Original Article

Journal of Reinforced Plastics

and Composites

Environmental effects on viscoelastic 2014, Vol. 33(8) 749–757

! The Author(s) 2014
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DOI: 10.1177/0731684413515955
thermoplastic composites jrp.sagepub.com

Rogério L Mazur1,2, Pedro C Oliveira3, Mirabel C Rezende1 and

Edson C Botelho2

Abstract
In the last years, thermoplastic composites have been introduced as structural materials for high performance aerospace
applications. However, these materials can present problems when exposed to moisture, temperature, and UV radiation,
and besides it may occur as the synergy among the main degradation mechanisms. Among the thermoplastic composite
materials, carbon fiber reinforced poly(ether-ketone-ketone) (PEKK) laminates have shown excellent balance of proper-
ties, including high glass transition temperature, high strength, stiffness and fracture toughness values, low moisture
absorption, and good environmental resistance. The aim of the present work was to evaluate the influence of the
environmental effect on the viscoelastic behavior and glass transition temperature of carbon fiber reinforced PEKK
thermoplastic composites. In this work, the effects of environmental degradation on the viscoelastic properties of this
composite material were studied by dynamic mechanical analyses. The most significant change was observed for the UV
radiation accelerated weathering conditioning effects. A decrease of the storage modulus from 40 to 10 GPa and the Tg
from 147 to 105 C is observed, which decreases consequently the composite stiffness and the service temperature after
exposed environmental effects. A synergetic degradation mechanism between UV radiation accelerated weathering test
and hygrothermal conditioning is clearly verified.

Keywords
Polymer-matrix composite, environmental degradation, dynamic mechanical analysis

landing gear doors, floor panels, and mobile surfaces

Introduction
such as elevators, radomes, flaps, among others.1–4
Advanced composite materials have experienced a Among the available thermoplastic advanced com-
rapid development in aircraft and aerospace structures posites, carbon fiber reinforced poly(ether-ketone-
in the last years. According to the literature,1 some of ketone) (PEKK) shows excellent balance of properties,
the reasons for this development are significant pro- including excellent thermal stability, low moisture
gress in materials science and technology, with high absorption, excellent flammability resistance, high
values of mechanical strength and stiffness and low
density together with development of powerful and
sophisticated numerical methods for structural ana- 1
Divisão de Materiais – IAE, Departamento de Ciência e Tecnologia
lysis. Associated with this fact, the competitiveness
Aeroespacial (DCTA), São José dos Campos, São Paulo, Brazil
with conventional materials become equally important. 2
Materials and Technology Department – Universidade Estadual Paulista
Nowadays, other requirements such as quality assur- (UNESP), Guaratinguetá, São Paulo, Brazil
3
ance, reproducibility, and predictability of behavior Departamento de Quı́mica – Universidade de São Paulo (USP), Lorena,
over the lifetime of the structure are required.1 São Paulo, Brazil
Recently, thermoplastic composite materials have
Corresponding author:
increased their use in several applications. In the aero- Rogério L Mazur, Divisão de Materiais – IAE, Departamento de Ciência e
nautical field, this kind of composite has found utiliza- Tecnologia Aeroespacial (DCTA), São José dos Campos, São Paulo, Brazil.
tion in internal artifacts and wings of Boeing’s aircraft, Email: [email protected]

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750 Journal of Reinforced Plastics and Composites 33(8)

toughness, and tensile modulus. PEKK has a glass radiation, and temperature variation) on viscoelastic
transition temperature (Tg) of around 156 C and melt- behavior and glass transition temperature of carbon
ing temperature (Tm) between 305 and 310 C.5–8 fiber-reinforced PEKK thermoplastic composites.
The mechanical properties of polymer-matrix com-
posites can be affected by environmental conditions.
Composite materials are typically exposed to multiple Experimental
environments, such as moisture, temperature, UV radi-
ation, salinity, etc., during service, which leads to the
Materials
possibility of synergistic degradation mechanisms. Both Specimens of carbon fiber-reinforced PEKK thermo-
moisture and UV radiation have adverse effects on the plastic composites were produced by using hot com-
mechanical properties of the polymeric matrix and can pression molding. During the process, the appropriate
strongly affect the performance of the composite.9–14 thermal cycle obtained in previous work was used.5
Excess of moisture can cause the absorption of water PEKK amorphous thermoplastic polymer with glass
by the matrix and consequently generate the plasticizer transition temperature of 156 C and softening tempera-
effect that can reduce the glass transition temperature, ture of 310 C was used as matrix. Carbon fiber fabric
affecting the strength of adhesion between the fiber and style Plain Weave (PW) (282-3 K), supplied by Hexcel
matrix. Kinetics of moisture absorption in polymeric Composites, was used as reinforcement. The laminate
composite is governed by diffusion of water molecules was processed with around 60% of reinforcement con-
inside the micro gaps between polymer chains. Two tent in volume, according to the acid digestion experi-
other mechanisms are capillary transport into the ments carried out based on ASTM-D3171 (Procedure
gaps and flaws at the interfaces between fiber and the B) standard. The composite laminate quality was also
polymeric matrix, because of incomplete percolation evaluated by an optical microscopy from Olympus BH
during the manufacturing process, and transport of Company.
water by microcracks in the matrix.9–14
The absorption of UV photons by polymers results
in photo-oxidative reactions that can affect their chem-
Environmental conditioning
ical structure resulting in the material deterioration, In order to evaluate the influence of the environmental
thus causing chain scission and/or chain crosslinking. effects on the viscoelastic and glass transition tempera-
Chain scission decreases the molecular weight of the ture behaviors of carbon fiber reinforced PEKK
polymer, reducing the strength and heat resistance. thermoplastic composite, the specimens were exposed
On the other hand, chain crosslinking and/or reticula- to a combination of temperature, UV radiation, and
tion lead to excessive brittleness and can result in moisture in environmental conditioning chambers.
microcracking. However, for extended exposure to The hygrothermal conditioning has been performed
UV radiation, matrix-dominated properties can suffer according to Procedure B of ASTM D 5229 M-12
severe deterioration, for example interlaminar shear standard in conditioning chamber from
strength, flexural strength, and flexural stiffness can Marconi—MA835-UR. The moisture level in the
all decrease. The fiber-dominated properties, such as laminate was periodically monitored as a function of
tensile modulus and tensile strength, are usually not the time by measuring the weight of traveler samples till
affected significantly, especially the carbon fiber-rein- the moisture equilibrium state is reached. During con-
forced materials.9–13 ditioning, the temperature was set at 80 C and the rela-
In service, failures of carbon fiber-reinforced thermo- tive humidity (RH) in the chamber was set at 90%. The
plastic composites are commonly attributed to ageing of specimens were submitted to environmental condition-
the material in its particular environment, brought ing on a moisture chamber up to eight weeks. The mois-
about by a combination of the effects of heat, light, ture gain percentage (M) during water absorption was
water, and mechanical stresses on the material. determined by using the following equation.
Thermoplastic composites can present problems due to
its moisture absorption. When this occurs, the moisture Mu  Ms
M¼  100 ð1Þ
plasticizes the matrix and weakens the fiber and matrix Ms
interface, leading to a reduction of Tg and changes of
mechanical properties, such as Young’s modulus. As where Mu is the wet weight (g) of specimen and Ms is
discussed previously, the Tg is an important material the initial weight of dry specimen.
property because it defines the temperature at which The UV accelerated weathering test has been based
the material properties are drastically reduced.9–18 according to the ASTM D 4587-11 and ASTM D 4329-
The aim of the present study was to report the influ- 13 standards, in conditioning chamber from Q-Lab
ence of the environmental effects (moisture, UV Corporation – QUV/Spray. The composite specimens

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Mazur et al. 751

were exposed to a repeated cycles of 8 h of UV radi-

ation with a power of 0.76 W/(m2.nm) at 60 C and 4 h
of water condensation at 50 C with UVB-313 type hot
lamp. The specimens were removed after 200, 600,
1200, and 2400 h of exposure in order to verify possible
changes in material properties. The UV radiation inten-
sity is emitted and monitored constantly.
In order to evaluate the thermal cycling effects of
carbon fiber/PEKK thermoplastic composites on its
viscoelastic behavior, specimens were submitted in a
thermal shock conditioning chamber from
Envirotronics TSV. 5-2-2-2-A.C (Two zone vertical
thermal shock), as depicted in Figure 1. These compos- cool
ite specimens were exposed for 1000 cycles of 30 min at
50 C and 30 min at +80 C, in order to simulate the
operating temperature of the aircraft and evaluate the
influence of thermal shock in its viscoelastic behavior.
Figure 1. Thermal shock conditioning chamber operations
scheme ‘‘Two zone vertical thermal shock’’ (Adapted from:
Dynamic mechanical analysis Envirotronics Operating Manual).

The dynamic mechanical analysis (DMA) was used to

determine possible changes in the viscoelastic behavior As can be observed in Figure 2, for carbon fiber
and in the glass transition temperatures of carbon fiber reinforced PEKK thermoplastic composite specimens,
reinforced PEKK laminates. This analysis was per- the curves fit well to the Fickian diffusion model.11–18 It
formed using a Thermal Analyzer TA Instruments is characterized experimentally by an uptake of mois-
2980 equipment, operating in three-point bending hori- ture that reaches an asymptotic value after a period of
zontal measuring system. The experimental conditions time, and the diffusion mechanism can be quantified by
used were dynamic force of 0.7 Nm, oscillation dis- equation (2).12
placement of 10 mm, 1.0 Hz frequency, heating rate of
3.0 C/min, and temperature range from 30 to 250 C.  
MT
log ¼ log k þ n logðtÞ ð2Þ
M1
Results and discussion
where MT is the moisture content at time t, M1 is the
Kinetics of moisture absorption moisture content at the equilibrium, and k and n are
Figure 2 shows a graph of the weight increase as func- constants.
tion of the exposed time for the carbon fiber reinforced Figure 3 shows the behavior of the experimental
PEKK thermoplastic composite specimens exposed at data when is graphed log(MT/M/) versus log(t) of
80 C and 90% RH. From this figure, it is observed that carbon fiber reinforced PEKK thermoplastic compos-
the moisture content in the composite increases quickly ite, based on equation (1). As can be observed, the
in the first hours (up to 6 h), reaching a moisture value 0.38 obtained approaches towards to the
absorption of around 0.18 wt%. Afterwards, this ten- Fickian diffusion case, in which the rate of diffusion
dency slowly approaches saturation (50 days) after pro- is much lower than the polymer segment mobility and
longed time, reaching a maximum moisture absorption the equilibrium is rapidly reached, and it is maintained
of around 0.23%. Therefore, absorption water, a prob- with independence of time.
lem that has been extensively studied for epoxy,17
appears to be negligible for the PEKK. Rearranging the diffusion equation of Fick during
Moisture absorption in polymers takes place the initial absorption of moisture,12–13,18 equation (3)
through of a diffusion process, in which water mol- is obtained and the coefficient of diffusion (D) defined
ecules are transported from areas with high water con- as the slope of a plot of (Mt/M/) versus (t)1/2 has been
centration to areas with lower moisture concentration. obtained according to equation (4).
The diffusion process depends on the temperature and
the relative moisture absorption and generally it can be  
fit by second Fick’s law, as observed by several MT 4 D 0:5 0:5
¼ t ð3Þ
authors.11–18 M1 b 

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752 Journal of Reinforced Plastics and Composites 33(8)

0.25

0.20
Moisture absorption (%)

0.15

0.10
Specimem 1
Specimem 2
0.05 Specimem 3
Specimem 4
Specimem 5

0.00

0 5 10 15 20 25 30 35 40
Time1/2 (h)

Figure 2. Graph of moisture absorption as function of exposed time (square root of hours) of carbon fiber-reinforced PEKK
thermoplastic composite.

b2 slope2 
D¼ ð4Þ −0.1
42
−0.2
where b is the sample thickness.
The calculated moisture diffusion coefficient value −0.3
(D ¼ 16.5  106 mm2/s) is very low and is in the same
log (Mt/M∞)

range for polymeric composite (D & 106 mm2/s), as −0.4

can be observed in the literature.18 However, the diffu-
sion coefficient can be influenced negatively by incom- −0.5

plete percolation during the manufacturing process or

−0.6
transport of water by microcracks in the matrix.
−0.7
−0.6 −0.4 −0.2 0.0 0.2 0.4 0.6 0.8 1.0
Environmental effects on viscoelastic properties and log(t)
Tg values
Figure 4 shows the behavior of DMA as function of Figure 3. Graph of log (MT/M/) versus log(t) of carbon fiber-
temperature for the carbon fiber-reinforced PEKK reinforced PEKK thermoplastic composite.
thermoplastic composite specimens, after the hygro-
thermal conditioning and not weathered specimens.
According to these results from tan d analyses, it can
be observed in Figure 4(a) a little reduction of the Tg in samples increased with respect to the non-conditioned
around 1.8%, suggesting that the hygrothermal condi- sample. Analyzing the Tg, an 8.5% lower value is
tioning plasticizes the polymeric matrix and facilitates observed for the hygrothermically conditioned carbon
the movement of polymer chains with the temperature fiber-reinforced PEKK thermoplastic composite speci-
increase. mens, when compared with not weathered specimens. In
Figure 4(b) shows the results from storage modulus this case, probably there is a gradient of moisture con-
(E0 ) analyses. Considering the temperature of 30 C, it is centration through the specimen in the Tg region, and a
verified that there is a little difference. The data suggest corresponding distribution of temperature dependent of
that the storage modulus (E0 ) of the conditioned the molecular relaxation times. These results confirm the

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Mazur et al. 753

(a) (b) 40000

165°C
0.30
Not weathered 35000 153°C
Hygrothermal conditioned
0.25
30000 140°C

Storage Modulus (MPa)

162°C
0.20 25000
tan δ

20000
0.15

15000 Not weathered

0.10 Hygrothermal conditioned

10000
0.05
5000
0 50 100 150 200 250
Temperature (°C) 0 50 100 150 200 250
Temperature (°C)

(c) 6000
162°C
Not weathered
5000
Hygrothermal conditioned
Loss modulus (MPa)

4000
154°C

3000

2000

1000

0
0 50 100 150 200 250
Temperature (°C)

Figure 4. DMA analyses of hygrothermal conditioned carbon fiber reinforced PEKK thermoplastic composite and non-conditioned
samples: (a) tan d; (b) storage modulus (E0 ), and (c) loss modulus (E00 ).

results obtained from tan d analyses, indicating a plas- the UV radiation conditioning did not show significant
ticization of the thermoplastic matrix. influence on the studied polymeric samples and it was
Figure 4(c) shows the loss modulus (E00 ) results for not possible to establish some correlation with the glass
not weathered and hygrothermal conditioned speci- transition temperature.
mens. It is observed that the Tg shows a decrease of Figure 5(b) shows the storage modulus (E0 ) results.
5.2% in the hygrothermal conditioned carbon fiber- Considering the temperature of 50 C, E0 values of 40,
reinforced PEKK thermoplastic composite specimens, 26, 18, and 10 GPa can be observed. This analysis
when compared with not weathered specimens. These shows a sharp decrease in the storage modulus (E0 ) of
results confirm the results of Tg obtained from tan d the conditioned specimens and the modification of the
and E0 analyses, indicating the plasticization of the profile of these curves. As observed by several research-
thermoplastic matrix. ers,9,10 this behavior suggests a relation with the deg-
Figure 5 shows the behavior of DMA as function of radation process (rupture of molecular chain bonds)
temperature for the carbon fiber-reinforced PEKK associated with the reticulation process. When UV radi-
thermoplastic composite specimens, after to be condi- ation and moisture (plasticization) act together, the
tioned in UV radiation accelerated weathering tests up matrix-dominated properties can suffer severe deterior-
to 200, 600, 1200 and 2400 h. ation, and consequently, some mechanical properties
According to the tan d results, it can be observed in such as storage modulus of polymeric composite may
Figure 5(a) that UV radiation accelerated weathering be affected. Analysing the Tg, a decrease from 147, 130,
specimens present glass transition temperatures of 161, 106 to 105 C is observed for the conditioned specimens
165, 169, and 167 C, respectively. Only the specimens for 200, 600, 1200, and 2400 h under these conditions,
conditioned for 200 h present a lower value (2.5%), respectively. The observed decrease of both modulus
unlike the other samples. This analysis suggests that and Tg indicates an interfacial weakening in the fiber

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754 Journal of Reinforced Plastics and Composites 33(8)

(a) 0.28 (b) 45000

165°C 147°C
40000
200 h
0.24 200 h
35000 600 h
600 h 167°C
1200 h
1200 h

Storage Modulus (MPa)

130°C
0.20 30000 2400 h
2400 h

169°C 25000
tan δ

0.16
106°C
161°C
20000
0.12
15000
105°C
0.08 10000

5000
0.04
0
0 50 100 150 200 250 0 50 100 150 200 250
Temperature (°C) Temperature (°C)

(c) 4000
157°C
3500 200 h 160°C
600 h
3000 1200 h
2400 h
Loss Modulus (MPa)

2500

72°C
2000

162°C
1500
125°C
62°C
1000

500
118°C 162°C
0
0 50 100 150 200 250
Temperature (°C)

Figure 5. DMA analyses of UV radiation accelerated weathering test of carbon fiber-reinforced PEKK thermoplastic composite:
(a) tan d, (b) storage modulus (E0 ), and (c) loss modulus (E00 ).

and matrix interphase and a plasticizing effect on Tg is strongly affected by UV radiation. Thus, the Tg
PEKK, respectively. It should be remembered that obtained by E00 must be considered with some cau-
these temperatures (onset E0 ) are also considered as tion, because the UV radiation, in this case, did not
the most conservative Tg according to ASM show significant influence on material viscoelastic
Handbook—MIL 17. This behavior shows clearly the behavior. It is also known that UV radiation action
loss material elastic component, exposed to multiple occurs from the surface into the material, as men-
environments during service, caused by synergetic deg- tioned in the literature.9,10,19 However, different
radation mechanism (UV radiation and moisture). The from E00 , the Tg values obtained by onset E0 presents
decrease of elastic modulus and glass transition tem- significant differences due to the influence of the UV
perature indicates the decrease of the composite stiff- conditioning on the material stiffness. This correl-
ness after exposure to UV radiation and moisture. ation indicates that for structural applications, the
Figure 5(c) shows the loss modulus (E00 ) results for Tg obtained by E0 is much more suitable, as recom-
UV radiation accelerated weathering tests conditioned mend by literature.19
specimens. As can be observed, the weathered speci- Figure 5(c) also shows thermal transitions named
mens presented a Tg very close, i.e. at 157, 160, 162 sub-Tg. These transitions are classified in b and g and
and 162 C. This analysis suggests that the UV radi- their types of motion are related with increased mobil-
ation conditioning did not show significant influence ity in either side chains or small groups of adjacent
on molecular chain bond. However, when the Tg is backbone atoms, as recommend by the literature.20
analyzed according to E0 curves, it is verified that the The g transition is related to moisture absorption in

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Mazur et al. 755

(a) (b)
50000
0.30
165°C
45000
0.25 40000 155°C
Not weathered

Storage modulus (MPa)

Thermal shock 167°C
35000
0.20
30000
tan δ

153°C
0.15 25000

20000 Not weathered

0.10 Thermal shock
15000

0.05 10000

5000
0.00
0 50 100 150 200 250 0 50 100 150 200 250
Temperature (°C) Temperature (°C)

(c) 6000
162°C

5000 163°C
Not weathered
Thermal shock
Loss modulus (MPa)

4000

3000

2000

1000

0
0 50 100 150 200 250
Temperature (°C)

Figure 6. DMA analyses of thermal shock conditioned and non-conditioned of carbon fiber-reinforced PEKK thermoplastic com-
posite: (a) tan d, (b) storage modulus (E0 ), and (c) loss modulus (E00 ).

Table 1. Results of DMA analyses of carbon fiber-reinforced PEKK themoplastic composite of non-conditioned and conditioned
specimens.

Conditioning Non-cond. Hygrothermal Accelerated weathering test Thermal shock

Time (h) – 1440 200 600 1200 2400 1000

Tg by loss modulus ( C) 162 154 157 160 162 162 163
Tg by storage modulus ( C) 153 140 147 130 106 105 155
Tg by tan d ( C) 165 162 161 165 169 167 167
E0 (Gpa) at 50 C 35 36 40 26 18 10 50

the polymer. These transitions (b mainly) are also presence of tan d peaks at 62, 72, 118, and 125 C, for
related with impact damping/strength of the material. exposition times of 200, 1200, and 2400 h, respectively.
As can be observed, the weathering effect by UV radi- Figure 6 shows the DMA behaviors as function of
ation on polymeric composite contributes is probably temperature of carbon fiber-reinforced PEKK thermo-
due to the moisture absorption process by the polymer plastic composite specimens, after the thermal shock
polymeric matrix. This phenomenon is shown by g tran- conditioning.
sitions present in the composite exposed at 200, 1200, According to the tan d analyses, it is observed in
and 2400 h. In this case, the Tg is characterized by the Figure 6(a) that the thermal shock conditioned

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756 Journal of Reinforced Plastics and Composites 33(8)

specimens presented the glass transition temperature at radiation accelerated weathering test and the hygrother-
167 C, 1.2% higher than non-conditioned samples. mal conditioning.
Figure 6(b) shows the storage modulus (E0 ) analyses.
Considering the temperature of 50 C, it is observed Acknowledgement
that the storage modulus (E0 ¼ 48 GPa) is 37%
The authors acknowledge the financial support received from
higher than that obtained for not weathered
CAPES and CNPq (Project no. 159815/2011-8, 305478/2009-
specimens (E0 ¼ 35 GPa). Furthermore, it is verified 5 and 302115/2009-9).
that the Tg by onset of storage modulus increases
slightly (1.3%) for the specimen submitted to thermal
shock effect (155 C) in comparison to that not wea- Funding
thered (153 C). These results suggest that the thermal This research received no specific grant from any funding
shock increases the stiffness slightly but did not affect agency in the public, commercial, or not-for-profit sectors.
the Tg.
Table 1 summarizes the results obtained in the References
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