SAMPE Journal - January/February 2022 - 12

FEATURE / PAN-BASED CARBON FIBRES
furnace is divided into the low-temperaturefurnace
and the high-temperature-furnace. The
same process parameters are used to produce
a reference fibre by thermal conversion of an
untreated PAN precursor. Samples are taken and
analyzed prior to stabilization and after each oven
during stabilization.
RESULTS
Figure 4 and Figure 5 show the comparison of the
stabilization degree between treated PAN fibres
and the untreated reference fibres throughout the
stabilization process.
With both the KMnO4
- and the N2
-pretreatment
the stabilization degree prior to the stabilization
of the pretreated fibres is even higher than the
degree of stabilization of the reference fibres
after stabilization oven 1. This means that the
conventional stabilization process could be
adjusted and the oven 1 can be skipped. Throughout
the stabilization until after oven 3 the pretreated
fibres show a higher degree of stabilization than
the untreated reference fibres which indicate
higher reaction speeds caused by the pretreatment
process. For further investigations, the FTIR
spectrum of the fibre samples have to be analyzed
(Figure 6).
While the FTIR spectrum of the KMnO4
-
pretreated fibres haven't shown any clear signs of
improved numbers of functional groups which
indicate a high reactions speed during stabilization
process, a proof for the effectiveness of the N2
-
pretreatment can be seen in Figure 6. The C=C,
C=N, N-H-group is the main indicator for the
cyclization process which forms with proceeding
cyclization a more and more distinct minimum
of transmission19
. It can be clearly seen that
the minimum of the pretreated fibres is always
significantly lower than that of the reference fibres
until after oven 2. This observation proves that the
pretreatment with N2
Figure 4. Comparison of stabilization degree between KMnO4-treated fibres
with reference fibre.
Figure 5. Comparison of stabilization degree between N2-treated fibres with
reference fibre.
in fact effect the reaction
speed and thus the speed for the formation of
cyclized areas within the PAN fibre.
The results of the analysis of the mechanical
properties are presented in Figure 7.
The pretreatment methods have a positive
effect on the tensile modulus of the resulting carbon
fibres. With the KMnO4
- and the N2
-pretreatment
methods the E-modulus of the carbon fibres were
increased by 6 and 8,5% in comparison to the
reference.
CONCLUSIONS
With both the KMnO4
- and the N2
-pretreatment
methods at least one of the four stabilization
Figure 6. FTIR spectrum of N2-treated fibres in comparison to reference
fibre (prior stabilization, after oven 1 and 2).
ovens can be skipped since the thermal or thermochemical treatment of
PAN fibres promote the desired reactions during the pretreatment as well as
the stabilization process. With a pretreatment time of only a few minutes the
stabilization time could be reduced by at least 11 - 20% (Figure 8). This means
that not only the production time could be lowered but also the investment
costs for future productions lines. Further, the tensile modulus of the carbon
12 | SAMPE JOURNAL | JANUARY/FEBRUARY 2022
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SAMPE Journal - January/February 2022

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SAMPE Journal - January/February 2022 - Cover1
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