• Restorative Dentistry and Endodontics
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• v.48 no.1
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• pp.3.1-3.14
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• 2023

Objectives: This study evaluated the effect of different nanoparticulated zinc oxide (nano-ZnO) and conventional-ZnO ratios on the physicochemical properties of calcium aluminate cement (CAC). Materials and Methods: The conventional-ZnO and nano-ZnO were added to the cement powder in the following proportions: G1 (20% conventional-ZnO), G2 (15% conventional-ZnO + 5% nano-ZnO), G3 (12% conventional-ZnO + 3% nano-ZnO) and G4 (10% conventional-ZnO + 5% nano-ZnO). The radiopacity (R_ad), setting time (S_et), dimensional change (D_c), solubility (S_ol), compressive strength (C_st), and pH were evaluated. The nano-ZnO and CAC containing conventional-ZnO were also assessed using scanning electron microscopy, transmission electron microscopy, and energy-dispersive X-ray spectroscopy. Radiopacity data were analyzed by the 1-way analysis of variance (ANOVA) and Bonferroni tests (p < 0.05). The data of the other properties were analyzed by the ANOVA, Tukey, and Fisher tests (p < 0.05). Results: The nano-ZnO and CAC containing conventional-ZnO powders presented particles with few impurities and nanometric and micrometric sizes, respectively. G1 had the highest Rad mean value (p < 0.05). When compared to G1, groups containing nano-ZnO had a significant reduction in the S_et (p < 0.05) and lower values of D_c at 24 hours (p < 0.05). The C_st was higher for G4, with a significant difference for the other groups (p < 0.05). The S_ol did not present significant differences among groups (p > 0.05). Conclusions: The addition of nano-ZnO to CAC improved its dimensional change, setting time, and compressive strength, which may be promising for the clinical performance of this cement.

• 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 (CO₃^2-) and sulfate (SO₄^2-) 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.

• 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.

• Journal of the Mineralogical Society of Korea
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• v.20 no.1 s.51
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• pp.47-60
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• 2007

While sedimentological researches on Western coastal tidal flats of Korea have been much pelformed previously, mineralogical and biogeochemical studies are beginning to be studied. The objectives of this study were to investigate mineralogical characteritics of the inter-tidal flat sediments and to explore phase transformation of iron(oxyhydr)oxides and biomineralization by metal-reducing bacteria enriched from the inter-tidal flat sediments from Muan, Jeollanam-do, Korea. Inter-tidal flat sediment samples were collected in Chungkye-myun and Haeje-myun, Muan-gun, Jeollanam-do. Particle size analyses were performed using the pipette method and sedimentation method. The separates including sand, silt and clay fractions were examined by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), and X-ray diffiaction (XRD). After enriching the metal-.educing bacteria from the into,-tidal flat sediments, the bacteria were used to study phase transformation of the synthesized iron (oxyhydr)oxides and iron biomineralization using lactate or glucose as the electron donors and Fe(III)-containing iron oxides as the electron accepters. Mineralogical studies showed that the sediments of tidal flats in Chung]rye-myun and Haeje-myun consist of quartz, plagioclase, microcline, biotite, kaolinite and illite. Biogeochemical researches showed that the metal-reducing bacteria enriched from the inter-tidal flat sediments reduced reddish brown akaganeite and mineralized nanometer-sized black magnetite. The bacteria also reduced the reddish brown ferrihydrite into black amorphous phases and reduced the yellowish goethite into greenish with formation of nm-sized phases. These results indicate that microbial Fe(III) reduction may play one of important roles in iron and carbon biogeochemistry as well as iron biomineralization in subsurface environments.

• Restorative Dentistry and Endodontics
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• v.35 no.2
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• pp.80-87
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• 2010

The purpose of this study was to compare the different canal irrigation methods to prevent the formation of precipitate between sodium hypochlorite (NaOCl) and chlorhexidine (CHX). Extracted 50 human single-rooted teeth were used. The root canals were instrumented using NiTi rotary file (Profile .04/#40) with 2.5% NaOCl and 17% EDTA as irrigants. Teeth were randomly divided into four experimental groups and one control group as follows; Control group: 2.5% NaOCl only, Group 1: 2.5% NaOCl + 2% CHX, Group 2: 2.5% NaOCl + paper points + 2% CHX, Group 3: 2.5% NaOCl + preparation with one large sized-file + 2% CHX, Group 4: 2.5% NaOCl +95% alcohol+ 2% CHX. The teeth were split in bucco-lingual aspect and the specimens were observed using Field Emission Scanning Electron Microscope. The percentages of remaining debris and patent dentinal tubules were determined. Statistical analysis was performed with one-way analysis of variance (ANOVA). Energy Dispersive x-ray Spectroscopy was used for analyzing the occluded materials in dentinal tubule for elementary analysis. There were no significant differences in percentage of remaining debris and patent tubules between all experimental groups at all levels (p > .05). In elementary analysis, the most occluded materials in dentinal tubule were dentin debris. NaOCl/CHX precipitate was detected in one tooth specimen of Group 1. In conclusion, there were no significant precipitate on root canal, but suspected material was detected on Group 1. The irrigation system used in this study could be prevent the precipitate formation.

• Journal of dental hygiene science
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• v.16 no.3
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• pp.235-241
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• 2016

This study was conducted to provide basic understanding regarding possible enamel erosion by three kinds of fist-aid antipyretic and analgesic medicines over a period of time, with comparison and analysis of the resulting deciduous teeth surface and microhardness changes. The analysis was performed using energy dispersive X-ray spectroscopy (EDX) and scanning electron microscope (SEM) to examine the surface erosion and changes. The Kruskal-Wallis test show differences in surface erosion and changes after 3, 5 and 8 days of treatment as well as before and after the treatment in each group. According to the results, there was no significant difference in the early deciduous teeth enamel surface microhardness (p>0.01). However there were signigicant changes after 3, 5, and 8 days (p<0.01). Calcim (Ca) and phosphorous (P) analysis using EDX showed significant differences in the enamel characteristics according to each tissue area after 8 days (p<0.05), but there was no significant difference in any of the areas for P content (p>0.05). In the surface observation with the SEM treatment with Children's Tylenol$^{(R)}$ tablet, which has the lowest pH, looked the roughest, followed by Brufen syrup for children and Children's Tylenol$^{(R)}$ suspension. Based on these results, it should be considered that antipyretic and analgesic medicines for children, which have lower pH values, may cause tooth erosion. Hence, it is necessary to give special attention to oral hygiene in young children or infants by brushing their teeth after such drugs are administered.

• 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.

• Korean Journal of Heritage: History & Science
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• v.55 no.3
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• pp.120-129
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• 2022

The purpose of this study is to analyze the chemical composition of smalt pigments used in 10 large Buddhist paintings in the Joseon Dynasty using energy dispersive X-ray spectroscopy, and to clarify the material and characteristics by observing morphological characteristics using polarized light microscopy and a scanning electron microscope. Through chemical composition analysis, the smalt of all 10 large Buddhist paintings is judged to be potash glass using SiO₂ as a former and K₂O as a flux. In addition to the components related to cobalt ore used as a colorant, the paintings were found to contain high levels of As₂O₃, BaO, and PbO. The smalt particles did not have specific forms, and were blue in color, with various chromaticity. In some particles, conchoidal fracture, spherical bubbles, and impurities were observed. Through backscattered electron images, it was found that the smalt from paintings produced in the early 18th century AD had a high level of As, but the smalt from paintings produced from the mid-18th century AD onwards exhibited various contrast differences from particle to particle, and there was smalt with high levels of As, Ba, and Pb. Through the above results, the large Buddhist paintings in the Joseon Dynasty are divided into three smalt types. Type A is a type with high As₂O₃, type B is a type with high BaO, and type C is a type with high PbO. Looking at the three types of smalt pigments by the period of production, although some in-between periods were not detected, type A was confirmed to have been used from 1705 to 1808, while type B and type C were shown to have appeared in 1750 and used until 1808. This reveals that only one type of smalt was used until the early 18th century AD, and from the middle of the 18th century AD, several types of smalt were mixed and used in one large Buddhist painting. Studies such as this research are expected to provide insights into the characteristics of the smalt pigments used to produce large Buddhist paintings at the time.

• Restorative Dentistry and Endodontics
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• v.22 no.1
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• pp.1-33
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• 1997

The objective of this study was to analyze the in vitro and in vivo corrosion products of low and high copper amalgams. The four different types of amalgam alloy used in this study were Fine cut, Caulk spherical, Dispersalloy, and Tytin. After each amalgam alloy and Hg were triturated according to the directions of the manufacturer by means of the mechanical amalgamator(Amalgam mixer. Shinhung Co. Korea), the triturated mass was inserted into a cylindrical metal mold which was 12mm in diameter and 10mm in height. The mass was condensed by 150Kg/cm compressive force. The specimen was removed from the mold and aged at room temperature for about seven days. The standard surface preparation was routinely carried out by emery paper polishing under running water. In vitro amalgam specimens were potentiostatically polarized ten times in a normal saline solution at $37^{\circ}C$(potentiostat : HA-301. Hukuto Denko Corp. Japan). Each specimen was subjected to anodic polarization scan within the potential range -1700mV to+400mV(SCE). After corrosion tests, anodic polarization curves and corrosion potentials were obtained. The amount of component elements dissolved from amalgams into solution was measured three times by ICP AES(Inductive Coupled Plasma Atomic Emission Spectrometry: Plasma 40. Perkim Elmer Co. U.S.A.). The four different types of amalgam were filled in occlusal and buccal class I cavities of four human 3rd molars. After about five years the restorations were carefully removed after tooth extraction to preserve the structural details including the deteriorated margins. The occlusal surface, amalgam-tooth interface and the fractured surface of in vivo amalgam corrosion products were analyzed. In vivo and in vitro amalgam specimens were examined and analyzed metallographically by SEM(Scanning Electron Microscope: JSM 840. Jeol Co. Japan) and EDAX(Energy Dispersive Micro X-ray Analyser: JSM 840. Jeol Co. Japan). 1. The following results are obtained from in vitro corrosion tests. 1) Corrosion potentials of all amalgams became more noble after ten times passing through the in vitro corrosion test compared to first time. 2) After times through the test, released Cu concentration in saline solution was almost equal but highest in Fine cut. Ag and Hg ion concentration was highest in Caulk spherical and Sn was highest in Dispersalloy. 3) Analyses of surface corrosion products in vitro reveal the following results. a)The corroded surface of Caulk spherical has Na-Sn-Cl containing clusters of $5{\mu}m$ needle-like crystals and oval shapes of Sn-Cl phase, polyhedral Sn oxide phase. b)In Fine cut, there appeared to be a large Sn containing phase, surrounded by many Cu-Sn phases of $1{\mu}m$ granular shapes. c)Dispersalloy was covered by a thick reticular layer which contained Zn-Cl phase. d)In Tytin, a very thin, corroded layer had formed with irregularly growing Sn-Cl phases that looked like a stack of plates. 2. The following results are obtained by an analysis of in vivo amalgam corrosion products. 1) Occlusal surfaces of all amalgams were covered by thick amorphous layers containing Ca-P elements which were abraded by occlusal force. 2) In tooth-amalgam interface, Ca-P containing products were examined in all amalgams but were most clearly seen in low copper amalgams. 3) Sn oxide appeared as a polyhedral shape in internal space in Caulk spherical and Fine cut. 4) Apical pyramidal shaped Sn oxide and curved plate-like Sn-Cl phases resulted in Dispersalloy. 5) In Tytin, Sn oxide and Sn hydroxide were not seen but polyhedral Ag-Hg phase crystal appeared in internal space which assumed a ${\beta}_l$ phase.