• Title/Summary/Keyword: TEM analysis

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Silica and Iron Oxide Recovery and Mineral Carbonation from Serpentine Minerals Using Acid Dissolution and pH Swing Processes (산 처리와 pH 조절을 이용한 사문석군 광물로부터 규소와 철산화물 회수 및 광물 탄산화 연구)

  • Baek, Jiyeon;Jo, Yeonu;Lee, Jeongheon;Kwon, Nayoon;Kim, Yeram;Choi, Suk;Kim, Sunghee;Roh, Yul
    • 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.

Liposome Formation and Active Ingredient Capsulation on the Supercritical Condition (초임계 상태에서 리포좀의 생성 및 약물봉입)

  • Mun, Yong-Jun;Cha, Joo-Hwan;Kim, In-Young
    • Journal of the Korean Applied Science and Technology
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    • v.38 no.6
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    • pp.1687-1698
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    • 2021
  • This study is to produce multiple layers of liposomes in a supercritical state and encapsulates active ingredients in order to stably encapsulate thermodynamically unstable active ingredients. In order to form a liposome in a supercritical state, a mixed surfactant development including vegetable-derived hydrogenated phosphatidyl choline and their delivative, hydrogenated sucrose distearate was synthesized as high purity. It describes a manufacturing method of injecting liquid carbon dioxide into a reactor to create a supercritical state and stirring to produce a giant liposome, and adding and loading genistein and quercetin. The HLB of the mixed lipid complex (SC-Lipid Complex) was 12.50, and multiple layers of liposome vesicles were formed even at very low concentrations. This surfactant had a specific odor with a pale yellow flake, the specific gravity was 0.972, and the acid value was 0.12, indicating that it was synthesized with high purity. As a result of the emulsifying capacity experiment using 20 wt% capric/capric triglyceride and triethylhexanoin using SC-Lipid Complex, it was found to have 96.2% emulsifying power. SC LIPOSOME GENISTEIN was confirmed that a multi-layer liposome vesicle was formed through a transmission electron microscope (Cryo-TEM) for the supercritical liposome encapsulated with genistein. The primary liposome particle size in which genistein was encapsulated was 253.9 nm, and the secondary capsule size was 18.2 ㎛. Using genistein as the standard substance, the encapsulation efficiency of supercritical liposomes was 99.5%, and general liposomes were found to have an efficiency of 93.6%. In addition, the antioxidant activity experiment in which quercetin was sealed was confirmed by the DPPH method, and it was found that the supercritical liposome significantly maintained excellent antioxidant activity. In this study, thermodynamically unstable raw materials were sealed into liposomes without organic solvents in a supercritical state. Based on these results, it is expected that it can be applied to various forms such as highly functional skincare cosmetics, makeup cosmetics, and scalp protection cosmetics.

A Study of Properties and Coating Natural Mineral Pumice Powder of in Korea (한국산 천연 광물 부석 파우더 코팅 및 특성에 관한 연구)

  • Kim, In-Young;Noh, Ji-Min;Nam, Eun-Hee;Shin, Moon-Sam
    • Journal of the Korean Applied Science and Technology
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    • v.36 no.2
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    • pp.498-506
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    • 2019
  • This study is based on a coating method that provides utilization value as a micronised powder for cosmetic raw materials using natural minerals buried in Bonghwa, Gyeongsangbuk-do in Korea. The mineral powder name is called Buseok, and chemical name is pumice powder. The results of a study on the efficacy of cosmetics are reported by the development of particulate powder to assess the performance of this powder. First of all, in order to coat the surface of this powder with oil, aluminum hydroxide was coated on the particulate surface and then coated with alkylsilan. In addition, it was coated with vegetable oil to prevent condensation of the powder and increase the dispersion in the oil phase. First; the particle size of pumice powder was from 10 to 50mm having porous holes on the surface of the particles. Second; The components of this powder contained $SiO_2$, $Al_2O_3$, $Fe_2O_3$, MgO, CaO, $K_2O_2$, $Na_2O$, $TiO_2$, $TiO_2$, MnO, $Cr_2O_3$, $V_2O_5$. Third: The particles of this powder have a planetary structure and are reddish-brown with porosity through SEM and TEM analysis. Fourth; the far-infrared radiation rate of this parabolic powder was $0.924{\mu}m$, and the radiative energy was $3.72{\times}102W/m^2$ and ${\mu}m$. In addition, the anion emission is 128 ION/cc, which shows that the coating remains unchanged. Based on these results, it is expected to be widely applied to basic cosmetics such as BB cream, cushion foundation, powderfect, and other color-coordinated cosmetics, sunblock cream, wash-off massage pack as an application of cosmetics. (Small and Medium Business Administration: S2601385)

Micromorphological and Chemical Characteristics of Cengal (Neobalanocarpus heimii) Heartwood Decayed by Soft Rot Fungi

  • Kim, Yoon Soo;Singh, Adya P.;Wong, Andrew H.H.;Eom, Tae-Jin;Lee, Kwang Ho
    • Journal of the Korean Wood Science and Technology
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    • v.34 no.2
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    • pp.68-77
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    • 2006
  • The heartwood of cengal (Neobalanocarpus heimii) is known to have a high degree of decay resistance by virtue of its high extractive content. After 30 years in ground contact an utility pole of this tropical hardwood was found to be degraded only in the surface layers by cavity-forming soft rot fungi. The present work was undertaken 1) to characterize the degradation of cengal heartwood from the aspect of ultrastructure and chemistry and 2) to investigate the correlation between soft rot decay and its extractive microdistribution in wood tissues. The chemical analysis of cengal heartwood revealed the presence of a high amount of extractives as well as lignin. The wood contained a relatively high amount of condensed lignin and the guaiacyl units. Microscopic observations revealed that vessels, fibers and parenchyma cells (both ray and axial parenchyma) all contained extractives in their lumina, but in variable amounts. The lumina of fibers and most axial parenchyma were completely or almost completely filled with the extractives. TEM micrographs showed that cell walls were also impregnated with extractives and that pit membranes connecting parenchyma cells were well coated and impregnated with extractives. However, fungal hyphae were present in the extractive masses localized in cell lumina, and indications were that the extractives did not completely inhibit fungal growth. The extent of cell wall degradation varied with tissue types. The fibers appeared to be more susceptible to decay than vessels and parenchyma. Middle lamella was the only cell wall region which remained intact in all cell types which were severely degraded. The microscopic observations suggested a close correlation between extractive microdistribution and the pattern and extent of cell wall degradation. In addition to the toxicity to fungi, the physical constraint of the extractive material present in cengal heartwood cells is likely to have a profound effect on the growth and path of invasion of colonizing fungi, thus conferring protection to wood by restricting fungal entry into cell walls. The presence of relatively high amount of condensed lignin is also likely to be a factor in the resistance of cengal heartwood to soft rot decay.

Chemical and TEM Studies of Chklorites in the Talc Deposites of the Chungnam Area, Korea (우리나라 충남지역 활석광상에서 산출되는 녹니석의 화학적 및 투과전자현미경 연구)

  • Geon-Young Kim;Soo Jin Kim
    • Journal of the Mineralogical Society of Korea
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    • v.13 no.2
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    • pp.53-64
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    • 2000
  • Chlorite from the talc deposits in the Chungnam area, Korea, has been studied using electron microprobe analysis and high resolution transmission electron microscopy (HRTEM), Talc orea are hydrothermal alteration products of serpentinite which was originated from ultramafic rocks. Chlorite occurs in close association with talc ores of with the black alteration zone between talc ore bodies and granitic gneiss. It is the most abundant impurity mineral of talc ores. Chlorite in association with talc is characterized by very high but narrow variation in Mg/(Mg+Fe) ratios (0.784~0.951), significant octahedral substitution (-0.200~0.692), wide variation in Al contents (1.085~3.160 / 14 oxygens), and high Cr and Ni contents. It was formed under a very limited but high Mg/(Mg+Fe) condition in close connection with serpentinite. Chlorite in the black alteration zone is characterized by a high Fe content, wide variation in Mg/(Mg+Fe) ratios (0.378~0.852), narrow octahedral substitution (-0.035~0.525), high narrow Al contents (1.468~2.959), and low Cr and Ni contents. It was formed under a low Mg/(Mg+Fe) and relatively Al-rich condition in close connection with county rocks. Two different chemical modes for chlorite suggest two different origins for two different chlorites. Although most of chlorites show typical 14-$\AA$ lattice fringe images under HRTEM, some chlorites show fringe images of 21-$\AA$ (14$\AA$+7$\AA$) spacings within (001) lattice-fringe images of chlorite (14$\AA$). But brown chlorite from the black zone has high Ti and K contents suggesting that mica was the precursor of brown chlorite. Such possibility is also supported by the fact that lattice-fringe images of brown chlorite show 14-$\AA$ chlorite layers in which 10-$\AA$ mica single layer or packets are interlayered. Partial terminations from 3 mica layers to 2 chlorite layers are often observed. It, therefore, is suggested that the chlorite associated with talc ores is a hydrothermal alteration products of serpentinite, whereas the chlorites in the black alteration zone is a hydrothermal alteration product of granitic gnesis under a partial influence of serpentinite.

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High Quality Nano Structured Single Gas Barrier Layer by Neutral Beam Assisted Sputtering (NBAS) Process

  • Jang, Yun-Sung;Lee, You-Jong;Hong, Mun-Pyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.251-252
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    • 2012
  • Recently, the growing interest in organic microelectronic devices including OLEDs has led to an increasing amount of research into their many potential applications in the area of flexible electronic devices based on plastic substrates. However, these organic devices require a gas barrier coating to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency OLEDs require an extremely low Water Vapor Transition Rate (WVTR) of $1{\times}10^{-6}g/m^2$/day. The Key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required ($1{\times}10^{-6}g/m^2$/day) is the suppression of defect sites and gas diffusion pathways between grain boundaries. In this study, we developed an $Al_2O_3$ nano-crystal structure single gas barrier layer using a Neutral Beam Assisted Sputtering (NBAS) process. The NBAS system is based on the conventional RF magnetron sputtering and neutral beam source. The neutral beam source consists of an electron cyclotron Resonance (ECR) plasma source and metal reflector. The Ar+ ions in the ECR plasma are accelerated in the plasma sheath between the plasma and reflector, which are then neutralized by Auger neutralization. The neutral beam energies were possible to estimate indirectly through previous experiments and binary collision model. The accelerating potential is the sum of the plasma potential and reflector bias. In previous experiments, while adjusting the reflector bias, changes in the plasma density and the plasma potential were not observed. The neutral beam energy is controlled by the metal reflector bias. The NBAS process can continuously change crystalline structures from an amorphous phase to nano-crystal phase of various grain sizes within a single inorganic thin film. These NBAS process effects can lead to the formation of a nano-crystal structure barrier layer which effectively limits gas diffusion through the pathways between grain boundaries. Our results verify the nano-crystal structure of the NBAS processed $Al_2O_3$ single gas barrier layer through dielectric constant measurement, break down field measurement, and TEM analysis. Finally, the WVTR of $Al_2O_3$ nano-crystal structure single gas barrier layer was measured to be under $5{\times}10^{-6}g/m^2$/day therefore we can confirm that NBAS processed $Al_2O_3$ nano-crystal structure single gas barrier layer is suitable for OLED application.

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Synthesis of Ceria Nanoparticles Using Supercritical Methanol with Various Surface Modifiers (초임계 메탄올을 이용한 표면개질된 세리아 나노입자의 합성)

  • Ahn, Ki Ho;Shin, Nae-Chul;Kim, Minsoo;Youn, Yong-Suk;Hong, Giyoung;Lee, Youn-Woo
    • Korean Chemical Engineering Research
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    • v.50 no.4
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    • pp.678-683
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    • 2012
  • Ceria is one of the most important catalytic materials which can be used in three-way catalysts, waste water treatment, petroleum refining, etc. So far, many methods have been studied to produce ceria nanoparticles. In this study, ceria nanoparticles were prepared via solvothermal synthesis using supercritical methanol in short reaction time using a batch reactor. The size of synthesized ceria nanoparticles in supercritical methanol is 6 nm without capping agent, which is smaller than that made in supercritical water at the same conditions of $400^{\circ}C$ and 30 MPa. Size difference results from density and critical point difference between water and methanol and slow reaction rate at the surface of ceria particles in supercritical methanol which reduces crystal growth rate. Several organic compounds were added to modify the surface of ceria nanoparticles, and in-situ surface modification was confirmed by FT-IR and TGA analysis. Surface modified ceria nanoparticles have excellent dispersibility in organic solvent. Size and shape of surface modified ceria particles can be controlled by adjusting molar ratio of modifier to precursor and selection of modifier.

Effects of Microstructures on the Toughness of High Heat Input EG Welded Joint of EH36-TM Steel (EH36-TM강의 대입열 EGW 용접부 저온 인성에 미치는 미세 조직의 영향)

  • Choi, Woo-Hyuk;Cho, Sung-Kyu;Choi, Won-Kyu;Ko, Sang-Gi;Han, Jong-Man
    • Journal of Welding and Joining
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    • v.30 no.1
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    • pp.64-71
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    • 2012
  • The characteristics of high heat input (342kJ/cm) EG (Electro Gas Arc) welded joint of EH36-TM steel has been investigated. The weld metal microstructure consisted of fine acicular ferrite (AF), a little volume of polygonal ferrite (PF) and grain boundary ferrite (GBF). Charpy impact test results of the weld metal and heat affected zone (HAZ) met the requirement of classification rule (Min. 34J at $-20^{\circ}C$). In order to evaluate the relationship between the impact toughness property and the grain size of HAZ, the austenite grain size of HAZ was measured. The prior austenite grain size in Fusion line (F.L+0.1 mm) was about $350{\mu}m$. The grain size in F.L+1.5 mm was measured to be less than $30{\mu}m$ and this region was identified as being included in FGHAZ(Fine Grain HAZ). It is seen that as the austenite grain size decreases, the size of GBF, FSP (Ferrite Side Plate) become smaller and the impact toughness of HAZ increases. Therefore, the CGHAZ was considered to be area up to 1.3mm away from the fusion line. Results of TEM replica analysis for a welded joint implied that very small size ($0.8\sim1.2{\mu}m$) oxygen inclusions played a role of forming fine acicular ferrite in the weld metal. A large amount of (Ti, Mn, Al)xOy oxygen inclusions dispersed, and oxides density was measured to be 4,600-5,300 (ea/mm2). During the welding thermal cycle, the area near a fusion line was reheated to temperature exceeding $1400^{\circ}C$. However, the nitrides and carbides were not completely dissolved near the fusion line because of rapid heating and cooling rate. Instead, they might grow during the cooling process. TiC precipitates of about 50 ~ 100nm size dispersed near the fusion line.

The Effect of the Crystalline Phase of Zirconia for the Dehydration of Iso-propanol (이소프로판올의 탈수반응에서 지르코니아 촉매의 결정상에 따른 영향)

  • Sim, Hye-In;Park, Jung-Hyun;Cho, Jun Hee;Ahn, Ji-Hye;Choi, Min-Seok;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.208-213
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    • 2013
  • Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

Minimization of Recombination Losses in 3D Nanostructured TiO2 Coated with Few Layered g-C3N4 for Extended Photo-response

  • Kang, Suhee;Pawar, Rajendra C.;Park, Tae Joon;Kim, Jin Geum;Ahn, Sung-Hoon;Lee, Caroline Sunyong
    • Journal of the Korean Ceramic Society
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    • v.53 no.4
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    • pp.393-399
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    • 2016
  • We have successfully fabricated 3D (3-dimensional) nanostructures of $TiO_2$ coated with a $g-C_3N_4$ layer via hydrothermal and sintering methods to enhance photoelectrochemical (PEC) performance. Due to the coupling of $TiO_2$ and $g-C_3N_4$, the nanostructures exhibited good performance as the higher conduction band of $g-C_3N_4$, which can be combined with $TiO_2$. To fabricate 3D nanostructures of $g-C_3N_4/TiO_2$, $TiO_2$ was first grown as a double layer structure on FTO (Fluorine-doped tin oxide) substrate at $150^{\circ}C$ for 3 h. After this, the $g-C_3N_4$ layer was coated on the $TiO_2$ film at $520^{\circ}C$ for 4 h. As-prepared samples were varied according to loading of melamine powder, with values of loading of 0.25 g, 0.5 g, 0.75 g, and 1 g. From SEM and TEM analysis, it was possible to clearly observe the 3D sample morphologies. From the PEC measurement, 0.5 g of $g-C_3N_4/TiO_2$ film was found to exhibit the highest current density of $0.12mA/cm^2$, along with a long-term stability of 5 h. Compared to the pristine $TiO_2$, and to the 0.25 g, 0.75 g, and 1 g $g-C_3N_4/TiO_2$ films, the 0.5 g of $g-C_3N_4/TiO_2$ sample was coated with a thin $g-C_3N_4$ layer that caused separation of the electrons and the holes; this led to a decreasing recombination. This unique structure can be used in photoelectrochemical applications.