Curing differential scanning calorimetry

Two techniques, dynamic mechanical thermal analysis (DMTA) and dielectric thermal analysis (DETA), have been used for the study of resin cure. Differential scanning calorimetry (DSC) has also been employed (for a discussion of the theory and instrumentation of DSC, see Chapter 9). The application of differential photocalorimetry to the measurement of cure rates of photocurable resins is discussed in Chapter 12. 

Besides TMA, two other thermal analysis techniques are also commonly used for measuring Tg and degree of cure differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). 

The process known as transimidization has been employed to functionalize polyimide oligomers, which were subsequentiy used to produce polyimide—titania hybrids (59). This technique resulted in the successhil synthesis of transparent hybrids composed of 18, 37, and 54% titania. The effect of metal alkoxide quantity, as well as the oligomer molecular weight and cure temperature, were evaluated using differential scanning calorimetry (dsc), thermogravimetric analysis (tga) and saxs. 

The cure of novolaks with hexa has been studied with differential scanning calorimetry (dsc) and torsional braid analysis (tba) (46) both a high ortho novolak and a conventional acid-cataly2ed system were included. The dsc showed an exothermic peak indicating a novolak—hexa reaction ca 20°C higher than the gelation peak observed in tba. Activation energies were also calculated. 

Cure kinetics of thermosets are usually deterrnined by dsc (63,64). However, for phenohc resins, the information is limited to the early stages of the cure because of the volatiles associated with the process. For pressurized dsc ceUs, the upper limit on temperature is ca 170°C. Differential scanning calorimetry is also used to measure the kinetics and reaction enthalpies of hquid resins in coatings, adhesives, laminations, and foam. Software packages that interpret dsc scans in terms of the cure kinetics are supphed by instmment manufacturers. 

In order to optimize each embedding material property, complete cure of the material is essential. Various analytical methods are used to determine the complete cure of each material. Differential scanning calorimetry, Fourier transform-iafrared (ftir), and microdielectrometry provide quantitative curing processiag of each material. Their methods are described below. 

Strict control of the fusion process is imperative. In addition to thickness, hardness, continuity and adhesion checks, correct cure may be assessed by differential scanning calorimetry techniques, which are designed to measure any difference in the glass transition temperature of a laboratory-cured powder and the cured coating taken from the factory-coated pipe. 

Barton, J. M. The Application of Differential Scanning Calorimetry (DSC) to the Study of Epoxy Resins Curing Reactions. Vol. 72, pp. 111 — 154. 

This work discusses the thermal crosslinking and isomerization reactions occurring in the acetylene terminated isoimide prepolymer Thermid IP600. The techniques of Fourier Transform Infrared Spectrometry and Differential Scanning Calorimetry are used to determine the contribution of these two reactions during the thermal cure including their kinetics at 183° C. 

Differential scanning calorimetry (DSC) and thermomechanical analysis (TMA) were used to measure the glass transition temperatures (Tgs) of the uncured and cured AT-resins respectively (Figure 6). 

The initial Tg s found in column three of the table were determined by differential scanning calorimetry at a scan rate of 10°C/min. Final Tg s were determined by TMA on samples which had been cured in air at 550°F for 8 h. No residual exotherm was found in any of the samples when scanned by DSC following this cure cycle. 

Bisphthalonitrile monomers were cured neat, with nucleophilic and redox co-reactants, or in combination with a reactive diluent. Dynamic mechanical measurements on the resulting polymers from -150 to +300°C turn up several differences attributable to differences in network structure. Rheovibron results were supplemented with solvent extraction, differential scanning calorimetry (DSC), vapor pressure osmometry, and infrared spectroscopy to characterize the state of cure. 

Differential Scanning Calorimetry Analysis of the Thermal Curing of a,(O-bis (vinylbenzyl)PSU. Typical DSC curves for a,W-bis (hydroxyphenyl)-PSU and a,w-bis(vinylbenzyl)PSU are presented in Figure 4. The... 

Isothermal differential scanning calorimetry (DSC) measurements were carried out to investigate the curing kinetics [85]. Conversion vs time curves of DGEBPA-PACP systems prepared with 1 wt % of catalyst and without catalyst at identical curing temperature are overlaid in Fig. 31. 

The glass transition temperatures, specific for each thermosetting resin, are used to characterize cure kinetics. They can be measured by many techniques, of which the widely used are Differential Scanning Calorimetry (DSC) and Torsional Braid Analysis (TBA)... 

Differential Scanning Calorimetry (DSC) This is by far the widest utilized technique to obtain the degree and reaction rate of cure as well as the specific heat of thermosetting resins. It is based on the measurement of the differential voltage (converted into heat flow) necessary to obtain the thermal equilibrium between a sample (resin) and an inert reference, both placed into a calorimeter [143,144], As a result, a thermogram, as shown in Figure 2.7, is obtained [145]. In this curve, the area under the whole curve represents the total heat of reaction, AHR, and the shadowed area represents the enthalpy at a specific time. From Equations 2.5 and 2.6, the degree and rate of cure can be calculated. The DSC can operate under isothermal or non-isothermal conditions [146]. In the former mode, two different methods can be used [1] ... 

The purpose of the second dwell is to allow crosslinking of the matrix to take place. It is during the second dwell when the strength and related mechanical properties of the composite are developed. To characterize the exothermic crosslinking reaction of a thermosetting polymer matrix, a thermal cure monitor technique such as Differential Scanning Calorimetry... 

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