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Advanced Industrial and Engineering Polymer Research 2 (2019) 136e142

Contents lists available at ScienceDirect

Advanced Industrial and Engineering Polymer Research


journal homepage: http://www.keaipublishing.com/aiepr

Fatigue analysis and fatigue reliability of polypropylene/wood flour


composites
Md Minhaz-Ul Haque a, b, *, Koichi Goda a, Shinji Ogoe c, Yuta Sunaga d
a
Department of Mechanical Engineering, Yamaguchi University, Ube, Yamaguchi, 755-8611, Japan
b
Department of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, Bangladesh
c
Technology Development Centre, TOCLAS Co., Shizuoka, 432-8001, Japan
d
Kayaku Akzo Co., Sanyoonoda-City, Yamaguchi, 757-0002, Japan

a r t i c l e i n f o a b s t r a c t

Article history: Fatigue analysis and fatigue reliability of polypropylene (PP)/wood flour (WF) composites were studied.
Received 12 March 2019 The composites were prepared by incorporating wood flour with and without maleic anhydride and
Received in revised form peroxide (MAPO) into cellulose nanofibres impregnated polypropylene. The prepared composites were
22 April 2019
then characterized by tensile and fatigue analyses. The tensile strength and fatigue life of MAPO mixed
Accepted 4 July 2019
composites were lower compared with the composites without MAPO. It was also found that the fatigue
experimental data of the composites were widely scattered regardless of the type of composites. Hence,
Keywords:
in this study, a fatigue reliability of the composites was sought. Based on the fatigue experimental data,
Melt-viscosity
Wood plastic composite (WPC)
95% confidence band were created. Since 95% confidence lower band ensure 95% survivability and only
Fatigue behavior 5% failure of the composites, hence, from this study, it is suggested that the fatigue life obtained from 95%
Wood flour confidence lower band can be used as a material reliability index for safe fatigue design of the
Polypropylene composites.
© 2019 Kingfa SCI. & TECH. CO., LTD. Production and Hosting by Elsevier B.V. on behalf of KeAi
Communications Co., Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction the attention of WPC companies because of the free flowing nature
of WF compared with the natural fibres [12] as well as scope of
Application and demand of wood-plastic composite (WPC) in fabrication from recycled wood and recycled polypropylene
different sectors such as automotive industries, office appliances, [13e17].
housewares, furniture, outdoor deck floors, etc. [1e5] are In this study, PP/WF composites were fabricated by incorpo-
increasing each year due its cheapness and eco-friendly character. rating wood flour with and without maleic anhydride and peroxide
The major components of WPC are wood flour and mainly ther- (MAPO) into cellulose nanofibres (CNF) impregnated poly-
moplastic polymers such as polyethylene, polypropylene, polyvinyl propylene. Cellulose nanofibres was impregnated into PP matrix to
chloride etc. Wood flour as an inexpensive filler can reduce the cost increase the interfacial interaction among composite components.
of WPC largely [1]. Presence of wood flour into polymer matrices The advantages of addition of CNF into PP polymer had already
can also impart its physical and mechanical properties such as high been reported by Suzuki et al. [18,19]. In our previous study, a
strength and stiffness to the final composite materials. Poly- higher fatigue life of wet pulverized WF reinforced PP composite
propylene (PP)/wood flour (WF) composite, a typical WPC, is was reported [20,21]. Indeed, fibrils were generated on wood flour
basically made of polypropylene matrix and wood flour. In the particles surfaces by the wet pulverization. An improved fatigue life
fabrication of PP/WF composite, another important ingredient, of PP/WF composite was also claimed due to a higher crack
namely, maleic anhydride grafted polypropylene (MAPP), is usually deflection behavior of fibrillated WF. The improved fracture
used as a compatibilizer [6e11]. PP/WF compositess have drawn toughness and fatigue life of various nanoparticles incorporated
polymer systems had already been reported by several researchers.
As for examples, improved fatigue life and fracture toughness of
epoxy composites were found by incorporating carbon nanotube
* Corresponding author. Department of Mechanical Engineering, Yamaguchi
University, 2-16-1 Tokiwadai, Ube, Yamaguchi, 755-8611, Japan. [22], multi-walled carbon nanotube [23,24], graphene nano-
E-mail address: minhaz1978@gmail.com (M.M.-U. Haque). particles [25,26] etc.

https://doi.org/10.1016/j.aiepr.2019.07.001
2542-5048/© 2019 Kingfa SCI. & TECH. CO., LTD. Production and Hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
M.M.-U. Haque et al. / Advanced Industrial and Engineering Polymer Research 2 (2019) 136e142 137

Although the demand and application of PP/WF are increasing Cellulose nanofibres (CNF) suspension (solid content 10 wt%),
each year, use of PP/WF in structural applications faces a great BiNFi-s WFo-10010, fibres diameter 10e50 nm, specific surface area
challenge because of their fatigue reliability under different load 120 m2/g were supplied from Sugino, Japan.
conditions. Structural materials are susceptible to fatigue failure Wood flour (WF), trade name ARBOCEL®C100, bulk density
below the tensile strength of that material. Hence, for safe fatigue 140e180 g/l, mesh number 100, particle size 70e152 mm was pur-
design, the study of fatigue behavior of the composites is very chased from Rettenmaier & Sohne GmbH Co., Ltd., Rosenberg,
important, particularly if PP/WF composites are subjected to use in Germany.
long-term load bearing applications. Since materials deformation Maleic anhydride, purity 99.5%, solidifying point 52  C, was
mechanism under short-term and long-term mechanical loading is purchased from Nippon Shokubai Co. Ltd., Japan.
not always the same, and only the tensile test is not sufficient to do Organic peroxide, t-Butyl peroxy 3,5,5-trimethylhexanoate,
a prediction of their long term load bearing application [27]. purity 97 wt%, half life at 120, 140, 160, and 180  C, are about 1 h,
Generally, fatigue strength depends on the tensile strength of 10 min, 1 min, and 15 s, respectively were purchased from, Kayaku
composite materials and composite materials with higher tensile Akzo Co., Japan.
strength exhibited higher fatigue strength [28,29], but this was not
always happen, particularly at low cyclic stress. Liang et al. [30] and 2.2. Processing of the composites
Shivakumar et al. [31] reported that the higher tensile strength of
composites became less significant when cyclic stress was The PP/WF composites were prepared in three step processes. In
decreased i.e. at low cyclic stress some composite materials were the 1st step, cellulose nanofibres were dispersed into poly-
less sensitive to the fatigue damage. Hence, the study of fatigue propylene matrix by mixing of CNF suspension (solid content 10 wt
analysis and fatigue reliability of PP/WF is utmost necessary for safe %) with MAPP and neat PP at 190  C in a mixer. The mixing ratio of
fatigue design. PP, MAPP, and CNF was 90:5:5.
Prediction of fatigue life of composite materials is also a critical In the 2nd step, mixture of PP/CNF (20 wt%) and wood flour
issue as fatigue experimental data of composites are widely scat- (WF) (80 wt%) with and without maleic anhydride (2 phr) and
tered. Crack propagation rate for a uniform material was predicted peroxide (0.5 phr) was obtained by mixing them in a mixer at
by a linear elastic fracture mechanics of a single through-crack. 120e180  C for 5e20 mins.
However, in composite material, fatigue occurs by fibre breakage, In the 3rd step, the ground mixture were processed in a twin-
matrix cracking, crazing, matrix-fibre debonding, delamination etc. screw extruder (AS30, Nakatani, machinery, Co., Ltd.) by the addi-
Moreover, in a composite, due to its heterogeneity, cracks were tion of required amount of neat PP so that the components
spread to the entire area and some cracks could not propagate over composition wt% in each final composite become PP45/MAPP2.5/
large distance as they were deflected/arrested by hard filler [32]. CNF2.5/WF50. During processing of the composites, the tempera-
Thus, due to the heteroginity of composites the fatigue experi- ture at different zones in the extruder were maintained as fol-
mental data of composites are widely scattered. lowings: (1) 165  C, (2) 200  C, (3) 215  C, (4) 200  C, (5) 190  C, and
The main objective of this study was to find out a fatigue reli- (6) 190  C. The screw speed of extruder was 85 rpm and total
ability of PP/WF composites. In this study, effect of MAPO mixing on throughput was 9e12 kg/h. The processed composites based on
the fatigue life of PP/WF composites was also investigated. Maleic different conditions were coded as reported in the Table 1.
anhydride has two functional groups: anhydride group and double
bond. So, each molecule of maleic anhydride has possibility to be 2.3. Characterization techniques
bonded with PP radical as generated by peroxide through double
bond [33,34] as well as to be bonded with WF surfaces through Tensile test of dumbbell shaped specimens, obtained by injec-
anhydride group [35,36]. Based on this reaction probability, it was tion molding, of PP/WFcomposites was carried out by a Material
expected that the resultant composite system would exhibit an Testing Machine, EHF-F1, Shimadzu, Japan. A strain gauge (Kyowa
improved fatigue performance due to a higher components com- strain gauge, KFGS-2N-120-C1-11, Japan) of 2 mm with a gauge
patibilization. Concerning the fatigue reliability of the composites, factor of 2.14 ± 1.0% was inserted on the surface (at the middle
since fatigue experimental data are widely scattered, it is necessary point) of each specimen. The specimens were put in a humidity
to find out absolution that can be employed to calculate the safe control chamber at 25  C with 40% relative humidity (RH) for 5
fatigue design of the composites. In this study, the experimental days. The conditioned specimens were then tested using a load cell
data were fitted with a logarithmic linear line by a regression of 1 kN, gauge length of 18 mm and cross-head speed of 10 mm/min
technique. Based on the fatigue testing data, 95% confidence band at 25  C and 40% RH. The average maximum strength of composites
were also created. Since 95% confidence lower band ensure 95% was calculated by performing the test on five specimens of each
survivability and only 5% failure of the composites, hence, in this material.
study, fatigue lives of composites at different fatigue strength, Fatigue tests of the composite specimens were carried out by
based on 95% confidence band, were calculated that can be used the same instrument which was used for the tensile test. The
as a material reliability index for safe fatigue design of PP/WF fatigue test of the composites was also conducted at conditions
composites. of 25  C and 40% RH. The average maximum tensile strength
value, obtained by tensile test, was used as a reference
2. Experimental maximum stress level in estimation of the applied stress. The
following test conditions such as tension-tension loading mode,
2.1. Materials stress ratio 0.1, frequency 3.5 Hz and applied stress: 90, 80, 70
and 60% level of ultimate tensile strength were applied in fa-
Polypropylene (PP) pellet, trade name PPJ107G, melt flow index tigue test. At each load, at least two specimens of the compos-
30 g/10 min at 230  C/2.16 kg, density 0.9 g/cm3, melting point ites were tested.
150  C was received from Prime Polymer Co., Ltd., Tokyo, Japan. Measurements of rheological properties were performed using a
Maleic anhydride grafted polypropylene (MAPP) powder, trade capillary rheometer, LCR 7000, Dynixco, Japan. The diameter and
name Kayabrid 006PP, maleic anhydride content 2 wt%, was length of the capillary were 2 mm and 8 mm, respectively. Tests
received from Kayaku Akzo Co., Japan. were carried out at 180  C and at shear rates 100, 149, 223, 334 and
138 M.M.-U. Haque et al. / Advanced Industrial and Engineering Polymer Research 2 (2019) 136e142

Table 1
List of composite samples with their code.

Sample code Mixing conditions

Temperature ( C) Time (min) Maleic anhydride (phr) Peroxide (phr)

A 140 10
B 140 10 2 0.5
C 120 10 2 0.5
D 140 20 2 0.5
E 160 10 2 0.5
F 180 10 2 0.5
G 180 5 2 0.5
H 180 20 2 0.5

500 s1. From this test melt-viscosity of PP/WF composites were attempted to find a solution for fatigue reliability of PP/WF com-
measured. posites. To study the fatigue performance of the composites,
maximum stress versus number of cycles to fracture (SeN) curves
3. Results and discussion of the composites were plotted using the fatigue experimental data.
The data were then fitted in a logarithmic linear regression equa-
3.1. Tensile properties of the composites tion as shown below:

To determine the cyclic stress level of fatigue test, each com- smax ¼ b,logðNÞ þ c (1)
posite sample was firstly subjected to the tensile test. Fig. 1 repre-
where, smax is the applied maximum stress and N is a number of
sents a stress-strain curves with an over imposed column diagram
cycles to fracture. The values of b and c are constant and depend on
of tensile strength of neat PP and composites. The average tensile
the type of materials. For each and every composite material the
strength values and average toughness values calculated from the
values of correlation coefficient and R2 were found to be
stress-strain curves of different PP/WF composites are also reported
about 0.83 and >0.98, respectively. The value of correlation
in Table 2. In Fig. 1, it is noticed that the MAPO containing com-
coefficient, 0.83 indicated a strong downhill (negative) linear
posites BeH exhibited lower tensile strength compared with
relationship. The above regression equation (1) is similar to the
composite A. The lower tensile strength of MAPO containing
fatigue model equation developed by Mandell [40,41]:
composites BeH was probably due to the molecular degradation of
PP polymer by MAPO [37].
smax ¼ b,logðNÞ þ suts (2)
Although a little influence of MAPO mixing temperature and
time on the tensile strength of MAPO containing composites was where, suts is ultimate tensile strength. Fatigue strengths of
noticed, MAPO mixing temperature and time changes did not show different PP/WF composites at two different number of cycles were
a higher value of tensile strength of the composites compared with also calculated based on the equation (1) and the values are re-
the composite without MAPO. ported in Table 2. Fig. 2a shows SeN curves of neat PP and PP/WF
composites with and without MAPO. As shown in Fig. 2, composites
3.2. Fatigue behavior and fatigue reliability of the composites exhibited higher fatigue life compared with the neat PP. In Fig. 2a, it
can also be noticed that composites without MAPO i.e. composite A
Generally, composite materials display higher fatigue perfor- exhibited higher fatigue life compared with MAPO containing
mance than that of its matrix material. Rigid filler particles have composites B. In fibre reinforced composite, debonding of fibre/
ability to reduce the degree of matrix deformation in front of the matrix, fibre breakage, delamination and matrix cracking are the
crack tip that propagates in soft matrices [32,38]. Our previous major damage mechanisms [38]. Maleic anhydride has two func-
study [39] on fatigue analysis of PP/WF composites also showed a tional groups: anhydride group and double bond. A molecule of
good agreement with the literature results. In this study, we maleic anhydride has a possibility to be bonded with PP radical
generated by peroxide through double bond as well as to be bonded
withWF surfaces through the anhydride group. Consequently, the
resultant composite system would exhibit an improved fatigue

Table 2
Tensile strength and fatigue strength of CNF impregnated PP/WF composites.

Wood Toughness Tensile Fatigue strength (MPa)


flour (MJ/M3)b strength (MPa) at different number of cycle (N)a

103 (N) 106 (N)

PP 8.7 33.0 ± 0.4 25.5 17.9


A 4.6 46.9 ± 1.0 40.9 29.2
B 4.4 45.5 ± 0.4 40.3 27.1
C 3.9 45.3 ± 0.9 41.0 26.9
D 3.8 44.2 ± 0.2 39.0 24.9
E 3.9 44.5 ± 0.5 39.1 26.0
F 4.4 46.1 ± 0.5 40.6 27.1
G 4.4 45.1 ± 0.7 38.1 25.6
a
Calculated fatigue strengths based on equation (1).
b
Fig. 1. Tensile strength of neat PP and PP/WF composites. Toughness from the area of stress-strain curves.
M.M.-U. Haque et al. / Advanced Industrial and Engineering Polymer Research 2 (2019) 136e142 139

Fig. 2. SeN curves of neat PP and composites: (a) effect of MAPO, (b) effect of MAPO mixing temperature (c) effect of MAPO mixing time at 140  C, (d) effect of MAPO mixing
time at 180  C.

performance due to the components compatibilization. However, not show a higher fatigue life of the MAPO mixed composites
the fatigue performance of the MAPO composites were lower compared with the non-mixed composite A. Fig. 3 represents the
compared with the composites without MAPO. Since the main 95% confidence band of fatigue experimental data of neat PP,
components (PP, CNF and WF) and processing conditions were the composite A, and composite B as examples. Since fatigue experi-
same both in MAPO mixed as well as in non-mixed composites and mental data were widely scattered, therefore, based on the fatigue
maleic anhydride might also be grafted onto PP [34] that should testing data, 95% confidence band of neat PP and composites were
have a positive effect on the fatigue life of composites, but, the created using a SigmaPlot software. 95% confidence upper band
fatigue performance of composites was not improved. Thus, this indicated 5% survivability and 95% failure of the sample specimens,
behaviour indicated that MAPO had played a serious role on the whereas 95% confidence lower band indicated 95% survivability
deterioration of fatigue performance of the composites. It had been and 5% failure of the sample specimens. From the 95% confidence
reported that fatigue life increased with increasing molecular band the fatigue strengths at different frequency were also calcu-
weight of polymer [42]. Since melt-processing of PP with MAPO lated and the values are reported in Table 3.
causes chain scission of polypropylene [43,44], hence this lower Plot of 95% confidence lower band of neat PP and PP/WF com-
fatigue life of MAPO containing composites compared with the posites were created as shown in Fig. 4. Since 95% confidence lower
composite A can be attributed to degradation of PP chain that band ensure 95% survivability and only 5% failure of samples [45].
increased the rate of matrix cracking. Hence, from this study it can be suggested that the calculated data
MAPO mixing temperature and mixing time on the fatigue life of reported in Table 3 or the calculated fatigue life from 95% confi-
composites were also investigated. Fig. 2b displays the SeN curves dence lower band in Fig. 4 can be used as material reliability index
of composites B, C, E and F with MAPO mixing temperature 140, with 95% of certainty for safe fatigue design.
120, 160 and 180  C, respectively. Composite E with MAPO mixing
temperature 160  C exhibited the lowest fatigue performance as 3.3. Melt-viscosity of the composites
did tensile strength. Fig. 2c and d represent the effect of MAPO
mixing time on the fatigue life of MAPO mixed composites at two To investigate the effect of MAPO on the fatigue performances of
different temperature 140  C and 180  C, respectively. In Fig. 2c, it PP/WF composites the melt-viscosity of the composites were
can be noticed that composite B with MAPO mixing time 10 min measured. Fig. 5 represents the melt-viscosity of PP/WF composites
displayed higher fatigue life compared with the composite D with as a function of shear rates of 100e500 1/s. The melt-viscosity
MAPO mixing time 20 min. Whereas, at 180  C temperature com- experimental data of the composites were fitted to the classical
posite F with MAPO mixing time 10 min displayed higher fatigue power law expression [46].
life compared with the composite G with MAPO mixing time 5 min.
Although MAPO mixing temperature and mixing time had influ- h ¼ ARh uðnRh Þ (3)
enced on the fatigue performances of the MAPO mixed composites
that indicated some interaction among maleic anhydride, PP and where h represents the melt-viscosity of the composites and u
WF. However, variation of MAPO mixing temperature or time did represents the shear rate. In equation (3) ARh is a pre-exponential
140 M.M.-U. Haque et al. / Advanced Industrial and Engineering Polymer Research 2 (2019) 136e142

Fig. 3. SeN curves with 95% confidence band of fatigue experimental data of neat PP, composite A, and composite B.

Table 3
Fatigue strength of the composites calculated from 95% confidence band (lower line - upper line values).

Sample Fatigue strength (MPa) at different frequency (N)

103 104 105 106 107 108 109

PP 25.4e27.3 22.9e24.7 20.5e22.2 18.0e19.7 15.5e17.1 13.0e14.6 10.5e12.0


A 39.7e42.0 35.9e38.1 32.0e34.3 28.1e30.4 24.2e26.5 20.3e22.6 16.4e18.7
B 39.5e41.0 35.2e36.6 30.8e32.2 26.4e27.8 22.0e23.4 17.6e18.9 13.3e14.5
C 39.9e42.1 35.2e37.4 30.5e32.7 25.8e27.9 21.0e23.2 16.3e18.5 11.6e13.8
D 38.1e40.0 33.4e35.2 28.9e30.4 24.2e25.6 19.6e20.8 15.0e16.1 10.4e11.3
E 37.6e40.6 33.4e36.0 29.1e31.5 24.9e27.0 20.7e22.5 16.4e18.0 12.2e13.5
F 39.2e42.0 34.8e37.4 30.5e32.7 26.1e28.1 21.7e23.4 17.4e18.8 13.0e14.1
G 37.4e38.7 33.3e34.5 29.1e30.4 25.0e26.2 20.8e22.0 16.7e17.9 12.5e13.7

factor or consistency index and nRh is a shear thinning exponent or


flow behavior index whose values were found to be 0.5e0.6. For
each and every composite material, the values of correlation coef-
ficient and R2 were found to be about 0.93 and >0.99, respectively
(see Table 4). The value of correlation coefficient, 0.93 indicated a
very strong downhill (negative) linear relationship between shear
rate and melt-viscosity. In Fig. 5, it is obvious that the melt-viscosity
of composites decreased with increasing shear rates indicating a
pseudoplastic or shear-thinning characteristic of the composite
materials. The pseudo-plastics or shear-thinning behavior of PP/WF
composites had also been reported by Li et al. [47]. In Fig. 5a, it can
also be noticed that the melt-viscosity of MAPO mixed composite B
was lower compared the composite without MAPO, A.
Although, a higher melt-viscosity of composite B was expected
considering a higher interfacial interaction between PP matrix
phase and WF particles in presence of MAPO. The lower values of
melt-viscosity of MAPO containing composite B compared with the
composite A indicated the molecular degradation of PP polymer in
MAPO mixed composites. Melt-viscosity of PP polymer is depended
on the molecular weight of PP polymer [48] as well as in the
presence of peroxide molecular degradation of PP by chain scission
has already been investigated by Azizi et al. [44]. Fig. 4. 95% confidence lower band of neat PP and PP/WF composites.
M.M.-U. Haque et al. / Advanced Industrial and Engineering Polymer Research 2 (2019) 136e142 141

composites compared with the composites without MAPO. This


behaviour suggested that the effect of molecular degradation of PP
(as indicated by rheological measurement) on the fatigue perfor-
mance of the composites was more prominent compared with the
compatibilizing effect of MAPO.
Since fatigue experimental data were widely scattered, hence in
this study a fatigue reliability was sought. Based on the fatigue
experimental data 95% confidence band of neat PP and PP/WF
composites were created. Since 95% confidence lower band ensure
95% survivability and only 5% failure of the composites, hence, from
this study, it is suggested that the calculated fatigue life from 95%
confidence lower band can be used as a material reliability index
for safe fatigue design of PP/WF composites.

Conflicts of interest

The authors declare no conflict of interest.

Fig. 5. Melt-viscosity of the composites against shear rates: (a) effect of MAPO, (b)
effect of MAPO mixing temperature, (c) effect of MAPO mixing time.
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