• Elastomers and Composites
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• v.38 no.4
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• pp.326-333
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• 2003

Even though many studies have been reported about rubber vulcanization, it is still remained difficult to find a quantitative relationship between the final states of vulcanized rubber and initial formulation or processing conditions. Dynamic differential scanning calorimetry (DSC) method is known as a comparatively easy method to research for the rubber vulcanization in both experimental and analysis. In the present research, a study on the vulcanization reaction of NR/CB composites modified by isoprene(IR) and chloroprene(CR) rubbers is carried out using dynamic DSC method. Thermograms with several different heating rates were obtained and analyzed using the Kissinger method. Analysis showed that the vulcanization reaction was progressed through the first order reaction mechanism. In addition, the reaction temperature was severely influenced by the kinds or rubber modifiers, in this case, more influenced by CR than by IR. Those effects were clearly verified in the values of activation energy. Kinds of carbon blacks, however, could hardly influence on the reaction mechanism.

• Proceedings of the Korea Concrete Institute Conference
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• 2003.11a
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• pp.545-548
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• 2003

The purpose of this study is measures vulcanization properties of matter by time of room temperature vulcanization synthetic rubber sheet and the evaluation adhesive properties tested by concrete surface moisture. Also, Its estimated reaction mechanism and adhesion performance between protection mortar and waterproofing layer. The results showed that vulcanization progressed in room temperature and adhesion intensity increased regardless of moisture condition.

• Elastomers and Composites
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• v.39 no.3
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• pp.179-185
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• 2004

Frequency dependency or electrical property stabilization during vulcanization of modified NR/IR composite materials was studied using in-situ electrical property measuring technique. Volume resistivity(p) before and after vulcanization reaction of the sample was measured as the function or frequency in the range or 1Hz to 10kHz at reaction temperatures of 130, 140, 150, and $160^{\circ}C$, respectively. A double stabilization mode of frequency dependency was observed, in which a slow stabilization process of p to a value of ca. $1.0{\times}10^7\;{\Omega}-cm$ occurred after a drastic initial decrease from ca. $9.0{\times}10^7\;{\Omega}-cm$. In addition, notable temperature dependencies of p values were also observed before and after vulcanization reaction, that is, p values at 130 and $140^{\circ}C$ after vulcanization were observed as about 1/3 of those values before vulcanization. All the observed facts were considered as the results from the interaction between the electrode and the bulk sample materials, i.e., electronic charge-discharge, and from the structure change of samples including CB rearrangement by the vulcanization.

• Elastomers and Composites
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• v.27 no.4
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• pp.275-280
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• 1992

Vulcanization reaction was studied by DSC through the comparison cure states to physical properties and the investegation of chemicals effect on vulcanization. Reaction enthalpy showed a good correlation with physical properties, increased with the increase of sulfur content, and increased with accelerator content, as well, where the ratio of MOR to sulfur was less than 1.0. Reaction temperature was decreased with increasing accelerator content and decreased also with sulfur content where the ratio of MOR to sulfur was more than 1:3. As a result, the cure state and reaction temperature could be controlled effectively with the ratio of accelerator to sulfur in the range of a third to unity.

• Elastomers and Composites
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• v.38 no.3
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• pp.235-242
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• 2003

A vulcanization reaction characteristics of an isoprene rubber (IR)-modified natural rubber/carbon black (NR/CB) composite was studied using in-situ electrical property measuring technique. Since the electrical conductivity of the sample composite would be changed continuously during the vulcanization reaction by rearranging of the carbon black particles within the sample, volume resistivity (${\rho}$) might be obtained as a function or reaction time. A stabilization time ($t_i$), maximum reaction speed time ($t_p$), and volume resistivity at that time(${\rho}_p$) were defined from the data for the Arrhenius analysis. Volume resistivity ${\rho}$ showed a comparatively high value of ${\sim}10^8$ order before the reaction started, and dramatically decreased to be stabilized within $1{\sim}2$ minutes as soon as the reaction started. As the more time elapsed, thereafter, ${\rho}$ decreased monotonously to a certain constant value through a peak, ${\rho}_p$ at time $t_p$, which was considered as the maximum reaction rate. As a result, while $t_i$ values were comparatively constant as $1{\sim}2$ minutes, $t_p$ values showed to become shorter and shorter as the reaction temperature.

• Macromolecular Research
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• v.9 no.3
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• pp.157-163
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• 2001

The influences of carbon black loading and cure type on the cure characteristics including kinetics and dynamic mechanical properties were investigated for a styrene-butadiene rubber (SBR). The rate constants of accelerated sulfur vulcanization reaction at three different temperatures were determined using a cure rheometer, and they were compared with those from the direct measurement of sulfur concentration. The strain softening behavior under dynamic deformation, known as the Payne effect was also discussed depending on the carbon black loading and cure type.

• Elastomers and Composites
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• v.22 no.4
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• pp.333-339
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• 1987

A modern kinetic evaluation method for nonisothermal reactions measured with Differential Scanning Calorimetry(DSC) is presented. It is based on multiple linear regression analysis using a number of curve points in a selectable range of conversion. The obtained kinetic data are the basis to compute a reaction process under any condition e.g. isothermal or adiabatic. The DSC measurements was performed on a Mettler TA3000 SYSTEM with the built in evaluation software. Mainly the following reactions are discussed: vulcanization of natural rubber compounds containing vulcanizing accelerators. The purpose of this work is to analyse the vulcanization kinetics of typical NR vulcanization systems using DSC. These systems were chosen because they are typically reactive elastomer and are commercially important.

• Elastomers and Composites
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• v.46 no.2
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• pp.152-157
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• 2011

Effects of CR contents in NR/CR blends on the vulcanization kinetics and miscibility were studied by dynamic DSC and TGA, as well as the mechanical properties. While the vulcanization activation energy showed a constant value of $77.5{\pm}2.5$ kcal/mol regardless of CR contents, reaction rate, however, was observed to be somewhat lowered at increased CR contents. Partial miscibility was found between NR and CR phases at lower CR content of 3 wt%, but immiscibility was observed at higher CR content of 21 wt%. Mechanical properties were also affected by this miscibility, showing linear increase of compression set but decrease of tensile strength with CR contents in the blends.

• Elastomers and Composites
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• v.43 no.4
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• pp.281-287
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• 2008

Using solid state $^{13}C$ NMR, polybutadiene rubber vulcanizates were qualitatively and quantitatively analyzed. In the filled conventional system of BR vulcanizate accelerated with TBBS, addition to the olefinic double bond and substitution in the $\alpha$ position to the double bond occurred simultaneously. Also the latter $\alpha$ substitution reaction was faster than the former addition reaction at initial reaction time. In addition, it was suggested that double bond-addition-polysulfide structures might be modified into 5-membered and 6-membered cyclic structures in overcure time. These chain modifications were correlated with the decrease in the chemical crosslink density in overcure time.

• Elastomers and Composites
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• v.47 no.1
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• pp.54-64
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• 2012

Acrylonitrile was introduced in the emulsion SBR to increase compatibility between silica and rubber. AN-SBR/silica compounds showed faster vulcanization time and higher delta torque values than SBR 1721/silica compounds because interaction between nitrile group of AN-SBR and silanol group on the silica surface could make hydrogen bond that prevented adsorption of the accelerator on the silica surface, which improved the vulcanization reaction efficiency and enhanced the degree of crosslinking. AN-SBR/silica compound showed higher values in minimum torque than SBR 1721/silica compound during the vulcanization because AN-SBR has higher molecular weight than SBR 1721 in the raw material. When PEG was added to the SBR 1721 and AN-SBR compounds, vulcanization time was faster than SBR 1721 and AN-SBR compounds without PEG because PEG has a large number of ether linkages which show high compatibility with silanol group on the silica surface that prevented the adsorption of the accelerator and the ingredients on the silica surface, which improved the vulcanization reaction efficiency. In the mechanical properties, AN-SBR compounds showed higher modulus values at 100%, 300% than SBR 1721 compounds because interaction between nitrile group of AN-SBR and silanol group on the silica surface enhanced the degree of crosslinking. In the dynamic properties, AN-SBR compounds showed lower tan ${\delta}$ values at $0^{\circ}C$ than SBR 1721 compounds in accordance with the $T_g$ values. AN-SBR compounds showed lower tan ${\delta}$ values at $60^{\circ}C$ than SBR 1721 compounds because interaction between acrylonitrile and silica caused strong filler-rubber interaction that induced low energy dissipation by the filler-filler interaction.