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(for some materials, the glass transition can be determined only using dynamic mechanical analysis [DMA]). A minimum of two samples should be tested. If a data sheet of the material is available, the measured value should correspond with the manufacturer s data (within the measurement accuracy of the equipment). The values of Tg1 and Tg2 (measured on the same sample) should not be more than 7 C apart. If Tg2 is significantly below the Tg1 measurement, this may be a strong first indication that resin system degradation has started during the measurement procedure. It is recommended to confirm this finding using the Td measurement procedure.
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Thermal Decomposition Temperature (Td) The determination of the thermal decomposition temperature (Td) completes the initial assessment. This is a new test methodology, and both ASTM and IPC test procedures are available. IPC-TM-650, method 2.3.40, is called Procedure to Determine the Thermal Decomposition Temperature Td Using Thermo Gravimetric Analysis (TGA), and the ASTM methodology is called Standard Test Method for Rapid Thermal Degradation of Solid Electrical Insulating Materials by Thermo Gravimetric Analysis. In both cases, the test methodology is based on thermogravimetric analysis (TGA) of a laminate specimen that is heated with a set ramp rate assessing the onset and process of decomposition. At first, the thermoset laminate resin passes the glass transition point where the polymer changes from a rigid, brittle, and glasslike state to a softer and more rubberlike material. As the material is heated further, the three-dimensional cross-linked structure begins to break down and individual bonds in the polymer structure open. As decomposition continues, gaseous decomposition products are set free, which can be detected as a loss of mass of the sample in test. This usually goes hand in hand with visible damage to the sample (delamination and/or strong discoloration) and significant changes in the mechanical properties of the laminate. A dry test specimen of 2 20 mg is heated at 5 C/min to 150 C and then held at that temperature for 15 min. This ensures that the sample is completely dry and establishes the base weight used to characterize the weight loss. Then the sample is heated at 5 C/min up to a temperature of 800 C and the weight loss is continually recorded. The temperature at which a 5 percent weight loss of the sample is detected is defined as the Td. Although this test methodology is a good gauge of the thermal stability of laminate materials, the method and results must be evaluated carefully to ensure that correct conclusions are drawn from the results. For example, the results of this test are dependent on the surface/ volume ratio of the specimen in test-specimens of the same weight, but different surface areas will show different results. The sample with the large surface area loses weight at a faster rate and therefore shows a lower Td. Samples with a large percentage of nondecomposing filler or reinforcement material will also behave differently as the measured weight change is based only on the resin content of the sample. This again will lead to a seemingly higher measured Td, which may lead to erroneous conclusions. Finally, the process of decomposition is as important as the determined value of Td and a comparison of the onset of weight loss may also be a valuable parameter to assess when comparing laminate materials using this methodology. In general, a higher Td value is desirable for materials that are being selected for lead-free assembly processes as this indicates that the laminate withstands the higher assembly temperatures with an increased margin. Figure 12.2 shows an example of different Td measurements for three different laminate materials. It shows the typical decomposition rates for some sample materials and also highlights how the assessment of a material can change if different criteria are chosen. If the IPC value of 5 percent weight loss is chosen, then M3 is superior to M1 and M2. But if the materials engineer decides that the onset of weight loss (decomposition) is critical for the application, then M3 is the worst performing material. The authors recommend using materials with a high onset temperature as well as a high 5 percent decomposition temperature.
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