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Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

Microscopic Study of Decomposition-Inhibition in Stabilized $ClO_2$ Gas in Skeletal Muscle of Rat (흰쥐 골격근에서 안정화 이산화염소(Stabilized $ClO_2$)의 부패억제에 관한 현미경적 연구)

  • Hwang, Kyu-Sung;Jeong, Moon-Jin;Jeong, Soon-Jeong;Ahn, Yong-Soon;Lim, Do-Seon
    • Applied Microscopy
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    • v.41 no.4
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    • pp.277-284
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    • 2011
  • This study was conducted to determine the antiseptic effect of stabilized chlorine dioxide (S-$ClO_2$) on muscle tissue of rats. Skeletal muscle of 8-week old Sprague-Dawley rats was used. Light and transmission electron microscopic findings were observed in the control group, which was not treated with stabilized chlorine dioxide, and in the experimental group, which was treated with a stabilized chlorine dioxide powder in aqueous solution. According to the LM and TEM observations, the day 1 control group showed the initiation of endomysium collapse resulting in an unclear boundary of muscle fibers, and partial collapse of the mitochondrial membranes. All endomysium had collapsed, and bacteria were observed among muscle fibers in the day 2 and later groups. Shapes of muscles were not distinguishable in day 3 or later groups. In contrast, the day 1 and 3 experimental groups revealed detailed structure of typical muscles, but partial collapse of the mitochondrial membranes was observed in the day 3 and later groups. Subsequently, connective tissues collapsed and structures in the shape of concentric circles were observed. In summary, the day 1 control group showed the initial collapse of tissues, and shapes were not distinguishable in the day 3 and later groups because most of the tissues had collapsed. In contrast, the day 3 experimental group showed partial collapse, but the overall shapes of muscles were maintained as time went on, confirming the antiseptic effect of stabilized chlorine dioxide on muscles.

THE EFFECTS OF SURFACE CONTAMINATION BY HEMOSTATIC AGENTS ON THE SHEAR BOND STRENGTH OF COMPOMER (지혈제 오염이 콤포머의 전단결합강도에 미치는 영향)

  • Heo, Jeong-Moo;Kwak, Ju-Seog;Lee, Hwang;Lee, Su-Jong;Im, Mi-Kyung
    • Restorative Dentistry and Endodontics
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    • v.27 no.2
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    • pp.150-157
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    • 2002
  • One of the latest concepts in bonding are "total etch", in which both enamel and dentin are etched with an acid to remove the smear layers, and "wet dentin" in which the dentin is not dry but left moist before application of the bonding primer Ideally the application of a bonding agent to tooth structure should be insensitive to minor contamination from oral fluids. Clinically, contaminations such as saliva, gingival fluid, blood and handpiece lubricant are often encountered by dentists during cavity preparation. The aim of this study was to evaluate the effect of contamination by hemostatic agents on shear bond strength of compomer restorations. One hundred and ten extracted human maxillary and mandibular molar teeth were collected. The teeth were removed soft tissue remnant and debris and stored in physiologic solution until they were used. Small flat area on dentin of the buccal surface were wet ground serially with 400, 800 and 1200 abrasive papers on automatic polishing machine. The teeth were randomly divided into 11 groups. Each group was conditioned as follows : Group 1: Dentin surface was not etched and not contaminated by hemostatic agents. Group 2: Dentin surface was not etched but was contaminated by Astringedent$^{\circledR}$(Ultradent product Inc., Utah, U.S.A.) Group 3: Dentin surface was not etched but was contaminated by Bosmin$^{\circledR}$(Jeil Pharm, Korea.). Group 4: Dentin surface was not etched but was contaminated by Epri-dent$^{\circledR}$(Epr Industries, NJ, U.S.A.). Group 5: Dentin surface was etched and not contaminated by hemostatic agents. Group 6: Dentin sorface was etched and contaminated by Astringedent$^{\circledR}$. Group 7 : Dentin surface was etched and contaminated by Bosmin$^{\circledR}$. Group 8: Dentin surface was etched and contaminated by Epri-dent$^{\circledR}$. Group 9: Dentin surface was contaminated by Astringedent$^{\circledR}$. The contaminated surface was rinsed by water and dried by compressed air. Group 10: Dentin surface was contaminated by Bosmin$^{\circledR}$. The contaminated surface was rinsed by water and dried by compressed air. Group 11 : Dentin surface was contaminated by Epri-dent$^{\circledR}$. The contaminated surface was rinsed by water and dried by compressed air. After surface conditioning, F2000$^{\circledR}$ was applicated on the conditoned dentin surface The teeth were thermocycled in distilled water at 5$^{\circ}C$ and 55$^{\circ}C$ for 1,000 cycles. The samples were placed on the binder with the bonded compomer-dentin interface parallel to the knife-edge shearing rod of the Universal Testing Machine(Zwick Z020, Zwick Co., Germany) running at a cross head speed or 1.0 mm/min. Group 2 showed significant decrease in shear bond strength compared with group 1 and group 6 showed significant decrease in shear bond strength compared with group 5. There were no significant differences in shear bond strength between group 5 and group 9, 10 and 11.

Hydrothermal Alteration Related to Cretaceous Felsic Magmatism in the Seongsan Dickite Deposits, Korea; Estimation of Ore - Forming Temperature and aNa+/aK+ Ratio of the Hydrothermal Fluid (성산딕카이트광상에서의 백악기산성마그마티즘에 관련된 열수변질작용 ; 광상형성온도의 측정 및 열수용액의 aNa+/aK+)

  • Kim, In Joon
    • Economic and Environmental Geology
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    • v.25 no.3
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    • pp.259-273
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    • 1992
  • The Seongsan mine is one of the largest dickite deposits in the southwestern part of the Korean Peninsula. The main constithent minerals of the ore are dickite and quartz with accessory alunite, kaolinite and sericite. The geology around the Seongsan mine consists mainly of the late Cretaceous felsic volcanic rocks. In the studied area, these rocks make a synclinal structure with an axis of E-W direction plunging to the east. Most of the felsic volcanic rocks have undergone extensive hydrothermal alteration. The hydrothermally altered rocks can be classified into the following zones: Dickite, Dickite-Quartz, Quartz, Sericite, Albite and Chlorite zones, from the center to the margin of the alteration mass. Such zonal arrangement of altered rocks suggests that the country rocks, most of which are upper part of the rhyolite and welded tuff, were altered by strongly acid hydrothermal solutions. It is reasonable to consider that initial gas and solution containing $H_2S$ and other compounds were oxidized near the surface, and formed hydrothermal sulfuric acid solutions. The mineralogical and chemical changes of the altered rocks were investigated using various methods, and chemical composition of fifty-six samples of the altered rocks were obtained by wet chemical analysis and X.R.F. methods. On the basis of these analyses, it was found that some components such as $SiO_2$, $Al_2O_3$, $Fe_2O_3$, CaO, MgO, $K_2O$, $Na_2O$ and $TiO_2$ were mobilized considerably from the original rocks. The formation temperature of the deposits was estimated as higher than $200^{\circ}C$ from fluid inclusion study of samples taken from the Quartz zone. On the basis of the chemical composition data on rocks and minerals and estimated temperatures, the hydrothermal solutions responsible for the formation of the Seongsan dickite deposits were estimated to have the composition: $m_{K^+}=0.003$, $m_{Na^+}=0.097$, $m_{SiO_2(aq.)}=0.008$ and pH=5.0, here "m" represents the molality (mole/kg $H_2O$).

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Microwave Irradiation as a Way to Reutilize the Recovered Struvite Slurry and to Enhance System Performance (회수된 MAP 슬러리의 재이용과 공정효율 향상을 위한 도구로서의 극초단파 조사)

  • Cho, Joon-Hee;Lee, Jin-Eui;Ra, Chang-Six
    • Journal of Animal Science and Technology
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    • v.51 no.4
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    • pp.337-342
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    • 2009
  • The feasibility of reutilization of magnesium ammonium phosphate (MAP) or struvite slurry recovered from the process through microwave irradiation was studied in this experiment. For this purpose, 4 different operations were performed with or without Mg source addition and different levels of MAP recycled in a batch reactor. Dissolution rate of MAP, ${NH_4}^+$ elimination pattern and physicochemical changes of MAP during microwave irradiation were also studied. The result showed that only 33% orthophosphate ($PO_4-P$) and 27% $NH_4-N$ removal occurred without adding any external Mg source (run A), whereas 87% $PO_4-P$ and 40% $NH_4-N$ removed when 1.0 M ratio of $MgCl_2$ (run B) was added based on $PO_4-P$ in influent. Although the addition of 1.0 molar ratio of microwave irradiated MAP (Run C) removed lower $PO_4-P$ and $NH_4-N$ than 1.0 M $MgCl_2$ (run B), $PO_4-P$ removal was double when compared with no Mg addition (run A). Addition of half MAP and half $MgCl_2$ (run D) showed the similar removal efficiency (88% $PO_4-P$ and 35% $NH_4-N$) with sole $MgCl_2$ addition (run B). Based on these results, the reutilization of MAP irradiated by microwave would be a feasible way to enhance the removal efficiencies of N and P, as well as curtail the Mg chemical usage. Track study showed that $NH_4-N$ gradually increased at initial stage of microwave irradiation of MAP, and then started eliminating from liquor as temperature increased over $45^{\circ}C$. Dissolution rate of ${PO_4}^{-3}$ during microwave irradiation was proportional to the initial MAP concentration, having $0.0091x^{0.6373}$ mg/sec. It was found from the scanning electron microscope (SEM) study that physical structure of MAP crystal started breaking down into small cube granules within very short time by electromagnetic vibration force during microwave irradiation and then gradually melted down into solution.

IN VITRO STUDY OF DEMINERALIZATION INHIBITION EFFECT AND FLUORIDE UPTAKE INTO ADJACENT TEETH OF LIGHT-CURED FLUORIDE-RELEASING RESTORATIVES (수종의 불소방출 수복재의 탈회억제 효과 및 불소침투에 관한 연구)

  • Kim, Song-Yi;Choi, Sung-Chul;Kim, Kwang-Chul;Choi, Yeong-Chul;Park, Jae-Hong
    • Journal of the korean academy of Pediatric Dentistry
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    • v.37 no.3
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    • pp.288-297
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    • 2010
  • The purpose of this study was to evaluate the effect of light cured fluoride-releasing materials on the inhibition of demineralization. In addition, the pattern of fluoride uptake of adjacent tooth structure was analyzed with EPMA. Eighty intact premolars were restored with $Filtek^{TM}$ Z250(control group, composite), Fuji Filling $LC^{TM}$(RMGI), Dyract $AP^{(R)}$ (compomer) and Beautifil II(giomer). Restored teeth were stored in distilled water for 30 days. Then sixty teeth(n=15) were exposed to demineralizing solution(pH 4.3). Demineralized teeth were bisected and polished. The specimens were observed with confocal laser scanning microscope. The depth of outer lesion and the thickness of inhibition zone were measured. Remained twenty teeth(n=5) were bisected for fluoride uptake analysis. The fluoride analysis were taken at enamel-restoration interface and dentin-restoration interface by electron probe micro-analyzer. The results are as follows: 1. The depth of outer lesion of Fuji Filling $LC^{TM}$ Dyract AP, Beautifil II was shallower than that of $Filtek^{TM}$ Z250 at the margin of restoration(p<0.05). 2. The thickness of caries inhibition zone of Fuji Filling $LC^{TM}$, Dyract AP, Beautifil II was greater than that of $Filtek^{TM}$ Z250 at the margin of restoration(p<0.05). 3. Fuji Filling $LC^{TM}$, Dyract AP, Beautifil II groups showed the greater fluoride uptake into enamel and dentine around restoration than $Filtek^{TM}$ Z250 group. 4. In dentin the difference of fluoride concentration were greater than in enamel, and Dyract AP showed the greatest fluoride concentration in dentin.

An Experimental Study of Corrosion Characteristics and Compounds by Corrosion Factors in Iron Artifacts (철제유물 부식인자에 대한 부식양상 및 부식화합물 실험 연구)

  • Park, Hyung Ho;Lee, Jae Sung;Yu, Jae Eun
    • 보존과학연구
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    • s.33
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    • pp.33-43
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    • 2012
  • The corrosion phenomena of the iron artifacts was studied by morphology observation and instrumental analysis(EDS, XRD, Raman) with various corrosion factors in oder to verify to confirm the danger of corrosion factors. Corrosion compounds were collected by depositing pure Fe powder(99%) into a HCl, $HNO_3$, $H_2SO_4$, and $H_2O$ solution which contained the corrosion factors. Stereoscopic-microscope observations were then conducted determine the colors and shapes of the collected corrosion compounds, and SEM-EDS analysis was conducted to confirm the corrosion factors and the growth of these compounds. X-ray diffraction (XRD), Raman analyses were conducted to examine the crystal structure and compositions of the created corrosion compounds. The results of the experiment revealed that corrosion speed was faster in an acidic environment and corrosion of HCl and $H_2SO_4$ was greater than that of $HNO_3$. The corrosion compounds of HCl grew into a needle or chestnut-like shape after being affected by Cl- ion, and XRD and Raman analyses detected goethite and lepidocrocite. The corrosion compounds of $H_2SO_4$ was affected by S ion and grew into a slender-needle-like or cylindrical shape, and the XRD and Raman analyses detected goethite and lepidocrocite. The corrosion compounds of $HNO_3$ grew into a spherical or plate-like shape after being affected by O ion and the XRD and Raman analyses detected magnetite and lepidocrocite. Although the corrosion compounds of $H_2O$ grew into a spherical or plate-like shape after being affected by O ion, most of them were observed to have had spherical shapes, and the XRD and Raman analyses failed to detect corrosion compounds in them. It was found in the study that corrosion characteristics and compounds are diversely displayed according to the corrosion factor.

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CNT-Ni-Fabric Flexible Substrate with High Mechanical and Electrical Properties for Next-generation Wearable Devices (차세대 웨어러블 디바이스를 위한 높은 기계적/전기적 특성을 갖는 CNT-Ni-Fabric 유연기판)

  • Kim, Hyung Gu;Rho, Ho Kyun;Cha, Anna;Lee, Min Jung;Ha, Jun-Seok
    • Journal of the Microelectronics and Packaging Society
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    • v.27 no.2
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    • pp.39-44
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    • 2020
  • Recently, numerous researches are being conducted in flexible substrate to apply to wearable devices. Particularly, Conductive substrate researches that can implement the wearable devices on clothing are massive. In this study, we formed fiber substrate spraying CNT and Pd mixed solution on it and plated metal layer with electroless plating. Used SEM equipment and EDS analysis to analysis structure of the plated fiber substrate and discovered Ni layer was created. For check electrical properties, mapping was performed to check surface resistance and distribution of resistance of electroless plated fiber substrate with 4-point probe. It was confirmed that conductivity was improved as the duration of electroless plating was increased, and it was found that distribution of resistance by surface location was uniform. Changes in resistance due to mechanical stress were measured through tensile, bending, and twisting tests. As a result, it was confirmed that resistance change of flexible substrate gradually disappeared as plating time increased. Using UTM (Universal testing machine), it was analyzed mechanical properties of the electroless plated substrate with respect to changes in plating time were improved. In the case of conductive fiber substrate in which electroless plating was performed for 2 hours, tensile strength was increased by 16 MPa than fiber substrate. Based on these results, we found that Ni-CNT-Fabric flexible substrate is adequate for clothing-intergrated conductive substrate and we positively expect that this experiment shows flexible substrate can adapt to and develop not only a wearable device technology but also other fields needing flexibility such as battery, catalyst and solar cell.

APPLICATION OF ACIDIC PRIMER FOR ORTHODONTIC ADHESIVE SYSTEM (Acidic primer를 이용한 교정용 브라켓 접착의 전단결합강도)

  • Kim, Jin-Hee;Jin, Hun-Hee;Oh, Jang-Kyun
    • The korean journal of orthodontics
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    • v.31 no.1 s.84
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    • pp.137-147
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    • 2001
  • Acidic primer is the bonding agent which combines the conditioning and priming agent into the single solution and was originally developed for the dentin bonding system. It is less harmful to the tooth structure and more convenient to manipulate than the traditional etching procedure. The Purpose of this study is to evaluate the shear bond strength of various bonding materials when the enamel is treated with acidic primer for the bracket bonding procedure. Fifty recently extracted human premolars were randomly separated into five groups -Group I using Clearfil Liner Bond 2 adhesive system to the enamel treated with acidic primer, Group II using Transbond XT adhesive system to the enamel treated with acidic primer, Group III using panavia 21 adhesive system to the enamel treated with acidic primer, Group IV using Fuji-Ortho LC adhesive system to the enamel treated with acidic primer, Group V using Transbond XT adhesive system to the enamel treated with 37$\%$ phosphoric acid. The shear bond strength was measured with Instron universal testing machine after storing in $37^{\circ}C$ water bath for 48 hours. After debonding, the teeth and brackets were examined under scanning electron microscope (SEM) and assessed with the adhesive remnant index (ARI). The results were as follows : 1. There were no significant differences in shear bond strength between group III ($8.69{\pm}2.72MPa$), group IV (9.7 ± 3.16 MPa), and group V ($10.48{\pm}2.60MPa$) (p>0.05). 2. The shear bond strength of group III and group IV was significantly higher than that of group I ($1.09{\pm}0.53MPa$), and Group II ($2.70{\pm}1.46MPa$) (p<0.05). 3. The ARI of group IV ($2.1{\pm}1.1$) and group V ($2.9{\pm}0.3$) was significantly higher than that of group I ($0.2{\pm}0.4$), group II ($0.3{\pm}0.9$) and group III ($0.2{\pm}0.4$) (p<0.05). 4. There were no significant difference between the ARI of group IV and group V (p>0.05). This result suggests that the combination of acidic primer and some bonding adhesive can provide sufficient shear bond strength for clinical orthodontics.

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A bilayer diffusion barrier of atomic layer deposited (ALD)-Ru/ALD-TaCN for direct plating of Cu

  • Kim, Soo-Hyun;Yim, Sung-Soo;Lee, Do-Joong;Kim, Ki-Su;Kim, Hyun-Mi;Kim, Ki-Bum;Sohn, Hyun-Chul
    • 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.

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