The structural characteristics of Antheraea yamamai and Antheraea pernyi silk were investigated by using x-ray diffraction method, IR spectroscopy and polarizing microscopy. The amino acid composition, fiber density, thermal decomposition temperature and glass transition temperature were also measured for relating these physical properties to the structure in comparison with those of Bombyx mori silk fiber. There was no significant structural difference between A. yamamai and A. pernyi silk fiber on an examination of x-ray diffraction curve and IR spectrum. Both of these wild silk fibers showed double diffraction peaks at the Bragg angle 2Θ16.7˚ and 20.5˚by x-ray diffraction analysis as well as IR absorption peaks for the bending vibration of specific groups related to ala-ala amino acid sequence. On the other hand, the x-ray diffraction curve and IR spectrum of Bombyx mori silk fiber are different from those of wild silk fibers, indicating different crystal structure as well as amino acid sequences. It showed under the polarizing microscope examination that the birefringence and optical orientation factor of wild silk fibers are much lower than those of B. mori silk. Also, the surface of degummed wild silk fibers was characterized by the longitudinal stripes of microfibrils in the direction of fiber axies. The amino acid composition, which is strongly related to the fine structure and properties, was not significantly different between these two wild silk fibers. However, the alanine content was somewhat less and polar amino acid content more for A. yamamai. As a result of fiber density measurement, the specific gravities of B. mori, A. pernyi and A. yamamai were 1.355~1.356, 1.308~1.311, 1.265~1.301g/㎤ in the order, respectively. The calculated crystallinity(%) was 64% for B. mori and 51~52% for wild silk fibers, which showed same trend by IR method in spite of somewhat higher value. The thermal decomposition behaviour was examined by DSC and TGA, showing that the degradation temperature was in the order of B mori, A. prernyi and A. yamamai at around 350$^{\circ}C$. It was also observed by TGA that the decomposition seems to proceed step by step according to their specific regions in the fiber structure, resulting the difference in their thermal stabilities. The glass transition temperature was turned out to be 220$^{\circ}C$ for B. mori, 240$^{\circ}C$ A. yamamai and 255$^{\circ}C$ A. pernyi by the dynamic mechanical analysis. It is expected that the chemical properties are affected by the dynamic mechanical behavior in accordance with their structural characters.
The Deogbong napseok clay deposit which is composed mainly of dickite and pyrophyllite has been formed by hydrothermal alteration of the Late Cretaceous volcanic rocks consisting of andesitic tuff and andesite. The mineralogy of the napseok ores and the hydrothermal alteration processes have been studied in order to know the nature of the interaction between minerals and fluids for the formation of the deposit. Chemical distribution shows that alkali elements and silica were mobile but alumina was relatively immobile during the hydrothermal processes. It is evident that enrichment of alumina and leaching of silica from the host rock led to the formation of the napseok ore, whereas the enrichment of silica in the outer zone of the deposit gave rise to the silica zone. A large amount of microcrystalline quartz closely associated with dickite and pyrophyllite suggests the increasing activity of silica. Thus Si which was released away from the argillic zone by the increasing activity of silica. Thus Si which was released away from the argillic zone by the increasing activity of silica solubility moved out precipitating in the margin of the deposit to form the silica zone. Variation in dickite crystallinity implies the local change in the stability of the system. Thermodynamic calculation shows that the invariant point of pyrophyllite-dickite (kaolinite)-diaspore-quartz assemblages at 500 bars in the system $Al_{2}O_{3}-SiO_{2}-H_{2}O$ is about 300 $^{\circ}C$. Based on the mineral assemblages and the experimental data reported, it is estimated that the main episode of hydrothermal alteration occurred at least above 270 to 300 $^{\circ}C$ and $X_{CO_2}$ <0.025. Mineral occurrence and chemical variation indicate that the activity of Al is high in the upper part of the deposit, whereas the activity of Si is high in the lower part and the margin of the deposit. The nonequilibrium phase relations observed in the Deogbong deposit might be due to local change in intensive thermodynamic variables and fluid transport properties that resulted in the formation of nonequilibrium phases b of several stages.
Octenyl succinylated (OSA) potato starch was dextrinized by two methods: ultrasound (at 25, 50, or $70^{\circ}C$ for 1 h; OSA-25UT, OSA-50UT, and OSA-70UT, respectively) and acid hydrolysis (for 1 or 4 h; OSA-AD1H or OSA-AD4H, respectively), and the properties of the resulting starch were analyzed. The melting enthalpy of OSA-70UT decreased the most (from 14.0 to 10.0 mJ/mg), indicating chain degradation. For pasting properties, as ultrasound treatment temperature increased, peak viscosity decreased (2884, 2550, and 1888 cP, respectively), whereas acid hydrolysis increased peak viscosity and decreased pasting temperature. The relative crystallinity of OSA-dextrin produced by ultrasound or acid hydrolysis significantly decreased (from 33.61 to 14.90-26.03 and 19.28-20.05, respectively) as temperature or time increased, yet a B-type crystal pattern was maintained. Regarding emulsifying stability and sensory tests of mayonnaise prepared with OSA potato dextrin, mayonnaise with OSA-70UT was stable for short storage period (1 week), however mayonnaise with OSA-AD1H was the most suitable for long storage periods (from 2 to 4 weeks). In addition, the OSA-70UT was the most acceptable for mayonnaise in the sensory test.
Various Mn-oxides can oxidize Cr(III) to Cr(VI). Behaviors of chromium species in the oxidation system, especially on the oxide surface, are expected to control the reaction. During Cr(III) oxidation by birnessite and pyrolusite, Cr species in the reaction system were determined to elucidate their effects on the oxidation. Capacities of Cr oxidation of the two Mn-oxides were quite different. Solution pH and initial Cr(III) concentration also had significant effects on the Cr(III) oxidation by Mn-oxides. Chromium oxidation by pyrolusite was less than 5% of the oxidation by birnessite. The high crystallinity of pyrolusite could be one of the reasons and the difficulty of Cr (III) diffusion to the positive pyrolusite surface and Cr(VI) and Cr(III) adsorption seems to be other controlling factors. At pH 3, adsorption or precipitation of Cr species on the surface of birnessite were not found. Small amount of Cr(VI) adsorption was found on the surface of pyrolusite, but arty Cr precipitation on the oxide surface was not found. Therefore Cr(III) oxidation at pH 3 seems to be controlled mainly by the characteristics of Mn-oxides. Chromiun oxidation by Mn-oxides is thermodynamically more favorable at higher solution pH. However as solution pH increased Cr oxidation by birnessite was significantly inhibited. For Cr oxidation by pyrolusite, as pH increased the oxidation increased, but as Cr(III) addition increased the reaction was inhibited. Under these conditions some unidentified fraction of Cr species was found and this fraction is considered to be Cr(III) precipitation an the oxide surface. Chromium(III) precipitation on the oxide surface seems to play an important role in limiting Cr(III) oxidation by armoring the reaction surface on Mn-oxides as well as lowering Cr(III) concentration available for the oxidation reaction.
Journal of Korean Society of Environmental Engineers
/
v.38
no.11
/
pp.603-610
/
2016
This work studies the synthesis of birnessite (${\delta}-MnO_2$), a catalyst of oxidative-coupling reactions, from the powder of spent alkaline manganese batteries (SABP, <8 mesh) and evaluate its reactivity for 1-naphthol (1-NP) removals. Manganese oxides using commercial reagents ($MnSO_4$, $MnCl_2$) and the acid birnessite (A-Bir) by McKenzie method were also synthesized, and their crystallinity and reactivity for 1-NP were compared with one another. 96% Mn and 98% Zn were extracted from SABP by acid leaching at the condition of solid/liquid (S/L) ratio 1:10 in $1.0M\;H_2SO_4+10.5%\;H_2O_2$ at $60^{\circ}C$. From the acid leaching solution, 69% (at pH 8) and 94.3% (pH>13) of Mn were separated by hydroxide precipitation. Optimal OH/Mn mixing ratio (mol/mol) for the manganese oxide (MO) synthesis by alkaline (NaOH) hydrothermal techniques was 6.0. Under this condition, the best 1-NP removal efficiency was observed and XRD analysis confirmed that the MOs are corresponding to birnessite. Kinetic constants (k, at pH 6) for the 1-NP removals of the birnessites obtained from Mn recovered at pH 8 (${Mn^{2+}}_{(aq)}$) and pH>13 ($Mn(OH)_{2(s)}$) are 0.112 and $0.106min^{-1}$, respectively, which are similar to that from $MnSO_4$ reagent ($0.117min^{-1}$). The results indicated that the birnessite prepared from the SABP as a raw material could be used as an oxidative-coupling catalyst for removals of trace phenolic compounds in soil and water, and propose the recycle scheme of SAB for the birnessite synthesis.
The TiO$_2$ coating solutions were synthesized with different concentrations (T1-0.7N, T2-2.0N) of hydrochloric acid used as catalyst. and TiO$_2$ thin films were prepared by sol-gel dip coating. Their structural and optical properties were examined as a function of calcination temperature. XRD results showed that T1 thin films calcined at 400~80$0^{\circ}C$ had the anatase phase, while those calcined at 100$0^{\circ}C$ had the rutile phase. T2 thin films calcined at 40$0^{\circ}C$ and $600^{\circ}C$ had the anatase phase, with the rutile phase for calcination at 80$0^{\circ}C$. Crystallinity of T2 thin films was superior to that of T1 thin films. The crystallite size of TiO$_2$ thin films increased with increasing calcination temperature, and the crystallite size of anatase phase in T2 thin films was larger than that in T1 thin films, but the crystallite size of rutile phase in T2 thin films was smaller. The surface morphology of the films showed that the films were formed more densely in the rutile phase than in the anatase phase, this phenomenon appeared conspicuously in T2 thin films. The transmittance of the samples with thin films on quartz glass calcined at 100$0^{\circ}C$ was significantly reduced at wavelength range about 300-700 nm due to the increased absorption originating from the change of crystallite phase and composition of the films and the scattering effect originating from increasing crystallite size. The refractive index of TiO$_2$ thin films increased, and hence the film thickness as well as the porosity of TiO$_2$ thin films decreased with increasing calcination temperature. Furthermore, the refractive index of T2 thin films was higher than T1 thin films, and porosity of T2 films was lower.
Kaolinite [$Al_2Si_2O_5(OH)_4$] was successfully synthesized by a hydrothermal process from amorphous $Al(OH)_3$ and $SiO_2$ at $230^{\circ}C$ under the pressure of $30 kg/cm^2$. The experiments were performed varying temperatures ($180{\sim}280^{\circ}C$), pressure ($10{\sim}60kg/cm^2$), chemistry ($Al_2O_3/SiO_2 = 0.5{\sim}0.38$) and pH ($0.3{\sim}9.5$) of the solution. The autoclaving was carried out in a closed stainless steel vessel. Kaolinite appears from the starting composition of $Al_2O_3/SiO_2= 0.5$ with boehmite and was stable as a single phase with the composition of $Al_2O_3/SiO_2=0.45$. Boehmite was a stable phase below $200^{\circ}C$ for the 240 h period of autoclaving, but kaolinite appeared even in 20 h at $230^{\circ}C$. The single kaolinite phase of a good crystallinity was observed at pH ranging 2 to 6. That indicates that pH is one of the most critical parameters for the successful formation of kaolinite. The optimal molar ratio of $Al_2O_3$ to $SiO_2$ was determined to be 0.45. The XRD pattern of the synthesized kaolinite coincided with that of natural one and its morphology was the cluster type of the kaolinite crystals (diameter = ${\sim}3{\mu}m$), irrespective of starting material, composition and temperature.
Journal of the Korean Institute of Telematics and Electronics A
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v.33A
no.2
/
pp.96-113
/
1996
It has been found that the misfit dislocations in heavily boron-doped layers originate from wafer edges. Moreover, the propagation of the misfit dislocation into a heavily boron-doped region can be suppressed by placing a surrounding undoped region. Using a surrounding undoped region the disloction-free heavily boron-deoped silicon membranes have been fabricated. The measured surface roughness, fracture strength, and residual tensile stress of the membrane are 20.angs. peak-to-peak, 1.39${\times}$10$^{10}$ and 2.7${\times}$10$^{9}$dyn/cm$^{2}$, while those of the conventional heavily boron-doped silicon membrane with high density of misfit dislocations are 500 peak-to-peak, 8.27${\times}$10$^{9}$ and 9.3${\times}$10$^{8}$dyn/cm$^{2}$ respectively. The differences between these two membranes are due to the misfit dislocations. Young's modulus has been extracted as 1.45${\times}$10$^{12}$dyn/cm$^{2}$ for both membranes. Also, the effective lattice constant of heavily boron-doped silicon, the in-plane lattice constant of the conventional membrane, and the density of misfit dislocation contained in the conventional membrane have been extracted as density of misfit dislocation contained in the conventional membrane have been extracted as density of misfit dislocation contained in the conventional membrane have been extracted as 5.424.angs. 5.426.angs. and 2.3${\times}$10$^{4}$/cm for the average boron concentration of 1.3${\times}$10$^{20}$/cm$^{-23}$ cm$^{3}$/atom. Without any buffer layers, a disloction-free lightly boron-doped epitaxial layer with good crsytalline quality has been directly grown on the dislocation-free heavily boron-doped silicon layer. X-ray diffraction analysis revealed that the epitaxial silicon has good crystallinity, similar to that grown on lightly doped silicon substrate. The leakage current of the n+/p gated diode fabricated in the epitaxial silicon has been measured to be 0.6nA/cm$^{2}$ at the reverse bias of 5V.
Kim, K.Y.;Shin, K.S.;Han, S.H.;Lim, S.H.;Kim, H.J.;Jang, S.H.;Kang, T.
Journal of the Korean Magnetics Society
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v.10
no.2
/
pp.67-73
/
2000
Top spin valve samples with a structure Ta/NiFe/CoFe/Cu/CoFe/FeMn/Ta were deposited on a Si(100) substrate by changing d.c. magnetron sputtering conditions and the exchange-bias and magnetic properties of samples were investigated. The Exchange field, H$\_$ex/ increased with increase of sputtering power of FeMn from 30 to 150 W and CoFe from 30 to 100 W deposited on the Cu, the increase of H$\_$ex/ was found due to the improvement of preferred orientation of (111) FeMn phase from XRD results. In the case of Cu, H$\_$ex/ decreased with the increase of sputtering pressure ranging from 1 to 5 mTorr. The relationship between exchange field and resistance was investigated, spin valve samples with a large exchange field showed the lower resistance, which was strongly dependent on the good crystallinity and grain size increase as well as lower scattering effects. The Cu thickness was changed from 22 to 38 $\AA$ for Si/Ta/NiFe/CoFe/Cu(t), 30 W/CoFe, 100 W/FeMn, 100 W/Ta spin valve structures, MR ratio of 6.5 % and exchange field of about 190 Oe were obtained for the sample with Cu of 22 $\AA$ thickness. The increase of exchange field with decrease of Cu thickness was explained by FM/AFM spin-spin interaction.
Kim, Yoon-Hee;Cho, Moon-Jung;Shin, Keum;Kim, Tae-Jong;Kim, Nam-Hun;Kim, Yeong-Suk
Journal of the Korean Wood Science and Technology
/
v.38
no.3
/
pp.262-273
/
2010
In the enzymatic hydrolysis of rice straw and wood meals using extra-cellular enzymes from Fomitopsis palustris, key factors which enhanced the sugar conversion yield were investigated in this work, such as enzyme production and enzyme reaction conditions, surfactant effects, and the surface structure of substrates. F. palustris cultured with softwood mixture produced 12.0 U/$m{\ell}$ for endo-${\beta}$-1,4-gulcanase (EG), 116.68 U/$m{\ell}$ for ${\beta}$-glucosidase (BGL), 18.82 U/$m{\ell}$ for cellobiohydrolase (CBH), and 13.33 U/$m{\ell}$ for ${\beta}$-xylosidase (BXL). These levels of BGL, CBH, and BXL activities were two to four folds more than enzyme activities of F. palustris cultured with rice straw. The optimum reaction conditions of cellulase-RS which produced by F. palustris with rice straw and cellulase-SW which produced by F. palustris with softwood mixture were pH 5.0 at $45^{\circ}C$ and pH 5.0 at $50^{\circ}C$, respectively. The sugar conversion yield of cellulase-SW had the highest value of $40.6{\pm}0.6%$ within 72 h when rice straw was used as substrate. By adding 0.1% Tween 20 (w/w-substrate), the sugar conversion yield of rice straw was increased to 44%, which was about four fifths sugar conversion yield of commercial enzyme, Celluclast 1.5L (Novozyme A/S). A low crystallinity and an intensive fibril surface observed by the scanning electron microscope may explain the high sugar conversion yield of rice straw.
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