measured in H2/N2 mixed gas, separation factors of 2437 and 11032 were measured at 450℃ and 4 bar.

Phase Equilibria of the System Pd-Sb-Te and Its Geological Implications (팔라듐-안티몬-테루르 계(系)의 상평형(相平衡)과 지질학적(地質學的) 의의(意義))

  • Kim, Won-Sa;Chao, George Y.
    • Economic and Environmental Geology
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    • v.26 no.3
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    • pp.327-335
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    • 1993
  • Phase relations in the system Pd-Sb-Te were investigated at $1000^{\circ}$, $800^{\circ}$, and $600^{\circ}C$, using the sealed-capsule technique; the quenched products were studied by reflected light microscopy, X-ray diffraction, and electron microprobe analysis. At $1000^{\circ}C$, the solid phases Pd, $Pd_{20}Sb_7$, $Pd_8Sb_3$, $Pd_{31}Sb_{12}$, and $Pd_5Sb_2$ are stable with a liquid phase that occupies most of the isothermal diagram. Additional solid phases at $800^{\circ}C$ are $Pd_5Sb_3$, PdSb, $Pd_8Te_3$, $Pd_7Te_3$, and a continuous $Pd_{20}Te_7-Pd_{20}Sb_7$ solid solution becomes stable. At $600^{\circ}$, $PdSb_2$, $Pd_{17}Te_4$, $Pd_9Te_4$, PdTe, $PdTe_2$, $Sb_2Te_3$, and Sb and continuous PdSb-PdTe and $PdTe-PdTe_2$ solid solutions are stable. All the solid phases exhibit solid solution, mainly by substitution between Sb and Te to an extent that varies with temperature of formation. The maximum substitution (at.%) of Te for Sb in the Pd-Sb phases is: 44.3 in $Pd_8Sb_3$, 52.0 in $Pd_{31}Sb_{12}$, 46.2 in $Pd_5Sb_2$ at $800^{\circ}C$; 15.3 in $Pd_5Sb_3$, 68.3 in $PdSb_2$ at $600^{\circ}C$. The maximum substitution (at.%) of Sb for Te in the Pd-Te phases is 34.5 in $Pd_5Sb_3$ at $800^{\circ}C$, and 41.6 in $Pd_7Te_3$, 5.2 in $Pd_{17}T_4$, 12.4 in $Pd_9Te_4$, and 19.1 in $PdTe_2$ at $600^{\circ}C$. Physical properties and X-ray data of the synthetic $Pd_9Te_4$, PdTe, $PdTe_2$, $Pd_8Sb_3$, PdSb, and $Sb_2Te_3$ correspond very well with those of telluropalladinite, kotulskite, merenskyite, mertieite II, sudburyite, and tellurantimony, respectively. Because X-ray powder diffraction data consistently reveal a 310 peak ($2.035{\AA}$), the $PdSb_2$ phase is most probably of cubic structure with space group $P2_13$. The X-ray powder pattern of a phase with PdSbTe composition, synthesized at $600^{\circ}C$, compares well with that of testibipalladite. Therefore, testibiopalladite may be a member of the $PdSb_2-Pd(Sb_{0.32}Te_{0.68})$ solid solution series which is cubic and $P2_13$ in symmetry. Thus the ideal fonnula for testibiopalladite, presently PdSbTe, must be revised to PdTe(Sb, Te). Borovskite($pd_3SbTe_4$) has not been found in the synthetic system in the temperature range $1000^{\circ}-600^{\circ}C$.

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