Differential Scanning Calorimetry (DSC) is a thermal analysis technique used
to measure changes in heat flows associated with material transitions. DSC
measurements provide both qualitative and quantitative data on endothermic
(heat absorbing) and exothermic (heat evolving) processes. DSC is commonly
used to determine the glass transition temperature and crystalline melting
point of polymeric materials.
A simplified explanation of a DSC sample evaluation may be described as
follows. A material specimen is weighed and placed into a DSC sample pan.
The sample pan and an empty reference pan are placed within the DSC apparatus.
The DSC cell is heated or cooled at some controlled rate while continuously
monitoring the differential heat flow between the sample and reference pans.
The heat flow profile so obtained during the DSC heating or cooling run is
subsequently analyzed for any of several endothermic and/or exothermic
transitions.
Examples
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The DSC technique can be used to make qualitative statements about whether
or not polymer blend systems are miscible or immiscible, provided the
inherent homopolymer transition temperatures of the blend components are
sufficiently well separated. A description of the glass transition
temperature characteristics of two different polymer blend systems
evaluated by DSC will illustrate this point. Polymer blends based on
polystyrene (Tg = 100°C) and poly(dimethylphenylene oxide)
(Tg = 210°C) are miscible in all proportions. DSC thermal profiles
of various PS/PDMPO blend compositions show only a single glass transition
temperature, located somewhere between 100°C and 210°C, dependent
upon the relative weight fractions of the homopolymer components within the
blend. In contrast, polymer blends based on polystyrene and polyisoprene
(Tg = -70°C) are immiscible. PS/PI blends exhibit distinct phase
separated domains and show two characteristic glass transition temperatures
in the same temperature ranges as their respective homopolymer blend
components. In summary, polymer blend systems which show two Tgs by DSC are
recognized as being immiscible; those which show only a single Tg may or may
not be miscible.
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TeflonTM samples are manufactured using different processing conditions,
which directly influence the extent of crystallinity in the finished parts.
Using the heat of fusion of an ideal, 100% crystalline sample, the percent
crystallinity of manufactured samples may be determined by DSC. Specifically,
a TeflonTM sample was heated in a DSC cell and showed a characteristic
endothermic melting peak. The peak area was normalized and integrated to
quantify the experimental heat associated with the crystalline melting
process. By comparing the experimental heat value to that of a theoretical,
100% crystalline sample, the percent crystallinity of the sample was determined.