The purposes of this dissertation are to demonstrate that DSC theromoanaytical methods of vulcanization can provide useful informations on the vulcanization characteristics of industrial formulations and also provides the potential basis for a rapid and complete method of sulfur and vulcanizing accelerator analysis for quality control. The influences of those factors such as heating rate, scan temperature, vucanizing accelerator's type and concentration upon vulcanization exotherm in NR and NBR compounds in the presence of vulcanizing accelerators such as TMTD,MBTS,DPG,TMTM,CBS, and MBT were evaluated by means of DSC. In order to examine the credibility in the DSC method, the same samples which were used for DSC method were studied to compare the DSC results with the ODR (Oscillating Disk Rheometer) data. The results obtained were as follows 1. In the DSC dynamic experiments, the observed enthalpy results from vulcanization depends upon the heating rate; In the range of 2 to $20^{\circ}C/min$ of heating rate, as the heating rate was increased the enthalpy change was also increased. However, over the heating rate of $30^{\circ}C/min$ it was observed that the enthalpy change was decreased as the heating rate was further increased. Without regard to the change of enthalpy, tremendous instantaneous heat evolving was observed in the range of high heating rates. 2. For the samples which are added with various vulcanizing accelerators, the activation energies of vulcanization were as follows; 3. Regarding to the influences of vulcanizining accelerator's types upon the characteristics of vulcanization exotherm, NR and NBR compounds in the presence of thiuramsulphide compounds type accelerators such as TMTD, TMTM, were exhibited sharper and higher vulclanization exotherm than others. From the resuts of DSC thermograms which was distributed in even shape in the broad temperature range, it was clearly shown that the guanidine compounds type accelerator such as DPG acts as a delayed acting accelerator. 4. In the comparison of DSC and ODR results, the dependency of temperature in the cure rate and the observed conversions show good agreements between two results. 5. In the same curatives, by the comparison of glass transition temperatures, it was possible to predict relative values of maximum torques. Consequently, from the present studies, it is shown that the DSC thermoanalytical method can provide an alternate new method for rapid and complete quality control analysis of rubber industry.
Optimal dispersion and fabrication conditions of carbon nanotube (CNT) embedded in phenolic resin were determined by electrical resistance measurement; and interfacial property was investigated between plasma treated carbon fiber and CNT-phenolic composites by electro-micromechanical techniques. Wettability of carbon fiber was improved significantly after plasma treatment. Surface energies of carbon fiber and CNT-phenolic nanocomposites were measured using Wilhelmy plate technique. Since surface activation of carbon fiber, the advancing contact angle decreased from $65^{\circ}$ to $28^{\circ}$ after plasma treatment. It was consistent with static contact angle results of carbon fiber. Work of adhesion between plasma treated carbon fiber and CNT-phenolic nanocomposites was higher than that without modification. The interfacial shear strength (IFSS) and apparent modulus also increased with plasma treatment of carbon fiber.
Hong, So Hee;Han, Sun-Gie;Kim, Su Young;Won, Yong Sun
Clean Technology
/
v.28
no.3
/
pp.210-217
/
2022
Boron(B) is a rare resource used for various purposes such as glass, semiconductor materials, gunpowder, rocket fuel, etc. However, Korea depends entirely on imports for boron. Considering the global boron reserves and its current production rate, boron will be depleted on earth in 50 years. Thus, a process including proper adsorbent materials recovering boron from seawater is demanded. This research proposed carbonized nanofibers prepared from electrospun PAN(polyacrylonitrile) mats as promising materials to adsorb boron in aqueous solution. First, the mechanism of boron adsorption on carbonized nanofibers was investigated by DFT(density functional method)-based molecular modeling and the calculated energetics demonstrated that the boron chemisorption on the nitrogen-doped graphene surface by a two-step dehydration is possible with viable activation energies. Then, the electrospun PAN mats were stabilized in air and then carbonized in an argon atmosphere before being immersed in the boric acid aqueous solution. Analytically, SEM(scanning electron microscopy) and Raman measurements were employed to confirm whether the electrospinning and carbonization of PAN mats proceeded successfully. Then, XPS(X-ray photoelectron spectroscopy) peak analysis showed whether the intended nitrogen-doped carbon nanofiber surface was formed and boron was properly adsorbed on nanofibers. Those results demonstrated that the carbonized nanofibers prepared from electrospun PAN mats could be feasible adsorbents for boron recovery in seawater.
The crystallization behavior of the amorphous $Fe_{73.5}Cu_{1}Nb_{3}Si_{16.5}B_{6}$ alloy with isothermal annealing at $552^{\circ}C$ was studied by $M\"{o}ssbauer$ spectroscopy. The amorphous phase was revealed to coexist together with $Do_{3}-FeSi$ nanocrystalline and Cu-duster in annealed alloys by $M\"{o}ssbauer$ spectrum analysis. At the early stage of crystallization, Si content of FeSi is high due to the creation of Cu-cluster, and decreases with annealing until 60 minutes, which results in the increase in the mean hyperfine field of FeSi, and thereafter keeps constant. After 60 minutes, the decrease in the mean hyperfine field of the residual armrphous, in spite of a slight change in the volume fraction of the FeSi and the residual armrphous, is caused by the increase in the content of Nb and B in residual amorphous phase. Both directions of the hyperfine field, those of the FeSi and the residual amorphous, become randomly oriented in about 60 minutes. For FeSi and Cu-duster, the Avrami exponents are 0.51 and O.65, the activation energies are 2.35 eV and 2.44 eV, and the incubation times are 2.4 minutes and 0.8 minutes respectively. Earlier formation of Cu-duster than that of FeSi is coincidence with the fact that Cu atom promotes the nucleation of the FeSi.
The creep behavior of a rapidly solidified and consolidated Al-9.45wt%Fe-4.45wt%Cr alloy were investigated in the stress range 40 to 115 MPa and temperature range 300(0.53Tm) to 441$^{\circ}C$(0.66Tm). It is of use to available aerospace and automobile industries for the improved performance of materials used at high temperature. Because Al alloys with improved creep resistance offer the potential for lower weight and reduced costs in aerospace and automobile components (e.g., structural members and engine parts) through the replacement of heavier and more costly materials, the safety in use at high temperature is good. The alloy is characterized by high stress exponents and activation energies for creep, which are greatly dependent on the stress and temperature. Because the creep stress is seen to cause a strongly significant enhancement of coarsening, the coarsening rate of the dispersed particles in all crept specimens is faster than that in isothermally annealed specimens. Dislocations connecting dispersoids are observed more cofrequently in crept specimens with higher stress and lower temperature. The creep strain rates in the power law creep regime were found to be predicted much better by the Shorty and Rosler/Arzt equation with the inclusion of a threshold stress and dislocation detachment mechanism. The dispersoids in this alloy were acting a source of void nucleation that finally leaded to ductile fracture within the grain so called intergranular. Each void was initiated, grown and failed at the dispersoids in the aluminium matrix. Grain boundary accommodation of the slip produced, which result in initiation of the void and then final transgranular fracture. Therefore, it was confirmed that these dispersoids played an important role in the fracture mechanism by the formation of $Al_{13}Fe_4$, $Al_{13}Cr_2$ and $Al_2O_3$.
KIM Sang-Moo;PARK Seong-Min;CHOI Hyeon-Mee;LEE Keun-Tai
Korean Journal of Fisheries and Aquatic Sciences
/
v.30
no.5
/
pp.859-867
/
1997
In order to utilize the processing wastes of squid, chitosans were manufactured from the pens of domestic squid, Todarbdes pacificus and foreign squid, Ommastrephes bartrami and then, its rheological properties were studied. The amounts of nitrogen and minerals of the domestic squid pens were $11.4\%\;and\;0.1\%$ respectively, whereas those of its chitosan were $7.5\%\;and\;0.2\%$. In case of foreign squid pen and chitosan, the amounts of nitrogen and minerals were $12.1\%,\;0.8\%\;and\;7.8\%,\;0.2\%$ respectively. Intrinsic viscosity $([\eta]) $ of domestic and foreign squid pen chitosans were decreased with increasing pH from 3.4 to 5.4 which might be due to the reduced repulsion in inter- of intra- chitosan molecules. Intrinsic viscosity of the domestic and foreign squid pen chitosans were decreased with increasing NaCl concentration thus indicated that the domestic and foreign squid pen chitosans were polyelectrolyte molecules and stiffness of squid pen thitosans were 0.11 similar to that of k-carrageenan. Flow type of squid pen chitosan solutions were pseudoplastic fluids without yield stress by the viscosity measurement. But the squid pen chitosan solutions showed newtonian fluid up to $0.15\~0.24\%$ concentration for domestic and $0.21\~0.24\%$ concentration for foreign at $10\~50\%$. Concentration dependence of consistency index in infinitive dilute domain (Kc) were higher in the dilute domain than entangled domain. Activation energies (Ea) of the squid pen chitosans were 3.7, 6.3, 3.6, 4.0 and 4.1 Kcal/g moi for domestic and 3.2, 3.1, 3.4, 3.8 and 3.6 Kcal/g mol for foreign at 0.1, 0.15, 0.25, 0.35 and $0.5\%$, respectively.
A post-irradiation annealing study was conducted with use of reactor pressure vessel(RPV) steel A533B Cl.1 base metal irradiated to a dose of 4.84$\times$10$^{18}$ n/$\textrm{cm}^2$ at about 38$0^{\circ}C$. Microhardness and positron annihilation (PA) methods were used to obtain better understanding of the recovery of radiation hardening. Isochronal anneal experiments indicated that two recovery processes occur during annealing of irradiated specimens. The first recovery process occurs in the temperature range of 280-3O5$^{\circ}C$, Michrohardness and positron annihilation (PA) methods were used to obtain better understanding of the recovery of radiation hardening. Isochronal anneal experiments indicated that two recovery processes occur during annealing of irradiated specimens. The first recovery process occurrs in the temperature range of 280-305$^{\circ}C$. The variations of Ip, Iw and R parameters indicated that the formation of vacancy clusters by vacancy agglomeration and the annihilation of monovacancies are the first recovery process. The second recovery process occurs in the range of 405-49$0^{\circ}C$ and positron annihilation parameters measured indicated that the dissolution of carbon atoms decorated around vacancy-type defects and possible precipitates, and the annihilation of monovacancies give rise to the second recovery process. It was further indicated that radiation anneal hardening (RAH) in the range of 305-405$^{\circ}C$ between the temperature ranges for the two processes occurs due to the formation of carbon-decorated vacancy clusters and precipitates. The activation energies, orders of reaction and other characteristics of recovery processes were determined by the Meechan-Brinkman method. The activation energy for the first recovery process was determined as 1.76 eV and that for the second recovery process as 2.00eV. These values are lower than those obtained by other workers. This difference may be attributed to the lower copper content of the RPV steel used in the present study. The order of reaction for the first recovery process was determined as 1.78, while that for the second recovery process as 1.67 Non-integer orders of reaction for recovery processes seem to be attributed to the fact that several mechanisms for the first order and the second order of reaction are compounded in one process. This result also supports for the above conclusions from measurements of PA parameters.
The effects of deposition temperature on chemical vapor deposited silicon carbide (CVD-SiC) were studied to obtain high deposition rates and excellent bending strength characteristics. Silicon carbide prepared at $1250{\sim}1400^{\circ}C$ using methyltrichlorosilane(MTS : $CH_3SiCl_3$) by hot-wall CVD showed deposition rates of $95.7{\sim}117.2{\mu}m/hr$. The rate-limiting reaction showed the surface reaction at less than $1300^{\circ}C$, and the mass transfer dominant region at higher temperature. The activation energies calculated by Arrhenius plot were 11.26 kcal/mole and 4.47 kcal/mole, respectively. The surface morphology by the deposition temperature changed from $1250^{\circ}C$ pebble to $1300^{\circ}C$ facet structure and multi-facet structure at above $1350^{\circ}C$. The cross sectional microstructures were columnar at below $1300^{\circ}C$ and isometric at above $1350^{\circ}C$. The crystal phases were all identified as ${\beta}$-SiC, but (220) peak was observed from $1300^{\circ}C$ or higher at $1250^{\circ}C$ (111) and completely changed to (220) at $1400^{\circ}C$. The bending strength showed the maximum value at $1350^{\circ}C$ as densification increased at high temperatures and the microstructure changed from columnar to isometric. On the other hand, at $1400^{\circ}C$, the increasing of grain size and the direction of crystal growth were completely changed from (111) to (220), which is the closest packing face, so the bending strength value seems to have decreased.
A comparative study of enzymatic properties between the trypsin from the cat-shark Cephaloscyllium umbratile ( C-T) and the two trypsins from the mackerel Scomber japonicus $(M-T_A\;and\;M-T_B)$ was carried out following after the previous paper(Pyeun et al., 1991). Trypsin from cat-shark(C-T) showed the higher heat stability compared to the others $(M-T_A\;and\;M-T_B)$ and its denaturation constant$(K_D)$ was $10.68\times10^{-4}\;sec^{-1}\;at\;55^{\circ}C$ with BA-p-NA substrate. The activation energies(Ea) of the trypsins measured at a temperature range from $30^{\circ}C\;to\;50^{\circ}C$ were estimated to be 4.07 kcal/mole for C-T, 11.61 kcal/mole for $M-T_A$, and 8.43kcal/mole for $M-T_B$, respectively. The Km values were $24.9\times10^{-5}\;M\;for\;C-T,\;5.37\times10^{-5}\;M\;for\;M-T_A,\;and\;9.65\times10^{-5}\;M\;for\;M-T_B$. On the other hand, the Ki values for TLCK and DFP determined by Dixon plot were $1.50\times10^{-6}\;M\;and\;9.28\times10^{-6}\;M\;for\;C-T\;2.86\times10^{-6}\;M\;and\;2.11\times10^{-4}\;M\;for\;M-T_A\;and\;3.90\times10^{-6}\;M\;and\;1.60\times10^{-4}\;M\;for\;M-T_B$ Similar amino acid profiles were showed between three trypsins each other, with few exceptions of $M-T_B$ containing higher amount of arginine, and the smaller amount of tryptophan in C-T than the others.
$Ta_2O_5$ thin film IS a promising material for the high dielectrics of ULSI DRAM. In this study, $Ta_2O_5$ thin film was grown on p-type( 100) Si wafer by thermal metal organic chemical vapo deposition ( MCCVD) method and the effect of operating varialbles including substrate temperature( $T_s$), bubbler temperature( $T_ \sigma$), reactor pressure( P ) was investigated in detail. $Ta_2O_5$ thin film were analyzed by SEM, XRD, XPS, FT-IR, AES, TEM and AFM. In addition, the effect of various anneal methods was examined and compared. Anneal methods were furnace annealing( FA) and rapid thermal annealing( RTA) in $N_{2}$ or $O_{2}$ ambients. Growth rate was evidently classified into two different regimes. : (1) surface reaction rate-limited reglme in the range of $T_s$=300 ~ $400 ^{\circ}C$ and (2: mass transport-limited regime in the range of $T_s$=400 ~ $450^{\circ}C$.It was found that the effective activation energies were 18.46kcal/mol and 1.9kcal/mol, respectively. As the bubbler temperature increases, the growth rate became maximum at $T_ \sigma$=$140^{\circ}C$. With increasing pressure, the growth rate became maximum at P=3torr but the refractive index which is close to the bulk value of 2.1 was obtained in the range of 0.1 ~ 1 torr. Good step coverage of 85. 71% was obtained at $T_s$=$400 ^{\circ}C$ and sticking coefficient was 0.06 by comparison with Monte Carlo simulation result. From the results of AES, FT-IR and E M , the degree of SiO, formation at the interface between Si and TazO, was larger in the order of FA-$O_{2}$ > RTA-$O_{2}$, FA-$N_{2}$ > RTA-$N_{2}$. However, the $N_{2}$ ambient annealing resulted in more severe Weficiency in the $Ta_2O_5$ thin film than the TEX>$O_{2}$ ambient.
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