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FIGURE 12.5 Typical TMA scan.
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The test procedure is specified in IPC-TM-650, method 2.4.25C. The specimen should be a solid piece weighing between 15 mg and 25 mg. In the case of very thin materials, multiple pieces may be used. The specimen should be of the size and configuration that fits within the sample pan of the DSC equipment. All of the specimen preparation needs to take place before preconditioning to avoid any moisture influence prior to testing. Sample edges should be smoothed and burrs removed by light sanding or an equivalent method to achieve proper thermal conduction. Use care to minimize stress or heating of the specimen. Even though the IPC test method allows samples to be tested with copper cladding, the authors recommend testing only without copper cladding.This increases the relative mass of polymer in the DSC sample pan and leads to a better signal and detection of Tg. The samples need to be preconditioned for 2 hours at 105 C (221 F), then cooled to room temperature in a desiccator for at least a half-hour prior to testing. Place the specimen in a standard aluminum sample pan with an aluminum lid. For reference purposes, a cover lid crimped onto the sample pan should be used. Start the scan at a temperature at least 30 lower than the anticipated onset of Tg. Unless otherwise specified, a scan at a rate of 20 C/min (36 F/min) is recommended and the temperature ramp needs to be continued at least 30 C (54 F) above the anticipated transition region. The glass transition temperature is determined using the heat flow curve. In many cases, the DSC equipment will have applicable software installed to determine Tg. A tangent line is fit onto the curve above the transition region, and a second tangent line is fit below the transition region. The temperature on the curve halfway between the two tangent lines, or 1/2 d Cp, is the glass transition point Tg. Figure 12.6 shows an example of a DSC scan where the material has been scanned twice.The Tg of the first scan was 192.9 C. The second scan yielded a slightly higher value of 195.3 C (likely caused by additional curing of the material).
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FIGURE 12.6 Example of a DSC result.
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12.5.2.1.3 Tg by Dynamic Mechanical Analysis (DMA). Dynamic mechanical analysis applies an oscillatory stress or strain on the sample while the temperature is increased during the experiment. The ability of the material to elastically store the mechanical strain energy changes during the heat cycle as it changes its viscoelastic behavior from glassy to rubbery. This property change determines the glass transition temperature by DMA. The test procedure is specified in IPC-TM-650, method 2.4.24.2. The test specimen should consist of a strip of laminate material compatible to the measuring equipment. For all samples with woven reinforcement, it is necessary to make sure that the specimens are cut parallel or perpendicular to the woven structure. The analysis is based on an assumption of constant specimen geometry; therefore, the test specimens must be stiff enough not to deform plastically during the experiment. All copper needs to be etched off. While the IPC-method recommends preconditioning of the samples at 23 C and 50 percent RH for at least 24 hours prior to testing, the authors recommend preconditioning similar to that employed for TMA or DSC measurements. Samples are baked for 2 hours at 105 C (221 F), then cooled to room temperature in a desiccator for at least a half-hour prior to testing. The sample is mounted in the fixture making sure that it is perpendicular to the clamps. Both clamps are tightened using torque screwdrivers to ensure that the sample does not slip during the measurement and that no stresses have built up around the sample that could negatively influence the results. The sample is loaded with a frequency of 1 Hz (6.28 radian/sec) while it is heated in dry nitrogen or dry air at a rate of no faster than 2 C per min. The temperature ramp needs to be continued at least 50 C above the transition region. The glass transition temperature is defined as the temperature corresponding to the maximum in the tan d versus temperature curves at a frequency of 1 Hz. Tan d is calculated from Eq. 12.3. tan d = E /E (12.3)
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