Features
DSC can determine the melting point, crystallization temperature, and
glass transition point of a sample from the change in heat energy caused
by heating. It can also be used to determine crystallinity, purity,
reaction rate, and crystallization rate.
Application Examples
Structural change due to heating of the following materials:
Organic thin and thick films
Inorganic materials such as those in lithium-ion rechargeable
batteries
Principle
The heat-flux DSC continuously records the temperature difference
between a reference substance and the sample when heated
simultaneously.
From this temperature scan, the amount of heat, and the heat capacity
of the transition and/or reaction can be obtained. The method differs
from differential thermal analysis (DTA) in that the DSC temperature
difference is designed to be proportional to the input difference of the
thermal energy per unit time. As the temperature of the electric furnace
(heater block) increases at a constant rate, the reference sample and
the sample under measurement also increase at the same rate.
If an endothermic reaction occurs in the measurement sample, the
temperature rise stops while the reaction occurs, whereas it continues
in the reference sample. Hence, a temperature difference \(\mathrm{\Delta}T\) occurs between the two
samples.
\(\mathrm{\Delta}T\) is alleviated
by the heat flow flowing through the heat sensitive plate and the amount
of heat per unit time (heat flow) flowing into the sample is
proportional to the temperature difference between the two samples.
Therefore, by integrating \(\mathrm{\Delta}T\) with respect to time,
the heat generated/absorbed during the reaction can be determined, and
the heat capacity of the sample calculated.
Data example
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Figure 2. DSC charts
for a 1.130 mg In sample in an Al sample holder. The atmosphere was air,
temperature rise rate 20 \(℃\ \text{min}^{-
1}\), and sampling rate 10 Hz. When the heat flow decreases
(increases) by temperature, the reaction is endo (exo) thermic.
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Graphs in the format exemplified by Figure
2 (PDF file)
Numerical data of the graphs (Microsoft® Excel®
file)
Measurement specifications
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Outgassing may abort the measurement. Range must be below
decomposition temperature
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Constant temperature possible.
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Items for enquiries
Purpose and scope of the analysis
Desired measurement atmosphere, temperature range, temperature rise
rate
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Quantity, availability of pre-analysis samples
Shape, condition, size, possibility of destructive testing
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Desired delivery dates of preliminary and final results
Other relevant information
Caution
It may not be possible to measure samples that generate gases.
Contact us in advance to verify that the sample can be measured
This measurement is performed by MST’s subcontractor