Dynamical mechanical analysis

Other PDMS—sihca-based hybrids have been reported (16,17) and related to the ceramer hybrids (10—12,17). Using differential scanning calorimetry, dynamic mechanical analysis, and saxs, the microstmcture of these PDMS hybrids was determined to be microphase-separated, in that the polysiUcate domains (of ca 3 nm in diameter) behave as network cross-link junctions dispersed within the PDMS oligomer-rich phase. The distance between these... 

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). 

Glass-transition temperatures are commonly determined by differential scanning calorimetry or dynamic mechanical analysis. Many reported values have been measured by dilatometric methods however, methods based on the torsional pendulum, strain gauge, and refractivity also give results which are ia good agreement. Vicat temperature and britde poiat yield only approximate transition temperature values but are useful because of the simplicity of measurement. The reported T values for a large number of polymers may be found ia References 5, 6, 12, and 13. 

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... 

Thermal analysis iavolves techniques ia which a physical property of a material is measured agaiast temperature at the same time the material is exposed to a coatroUed temperature program. A wide range of thermal analysis techniques have been developed siace the commercial development of automated thermal equipment as Hsted ia Table 1. Of these the best known and most often used for polymers are thermogravimetry (tg), differential thermal analysis (dta), differential scanning calorimetry (dsc), and dynamic mechanical analysis (dma). 

Changes in heat capacity and measurement of T for blends have been used to determine components of copolymers and blends (126—129), although dynamic mechanical analysis has been found to give better resolution. Equations relating T of miscible blends and ratios of components have been developed from dsc techniques, eg, the Fox equation (eq. 1), where f the blend, or is the weight fraction of component 1 or 2,... 

In a similar fashion. Thermally Stimulated Current spectrometry (TSC) makes use of an appHed d-c potential that acts as the stress to orient dipoles. The temperature is then lowered to trap these dipoles, and small electrical currents are measured during heating as the dipoles relax. The resulting relaxation maps have been related to G and G" curves obtained by dynamic mechanical analysis (244—246). This technique, long carried out only in laboratory-built instmments, is available as a commercial TSC spectrometer from Thermold Partners L.P., formerly Solomat Instmments (247). 

Table 9. ASTM Standards on Dynamic Mechanical Analysis...

Thermal Properties. Spider dragline silk was thermally stable to about 230°C based on thermal gravimetric analysis (tga) (33). Two thermal transitions were observed by dynamic mechanical analysis (dma), one at —75° C, presumed to represent localized mobiUty in the noncrystalline regions of the silk fiber, and the other at 210°C, indicative of a partial melt or a glass transition. Data from thermal studies on B. mori silkworm cocoon silk indicate a glass-transition temperature, T, of 175°C and stability to around 250°C (37). The T for wild silkworm cocoon silks were slightly higher, from 160 to 210°C. 

The thermal glass-transition temperatures of poly(vinyl acetal)s can be determined by dynamic mechanical analysis, differential scanning calorimetry, and nmr techniques (31). The thermal glass-transition temperature of poly(vinyl acetal) resins prepared from aliphatic aldehydes can be estimated from empirical relationships such as equation 1 where OH and OAc are the weight percent of vinyl alcohol and vinyl acetate units and C is the number of carbons in the chain derived from the aldehyde. The symbols with subscripts are the corresponding values for a standard (s) resin with known parameters (32). The formula accurately predicts that resin T increases as vinyl alcohol content increases, and decreases as vinyl acetate content and aldehyde carbon chain length increases. 

Shock isolation is also possible usiag the dampiag characteristics of FZ elastomer. Dynamic mechanical analysis iadicates multiple transitions and a broad dampiag peak. This dampiag can be enhanced usiag formulatioas containing both siUca and carbon black fillers. 

In dynamic mechanical analysis of plastics, the material is subjected to a sinusoidal variation of stress and the strain is recorded so that 1, 2 and S can be determined. The classical variation of these parameters is illustrated in Fig. 2.55. 

The dynamic mechanical analysis of the ternary blends with 75 25 PVC-ENR bl6nd showed single Tg at all levels of XNBR concentrations, which indicates the miscibility of the system. In the 50 50 PVC-ENR blend, when the concentration of XNBR increased, the blend becomes progressively miscible. 

Thermal and thermomechanical analyses44 are very important for determining die upper and lower usage temperature of polymeric materials as well as showing how they behave between diose temperature extremes. An especially useful thermal technique for polyurethanes is dynamic mechanical analysis (DMA).45 Uiis is used to study dynamic viscoelastic properties and measures die ability to... 

A number of analytical techniques such as FTIR spectroscopy,65-66 13C NMR,67,68 solid-state 13 C NMR,69 GPC or size exclusion chromatography (SEC),67-72 HPLC,73 mass spectrometric analysis,74 differential scanning calorimetry (DSC),67 75 76 and dynamic mechanical analysis (DMA)77 78 have been utilized to characterize resole syntheses and crosslinking reactions. Packed-column supercritical fluid chromatography with a negative-ion atmospheric pressure chemical ionization mass spectrometric detector has also been used to separate and characterize resoles resins.79 This section provides some examples of how these techniques are used in practical applications. 

A difunctional bisphenol-A-based benzoxazine has been synthesized and characterized by GPC and 1II NMR (Fig. 7.39). A small of amount of dimers and oligomers also formed. Thermal crosslinking of bisphenol-A benzoxazine containing dimers and oligomers resulted in networks with relatively high Tgs. Dynamic mechanical analysis of the network showed a peak of tan 8 at approximately 185°C. 

Dynamic DSC, 409. See also Differential scanning calorimetry (DSC) Dynamic mechanical analysis (DMA), 138, 163, 241-242, 407, 409... 

Mechanical properties. See also Dynamic mechanical analysis (DMA) of polyamides, 138 of polyester LCPs, 52 of polyurethanes, 242-244 of semicrystalline aromatic-aliphatic polyesters, 45 Mechanical recycling, 208 Medical applications, for polyurethanes, 207... 

Dynamic mechanical analysis of siloxane-urea copolymers show a sharp loss peak around —110 °C corresponding to the Tg of the siloxane segment. The transition in... 

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