Curing dynamic mechanical analysis,

The volatile content of the treated paper is important because moisture acts as a temporary plasticizer to promote resin flow during early stages of pressing (9). Dynamic mechanical analysis of the treated paper is a very useful means to study the initial flow stages of a resin and the cure time required to complete cross-linking (10). 

The principal techniques for determining the microstmcture of phenoHc resins include mass spectroscopy, proton, and C-nmr spectroscopy, as well as gc, Ic, and gpc. The softening and curing processes of phenoHc resins are effectively studied by using thermal and mechanical techniques, such as tga, dsc, and dynamic mechanical analysis (dma). Infrared (ir) and electron spectroscopy are also employed. 

Dynamic mechanical analysis provides a useful technique to study the cure kinetics and high temperature mechanical properties of phenoHc resins. The volatile components of the resin do not affect the scan or limit the temperature range of the experiment. However, uncured samples must be... 

Gel time values of the three systems measured as abrupt change in the slope of G (t) under isothermal curing conditions show that gelation occurs earlier in PWE system at all temperatures considered as shown in Table 11.27. ETPI behaves like a catalyst for the primary epoxy-amino reaction which dominates the cure until vitrihcation occurs. Dynamic mechanical analysis and dielectric spectroscopic analysis carried out by the authors also confirm the above conclusions. 

In the absence of co-reactants, it is supposed that the polymerization is promoted by traces of water or other nucleophiles, since very pure monomer does not gel even after extended heating. Conversely, gelation may be accelerated by addition of phenols such as bisphenol A. Dynamic mechanical analysis of cured resins confirms that they are practically identical whether or not the phenol is added. 

An appropriate cure cycle was established based on the results obtained from the thermal analysis and cure rheology studies of the resin and cured BCB bar and dogbone shaped samples were fabricated for testing. Bar shaped specimens had the dimensions of 3.5 x 0.5 X 0.125 and were used to stake compact tension specimens for fracture toughness studies and for dynamic mechanical analysis of a torsion bar. Dogbone shaped specimens for tensile tests had a gauge area of 1 x 0.15 and were approximately 0.040 thick. 

Thermal analysis, moisture uptake and dynamic mechanical analysis was also accomplished on cured specimens. Thermal analysis parameters used to study cured specimens are the same as those described earlier to test resins. The moisture uptake in cured specimens was monitored by immersing dogbone shaped specimens in 71 C distilled water until no further weight gain is observed. A dynamic mechanical scan of a torsion bar of cured resin was obtained using the Rheometrics spectrometer with a temperature scan rate of 2°C/minute in nitrogen at a frequency of 1.6Hz. The following sections describe the results obtained from tests run on the two different BCB resin systems. Unless otherwise noted all tests have been run as specified above. 

The complex sorption behavior of the water in amine-epoxy thermosets is discussed and related to depression of the mechanical properties. The hypothesized sorption modes and the corresponding mechanisms of plasticization are discussed on the basis of experimental vapor and liquid sorption tests, differential scanning calorimetry (DSC), thermomechanical analysis (TMA) and dynamic mechanical analysis. In particular, two different types of epoxy materials have been chosen low-performance systems of diglycidyl ether of bisphenol-A (DGEBA) cured with linear amines, and high-performance formulations based on aromatic amine-cured tetraglycidyldiamino diphenylmethane (TGDDM) which are commonly used as matrices for carbon fiber composites. 

Dynamic mechanical analysis methods are frequently used to investigate polymerization and curing processes in reactive systems. These methods allow us to obtain both relative and absolute rheological characteristics of a material. Measurements can be made in both the fluid and solid states without affecting the inherent structure of the polymerizing system. 

One of most popular techniques for dynamic mechanical analysis is the torsion pendulum method. In a modification of this method designed to follow curing processes, a torsion bar is manufactured from a braid of fibers impregnated with the composition to be studied this is the so-called torsional braid analysis (TBA) method.61 62,148 The forced harmonic oscillation method has been also used and has proven to be valuable. This method employs various types of rheogoniometers and vibroreometers,1 9,150 which measure the absolute values of the viscoelastic properties of the system under study these properties can be measured at any stage of the process. The use of computers further contributes to improvements in dynamic mechanical analysis methods for rheokinetic measurements. As will be seen below, new possibilities are opened up by applying computer methods to results of dynamic measurements. 

In more recent studies from Gonzalez and co-workers [88-90] it was concluded from dynamic mechanical analysis of peroxide-cured NR that a non-uniform crosslinked network results if a large amount of peroxide is used. This result seems to be in line with the optical spectroscopy studies discussed. 

Glass transition temperatures (T ) were determined for partially cured resins as a function of the extent of cure by dynamic mechanical analysis. 

In dynamic mechanical analysis for thermosetting systems the principal use is to monitor the glass-transition temperature (Tg). In a DMTA Tg is defined as the maximum in loss modulus, loss compliance or loss tangent. For example. Figure 3.57 (Prime, 1997a) shows the various transitions for a cured magnetic ink coating that had previously been cured under air and N2. 

Figure 9. Results of dynamic mechanical analysis, showing loss factor as a function of temperature for unmodified epoxy (dashed curve), epoxy containing 28 wt% ETBN (dotted curve), epoxy containing 28 wt% PPU (dotted-dashed curve), and epoxy containing a blend of 14 wt% ETBN and 14 wt% PPU (solid curve). Epoxy formulation 100 parts ofbisphenol A diglycidyl ether (5.4 mol epoxy/kg), 5 parts of butane-1,4-dioldiglycidyl ether, 5 parts of dicyandiamide, 0.5 part of chlorotolurone accelerator, and 1 part of pyrogenic silica (Aeorosil 380). Cure 1 h at 140 °C, 1 h at 160 °C.

Dual Cure. Films were prepared for Dynamic Mechanical Analysis (DMA). All films were cast on release paper with a 4.5 mil draw down bar, and partially cured with two 200 watt/inch lamps at half power and a belt speed of 200 ft/min. The films were intentionally under cured to facilitate cutting with minimal flaws. After the films were cut into ii-inch test pieces, they were cured with two 200 watt/inch lamps at 100 ft/min, equal to 260 millijoules/cm dose. The instrument used for the DMA work was a Rheometrics RSA II Solids Analyzer. All tests were made at a frequency of 11 hz with a nominal strain of 0.05%, under nitrogen. Both temperature scans, at 2°C/minute, and isothermal runs were made. 

Demonstration of Dual Cure. To demonstrate thermal cure after UV cure three sets of films were prepared for Dynamic Mechanical Analysis (DMA). In the first set, four formulations were based on AM 1, AH 2, the epoxy acrylate, amd the urethane acrylate. Formulations used the test resin at 65% in TPGDA, and included 3% Darocur 1173 as a source of free radicals. DMA plots for the epoxy acrylate and urethane acrylate are shown in Figure 9. The elastic or storage modulus (E ) in the rubbery region is often used as a measure of crosslink density. The maximum of the tan delta plot, not shown, is... 

Dynamic mechanical analysis DMA Frequency Phase changes, polymer curing... 

Dynamic mechanical analysis DMA Moduli Phase changes, glass transitions, polymer cure... 

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