Kim, Daesup;Lim, Chaehun;Kim, Seokjin;Lee, Young-Seak
Applied Chemistry for Engineering
/
v.33
no.5
/
pp.496-501
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2022
In this study, an anode material for lithium secondary batteries was manufactured using petroleum-based residual oil, which is a petroleum refining by-product. Among petroleum-based residual oils, pyrolysis fuel oil (PFO), fluidized catalyst cracking-decant oil (FCC-DO), and vacuum residue (VR) were used as carbon precursors. The physicochemical characteristics of petroleum-based residual oil were confirmed through Matrix-assisted laser desorption/ionization Time-of-Flight (MALDI-TOF) and elemental analysis (EA), and the structural characteristics of anode materials manufactured from residual oil were evaluated using X-ray crystallography (XRD) and Raman spectroscopic techniques. VR was found to contain a wide range of molecular weight distributions and large amounts of impurities compared to PFO and FCC-DO, and PFO and FCC-DO exhibited almost similar physicochemical characteristics. From the XRD analysis results, carbonized PFO and FCC-DO showed similar d002 values. However, it was confirmed that FCC-DO had a more developed layered structure than PFO in Lc (Length of a and c axes in the crystal system) and La values. In addition, FCC-DO showed the best cycle characteristics in electrochemical characteristics evaluation. According to the physicochemical and electrochemical results of the petroleum-based residual oil, FCC-DO is a better carbon precursor for a lithium secondary battery than PFO and VR.
The studies were carried out to disclose the physical and chemical properties of sericin fraction obtained from silk cocoon shells and its characteristics of swelling and solubility. The following results were obtained. 1. The physical and chemical properties of sericin fraction. 1) In contrast to the easy water soluble sericin, the hard soluble sericin contains fewer amino acids include of polar side radical while the hard soluble amino acid sach as alanine and leucine were detected. 2) The easy soluble amino acids were found mainly on the outer part of the fibroin, but the hard soluble amino acids were located in the near parts to the fibroin. 3) The swelling and solubility of the sericin could be hardly assayed by the analysis of the amino acid composition, and could be considered to tee closely related to the compound of the sericin crystal and secondary structure. 4) The X-ray patterns of the cocoon filament were ring shape, but they disappeared by the degumming treatment. 5) The sericin of tussah silkworm (A. pernyi), showed stronger circular patterns in the meridian than the regular silkworm (Bombyx mori). 6) There was no pattern difference between Fraction A and B. 7) X-ray diffraction patterns of the Sericin 1, ll and 111 were similar except interference of 8.85A (side chain spacing). 8) The amino acids above 150 in molecular weight such as Cys. Tyr. Phe. His. and Arg. were not found quantitatively by the 60 minutes-hydrolysis (6N-HCI). 9) The X-ray Pattern of 4.6A had a tendency to disappear with hot-water, ether, and alcohol treatment. 10) The partial hydrolysis of sericin showed a cirucular interference (2A) on the meridian. 11) The sericin pellet after hydrolysis was considered to be peptides composed with specific amino acids. 12) The decomposing temperature of Sericin 111 was higher than that of Sericin I and II. 13) Thermogram of the inner portioned sericin of the cocoon shell had double endothermic peaks at 165$^{\circ}C$, and 245$^{\circ}C$, and its decomposing temperature was higher than that of other portioned sericin. 14) The infrared spectroscopic properties among sericin I, II, III and sericin extracted from each layer portion of the cocoon shell were similar. II. The characteristics of seriein swelling and solubility related with silk processing. 1) Fifteen minutes was required to dehydrate the free moisture of cocoon shells with centrifugal force controlled at 13${\times}$10$^4$ dyne/g at 3,000 R.P.M. B) It took 30 minutes for the sericin to show positive reaction with the Folin-Ciocaltue reagent at room temperature. 3) The measurable wave length of the visible radiation was 500-750m${\mu}$, and the highest absorbance was observed at the wave length of 650m${\mu}$. 4) The colorimetric analysis should be conducted at 650mu for low concentration (10$\mu\textrm{g}$/$m\ell$), and at 500m${\mu}$ for the higher concentration to obtain an exact analysis. 5) The absorbing curves of sericin and egg albumin at different wave lengths were similar, but the absorbance of the former was slightly higher than that of the latter. 6) The quantity of the sericin measured by the colorimetric analysis, turned out to be less than by the Kjeldahl method. 7) Both temperature and duration in the cocoon cooking process has much effect on the swelling and solubility of the cocoon shells, but the temperature was more influential than the duration of the treatment. 8) The factorial relation between the temperature and the duration of treatment of the cocoon cooking to check for siricin swelling and solubility showed that the treatment duration should be gradually increased to reach optimum swelling and solubility of sericin with low temperature(70$^{\circ}C$) . High temperature, however, showed more sharp increase. 9) The more increased temperature in the drying of fresh cocoons, the less the sericin swelling and solubility were obtained. 10) In a specific cooking duration, the heavier the cocoon shell is, the less the swelling and solubility were obtained. 11) It was considered that there are differences in swelling or solubility between the filaments of each cocoon layer. 12) Sericin swelling or solubility in the cocoon filament was decreased by the wax extraction.. 13) The ionic surface active agent accelerated the swelling and solubility of the sericin at the range of pH 6-7. 14) In the same conditions as above, the cation agent was absorbed into the sericin. 15) In case of the increase of Ca ang Mg in the reeling water, its pH value drifted toward the acidity. 16) A buffering action was observed between the sericin and the water hardness constituents in the reeling water. 17) The effect of calcium on the swelling and solubility of the sericin was more moderate than that of magnecium. 18) The solute of the water hardness constituents increased the electric conductivity in the reeling water.
Passive fitting of meso-structure and super-structures is a predominant requirement for the longevity and clinical success of osseointegrated dental implants. However, precision and passive fitting has been unpredictable with conventional methods of casting as well as for corrective techniques. Alternative to conventional techniques, electro discharge machining(EDM) is an advanced method introduced to dental technology to improve the passive fitting of implant prosthesis. In this technique material is removed by melting and vaporization in electric sparks. Regarding the efficacy of EDM, the application of this technique induces severe surface morphological and elemental alterations due to the high temperatures developed during machining, which vary between $10,000{\sim}20,000^{\circ}C$. The aim of this study was to investigate the morphological and elemental alterations induced by EDM process of casting dental gold alloy and non-precious alloy used for the production of implant-supported prosthesis. A conventional clinical dental casting alloys were used for experimental specimens patterns, which were divided in three groups, high fineness gold alloy(Au 75%, HG group), low fineness gold alloy(Au 55%, LG group) and nonprecious metal alloy(Ni-Cr, NP group). The UCLA type plastic abutment patterns were invested with conventional investment material and were cast in a centrifugal casting machine. Castings were sandblasted with $50{\mu}m\;Al_2O_3$. One casting specimen of each group was polished by conventional finishing(HGCON, LGCON, NPCON) and one specimen of each group was subjected to EDM in a system using Cu electrodes, kerosene as dielectric fluid in 10 min for gold alloy and 20 min for Ni-Cr alloy(HGEDM. LGEDM, NOEDM). The surface morphology of all specimens was studied under an energy dispersive X-ray spectrometer (EDS). The quantitative results from EDS analysis are presented on the HGEDM and LGEDM specimens a significant increase in C and Cu concentrations was found after EDM finishing. The different result was documented for C on the NPEDM with a significant uptake of O after EDM finishing, whereas Al, Si showed a significant decrease in their concentrations. EDS analysis showed a serious uptake of C and Cu after the EDM procedure in the alloys studied. The C uptake after the EDM process is a common finding and it is attributed to the decomposition of the dielectric fluid in the plasma column, probably due to the development of extremely high temperatures. The Cu uptake is readily explained from the decomposition of Cu electrodes, something which is also a common finding after the EDM procedure. However, all the aforementioned mechanisms require further research. The clinical implication of these findings is related with the biological and corrosion resistance of surfaces prepared by the EDM process.
Basic studies have been conducted regarding the crystal formation of hydroxyapatite which was produced in the treatment process of phosphate-containing wastewater using calcium ions as the precipitating agent for its employment as the material for artificial bones. The precipitation of hydroxyapatite were conducted in the synthetic solution which simulating human body fluid for its increased applicability. Ca($NO_3$)$_2$$.$$4H_2$O and ($NH_4$)$_2$$HPO_4$ were employed for the precipitation of hydroxyapatite and its composition was analyzed after drying at 80oC. The thermal behavior of precipitate was investigated by examining the change in its crystalline structure according to the sintering temperature. DTA/TG analysis showed that the escape of moisture from the precipitate occurred at ca. $100^{\circ}C$ and the decomposition of ammonia and the evaporation of lattice water were brought about at around $250^{\circ}C$. X-ray diffraction analysis indicated that the thermally treated precipitate consisted mainly of hydroxyapatite. For dried precipitate, the bonds in the component materials which used for the precipitate formation were observed by FT-IR, and after thermal treatment the major bonds in the precipitate were shown to be $OH^{-}$, $PO_4^{3-}$ , and $CO_3^{ 2-}$ , which were main comprising bonds of hydroxyapatite.
Objective of this research was to evaluate optimal conditions of arsenic adsorption in water by zero-valent iron (ZVI). Batch experiment showed that adsorption of arsenic by ZVI followed a Langmuir isotherm model. The masses of As(V) adsorbed onto ZVI were increased as decreasing pH of the reacting solution (pH 3: 2.05, pH 5: 1.82, pH 7: 1.24, pH 9: 1.03 mg As/g $Fe^0$) and as increasing the temperature ($15^{\circ}C$ : 1.59, $25^{\circ}C$ : 1.81, 35 : $1.93^{\circ}C$ mg As/g $Fe^0$). The SEM and EDS (energy dispersive X-ray spectrometer) analysis of morphology and structure of ZVI before and after reacting with arsenic in water revealed that a relatively smooth and large surface of ZVI was transformed into a coarse and small surface particle after the reaction. The EDS spectra on the chemical composition of ZVI demonstrated that arsenic was incorporated into ZVI by adsorption mechanism. The XRD analysis also identified that the only peak for $Fe^0$ in the ZVI before the reaction and confirmed that $Fe^0$ was transformed into $Fe_2O_3$ and FeOOH, and As into $FeAsO_4{\cdot}2H_2O$.
This study examined the changes of microstructural compositions in cement matrix according to the depth from the surface of a reinforced concrete (RC) column exposed to fire. The RC column was exposed to a standard fire for 180 minutes. After the fire test, core samples passing through the column section were obtained. Using the core samples, the remaining fractions of calcium-silicate-hydrates (C-S-H) and calcium hydroxide in cement matrix at the surface, the depth of 40 mm and 80 mm and the center (175 mm) were examined using thermal gravimetric analysis (TGA) and X-ray diffraction analysis (XRDA). Using nuclear magnetic resonance (NMR) technique, the silicate polymerization of C-S-H in cement matrix was also evaluated. The experimental results indicated that the amount of C-S-H loss at the center of column experiencing the transferred fire temperature of $236^{\circ}C$ has been underestimated as the TGA results showed the highest C-S-H contents are located at the depth of 80 mm, where the transferred fire temperature is $419^{\circ}C$. Moreover, the destruction of silicate connections at the center was observed as similar as that at the depth of 40 mm, where the transferred fire temperature was $618^{\circ}C$. This might be attributed to the temperature changes during cooling time after the fire test was neglected. Due to the relatively low thermal conductivity of concrete, the high temperature, which can affect the change of microstructure in cements, will hold longer at the center of the column than other depth.
Two new copper vanadium borophosphate compounds, $(NH_4)(C_2H_{10}N_2)_{5.5}[Cu(C_2H_8N_2)_2]_3[V_2P_2BO_{12}]_6{\cdot}17H_2O,\;Cu-VBPO1\;and\;(NH_4)(C_2H_{10}N_2)_{3.5}[Cu(C_2H_8N_2)_2]_5[V_2P_2BO_{12}]_6{\cdot}18H_2O$, Cu-VBPO2 have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, thermogravimetric analysis, IR spectroscopy, and elemental analysis. The structure of Cu-VBPO1 contains a layer anion, {$[Cu(C_2H_8N_2)_2]_3[V_2P_2BO_{12}]_6$}$^{12-}$, whereas Cu-VBPO2 has an open framework anion, {$[Cu(C_2H_8N_2)_2]_5[V_2P_2BO_{12}]_6$}$^{8-}$. Crystal Data: $(NH_4)(C_2H_{10}N_2)_{5.5}[Cu(C_2H_8N_2)_2]_3[V_2P_2BO_{12}]_6{\cdot}17H_2O$, monoclinic, space group I2/m (no. 12), $\alpha$ = 15.809(1) $\AA$, b = 31.107(2) $\AA$, c = 12.9343(8) $\AA$, $\beta$ = 104.325(1)$^{\circ}$, Z = 2; $(NH_4)(C_2H_{10}N_2)_{3.5}[Cu(C_2H_8N_2)_2]_5[V_2P_2BO_{12}]_6{\cdot}18H_2O$, tetragonal, space group $P4_2$/mnm (no.136), $\alpha$ = 26.832(1) $\AA$, c = 18.021(1) $\AA$, Z = 4.
The main objective of this study is the assessment of the ability of limestone mortars to resist to different chemical attacks. The ability of polypropylene (PP) fibres waste used as reinforcement of these concrete materials to enhance their durability is also studied. Crushed sand 0/2 mm which is a fine limestone residue obtained by the crushing of natural rocks in aggregates industry is used for the fabrication of the mortar. The fibres used, which are obtained from the waste of domestic plastic sweeps' fabrication, have a length of 20 mm and a diameter ranging between 0.38 and 0.51 mm. Two weight fibres contents are used, 0.5 and 1%. The durability tests carried out in this investigation included the water absorption by capillarity, the mass variation, the flexural and the compressive strengths of the mortar specimens immersed for 366 days in 5% sodium chloride, 5% magnesium sulphate and 5% sulphuric acid solutions. A mineralogical analysis by X-ray diffraction (XRD) and a visual inspection are used for a better examination of the quality of tested mortars and for better interpretation of their behaviour in different solutions. The results indicate that the reinforcement of limestone mortar by PP fibres waste is an excellent solution to improve its chemical resistance and durability. Moreover, the presence of PP fibres waste does not affect significantly the water absorption by capillarity of mortar nether its mass variation, when exposed to chloride and sulphate solutions. While in sulphuric acid, the mass loss is higher with the presence of PP fibres waste, especially after an exposure of 180 days. The results reveal that these fibres have a considerable effect of the flexural and the compressive behaviour of mortar especially in acid solution, where a reduction of strength loss is observed. The mineralogical analysis confirms the good behaviour of mortar immersed in sulphate and chloride solutions; and shows that more gypsum is formed in mortar exposed to acid environment causing its rapid degradation. The visual observation reveals that only samples exposed to acid attack during 366 days have showed a surface damage extending over a depth of approximately 300 ㎛.
Journal of the Korean Crystal Growth and Crystal Technology
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v.20
no.5
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pp.237-242
/
2010
Magnesium-substituted BCP (biphasic calcium phosphate) powders were prepared by incorporating small amounts of magnesium into the structure of different hydroxyapatite (HAp)/${\beta}$-tricalcium phosphate (${\beta}$-TCP) ratios through coprecipitation method. A series of magnesium substitutions ranging from 0, 0.5, and 1.0 wt%, which are comparable to the measured magnesium contents, were performed. The obtained powders were characterized by the following analytical techniques: X-ray diffraction analysis (XRD), Thermo Gravimetric Analyzer (TGA) and Fourier transform infrared spectroscopy (FT-IR). The results have shown that substitution of magnesium in the calcium-deficient apatites resulted in the formation of biphasic mixtures of different HAP/${\beta}$-TCP ratios after heating above $1000^{\circ}C$. The 1.0 wt% magnesiumsubstituted-BCP were soaked in Hank's solutions after 2 weeks to observe the morphology of the biocement, especially needle-like hydroxyapatite crystals and to estimate the length and diameter of nanoneedle crystals.
Kim, Jae-Gon;Kweon, Seon-Ja;Yun, Hyun-Du;An, Soo-Hyeon;Baik, Byeong-Ju
Journal of the korean academy of Pediatric Dentistry
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v.25
no.1
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pp.209-224
/
1998
The purpose of this study was to compare the amount of calcium fluoride deposited on the enamel and dentin surface and to obtain information on the morphological change and crystallographic details of mineral deposition after 12,000ppm APF application in vitro. The bovine enamel and dentin blocks were randomly assigned to eight groups according to artificial caries lesion formation and difference of fluoride application time. The fluoride concentration and morphological characteristics on the treated enamel and dentin surface were investigated by using fluoride quantitative analysis and SEM. The powdered enamel and dentin of the intact bovine incisors were prepared for the X-ray diffraction analysis. The following results were obtained. 1. The amounts of KOH-soluble fluoride on the carious enamel and dentin surface after 24h APF application were higher than after only 5min APF application(p<0.05), but in the case of the sound enamel and dentin surface were similar after 5min and 24h application (P>0.05). The fluoride content was highly increased in the carious dentin as compared with sound dentin after APF application(P<0.05). 2. The carious enamel surface after APF application, the demineralized enamel surface were recovered a more dense enamel surface and precipitation of crystal was observed a distintive surface layer of spherical globules of about 1 m diameter. In the case of the fluorided carious dentin surface, precipitation of calcium fluoride-like material was deposited both inside the dentinal tubules as well as in the intertubular regions. 3. The crystallographic structure of powdered enamel and dentin after 24h APF application had large crystallities of apatite and CaF2 diffraction peaks in the enamel as compared with dentin. The diffraction data collected from the 27.50-29.50(2) angular range of the powdered enamel, the (105) apatite, (225) apatite and (111) CaF2 peaks of the enamel crystallities were detected after 24h APF application.
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