a r t i c l e i n f o a b s t r a c t
Article history: Thermo-mechanical properties and erosion performance of short carbon bre reinforced vinyl ester resin
Received 10 July 2010 based isotropic polymer composites with four different bre weight fractions have been investigated. The
Accepted 10 November 2010 storage, loss and damping characteristics were analysed to assess the energy absorption/viscous recover-
Available online 3 December 2010
able energy dissipation and reinforcement efciency of the composites as a function of bre content in
the temperature range of 0140 C. The composite with 30 wt.% of short carbon bres has been observed
Keywords: to exhibit superior thermo-mechanical response with highest energy dissipation/damping ability accom-
Polymer matrix
panied with a constant storage modulus without any substantial decay till 60 C. The erosion rates (Er) of
Mechanical
Wear
these composites are evaluated at different impingement angles (3090), bre loadings (2050 wt.%),
impact velocities (4376 m/s), stand-off distances (5585 mm) and erodent sizes (250600 lm) follow-
ing the erosion test schedule in an air jet type test rig. An optimal parameter combination is determined
and subsequently validated for erosion rate minimization following Taguchi method and by conducting
conrmation experiments. A correlation between the loss-modulus inverse and the erosion rate has been
observed which conceptually establishes a possible mechanistic equivalence between erosion and
dynamic mechanical loading modes. The morphologies of eroded surface are examined by the scanning
electron microscopy to investigate the nature of wear-craters, material damage mode and other qualita-
tive attributes responsible for promoting erosion.
2010 Elsevier Ltd. All rights reserved.
0261-3069/$ - see front matter 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2010.11.019
S. Kumar et al. / Materials and Design 32 (2011) 22602268 2261
polymer composites is usually higher than that of the un-rein- Mechanical Analysis (DMA) was conducted in a nitrogen atmo-
forced polymer matrix and poorer than metallic materials [25]. sphere at a xed frequency of 1 Hz, heating rate of 5 C/min, a tem-
Solid particle erosion manifests itself in many facets such as perature range of 0150 C and a strain of 1% on rectangular
thinning of components, surface roughening, surface degradation, samples with approximate dimensions of 38 12.5 3.5 mm
macroscopic scooping appearance and reduction in functional life using a Q800 DMA instrument in bending mode [8].
of structures. Hence, solid particle erosion has been considered
as a serious problem being responsible for many failures in engi- 2.3. Test apparatus for erosion experiment
neering applications. The inuence of various experimental vari-
ables (impingement angle, impact velocity, erodent type, size, The short bre reinforced composites are molded into dimen-
shape and hardness) and target material variables/properties sion of 150 mm 150 mm 3 mm from which test samples of
(strength, ductility, crystallinity, cross link density, reinforcement approximately 30 mm 30 mm are cut using a diamond cutter
content and arrangement) on solid particle erosion of polymers for erosive performance evaluation on an erosive wear test rig.
and their composites was comprehensively reviewed recently by The erosion experiments are carried out as per ASTM G76 on the
Barkoula and Karger-Kocsis and previously by Harsha et al. [6,7]. erosive wear test rig shown schematically in Fig. 1, which is com-
However, the erosive wear behaviour of short bre reinforced posed of an air compressor, an air drying unit, a conveyor belt-type
polymer composites is an area which is ill addressed till date de- particle feeder and an air particle mixing and accelerating cham-
spite the success of their corresponding long bre composites. ber. The dried and compressed air is then mixed with the silica
Hence, the present paper comprehensively makes an attempt to sand which is fed constantly by a conveyor belt feeder into the
study the erosive performance of short carbon bre reinforced vi- mixing chamber and then accelerated by passing the mixture
nyl ester resin composites since carbon bre offers the dual advan- through a convergent brass nozzle of 3 mm internal diameter.
tage of enhanced toughness and thermal resistance compared to The set up is capable of creating reproducible erosive situations
glass and aramid bres, on one hand, and on the other, vinyl ester for assessing erosion wear resistance of the composite samples.
resin offering the best performance combination of epoxy and The erodent particles impact the specimen which can be held at
unsaturated polyester resins in terms of stiffness and chemical different angles with respect to the direction of erodent ow. The
resistance. velocity of the eroding particles is determined using standard dou-
ble disc method [9]. The apparatus is equipped with a heater which
can regulate and maintain the erodent temperature at any pre-
2. Experimental
determined xed value during an erosion trial. In the present
study, dry silica sand (assumed to be of pyramidal shaped) of dif-
2.1. Preparation of composites
ferent particle sizes (250 lm, 355 lm, 420 lm and 600 lm) are
used as erodent. Before the erosive performance tests all speci-
Short carbon bres (density: 1.81 g/cm3) (Zoltek) of 6 mm
mens were cleaned with acetone, balanced at electronic balance
length are used to prepare the composites. The curing of vinyl ester
with the accuracy of 0.1 mg. Great care is given to ensure clean sur-
resin is done by incorporation of: 2% methyl ethyl ketone peroxide
face before and after the tests. Sand and dust particles are cleaned
(MEKP) catalyst, 0.3% cobalt naphthenate (accelerator) is also
after erosion test with air blasting and then balanced carefully.
added together with 0.05% of 2,4-pentanedione (2,4-P) used as a
retarder for the extension of the reaction gel time. The resin is sup-
2.3.1. Erosion performance evaluation
plied by Ciba-Geigy having density 1.05 g/cm3 and 40 Barcol Hard-
The erosive performance were determined following the Tagu-
ness is used as the matrix material. The matrix tensile modulus and
chis technique as a multi-parametric optimization model since
strength are about 2.63.4 GPa and 65 MPa, respectively; exural
the erosive performance may be a functional variable of ve inde-
modulus and strength are about 3.6 GPa and 125 MPa respectively;
pendent parameters and their simultaneous interaction. Using this
and heat distortion temperature is 105 C. Composites having dif-
technique: (a) rstly the control factors have been identied and
ferent bre content were prepared by varying the weight fraction
(b) subsequently steady-state erosion characteristics of the com-
of bres from 20 wt.% to 50 wt.%. It is then mixed with vinyl ester
posites were determined at three selected level of optimally con-
resin and the mixture is poured into various molds conforming to
trolled operating variables.
the requirements of various testing and characterization standards.
The entrapped air bubbles (if any) are removed carefully with a
2.3.1.1. Parametric optimization by design of experiment (DOE). The
roller and the mold is closed for curing at a temperature of 30 C
evaluation of erosion performance is carried out by adopting a
for 24 h at a constant pressure of 10 kg/cm2. The details of compos-
DOE approach following the Taguchi technique to minimize overall
ite designation and composition are given in Table 1.
testing time and the experimental costs for parametric optimiza-
tion followed by the steady state erosive wear rate determination
2.2. Dynamic mechanical properties at the optimized parameter levels. The Taguchi method, straight-
forward and consistent, involves laying out the experimental con-
The thermo-mechanical properties of the composites were ditions using specially constructed tables known as orthogonal
measured using Dynamic Mechanical Analysis (DMA). Dynamic arrays. The L16 (45) inner orthogonal array permits the analysis
of ve four-level factors. The array consists of 16 rows, where each
row represents a trial condition with a particular combination of
Table 1
Details of composite designation and composition.
factor level settings. The static and the dynamic variables chosen
for the test are given in Table 2 and four levels of chosen control
Composite designation Composition (wt.% fraction) factors are given in Table 3. The controllable factors are assigned
Vinyl ester resin Carbon bre to a particular column of the orthogonal array. Accordingly, the
VCF0 100 00 present study assigns the impact velocity (factor A), bre loading
VCF20 80 20 (factor B), impingement angle (factor C), stand-off distance (factor
VCF30 70 30 D) and erodent size (factor E) to Columns 1, 2, 3, 4 and 5 of the
VCF40 60 40
adopted L16 (45) inner orthogonal array, respectively (Table 3)
VCF50 50 50
and each trial will be replicated three times with different level
2262 S. Kumar et al. / Materials and Design 32 (2011) 22602268
3.2. Erosive performance of the composites By combining like-terms, the equation reduces to
3.2.2. ANOVA and the effects of factors Among numerous factors inuencing the erosion performance
In order to nd out the statistical signicance of various factors of materials, the most important are impingement angle, impact
like impact velocity (A), bre loading (B), impingement angle (C), velocity and particle size as shown by Taguchi methods. In order
stand-off distance (D) and erodent size (E) on erosion rate, analysis to quantify the extent of the damage, the erosion rate of weight
of variance (ANOVA) is performed on experimental data. Table 5 loss is usually expressed as the weight of material removed by unit
shows the results of the ANOVA with the erosion rate. This analysis weight of impacting particles.
is undertaken for a level of condence of signicance of 95%. The
last column of the table indicates that the main effects are highly 3.3.1. Inuence of impingement angle
signicant (all have very small p-values) [13]. It is well known that impingement angle is one of the most
From Table 5, one can observe that impact velocity (p = 0.004), important parameters in erosion behaviour. Fig. 6 shows the inu-
stand-off distance (p = 0.013), erodent size (p = 0.374) and bre ence of impingement angle on the steady-state erosion rate of
loading (p = 0.400) have great inuence on wear rate but impinge- short carbon bre reinforced vinyl ester resin composites at a con-
ment angle (p = 0.889) has less signicant contribution on erosion stant impact velocity of (54 m/s), erodent size of 355 lm and
rate. stand-off distance of 65 mm. It can be seen that steady-state ero-
sion rate is maximum at 60 impingement angle for all the com-
3.2.3. Conrmation experiment posites irrespective of the bre loading. In the literature,
The optimal combination of control factors has been deter- materials are broadly classied as ductile or brittle, based on the
mined in the previous analysis. However, the nal step in any de- dependence of their erosion rate with impingement angle. The
sign of experiment approach is to predict and verify improvements ductile behaviour is characterized by maximum erosion rate at
in observed values through the use of the optimal combination le- low impingement angle, typically 15 < a < 30. On the other hand,
vel of control factors. The conrmation experiment is performed by if the maximum erosion rate occurs at normal impact (a = 90), the
taking an arbitrary set of factor combination A2B3C4D2E3 on erosion behaviour of material is brittle [14,15]. Reinforced composites have
rate as evident from Table 6. The estimated S/N ratio for wear rates been found to exhibit semi-ductile behaviour with the maximum
can be calculated with the help of following predictive equation: erosion rate at intermediate impingement angles, typically
45 < a < 60 [3,16,17]. However, the above classication is not
g 1 T A2 T B3 T C 4 T D2 T E3 T 3
absolute as the erosion behaviour of materials strongly depends
g 1 is the predicted average, T is the overall experimental average upon the experimental conditions and composition of target mate-
A2 ; B3 ; C 4 ; D2 and E3 is the mean response for factors at designated rials. Although there is a dispute about this classication-failure,
levels. Barkoula and Karger-Kocsis [5] argued that the erosive wear
Table 4
Experimental design using L16 orthogonal array.
Expt. no. A (m/s) B (%) C (degree) D (mm) E (lm) Er (104 mg/kg) S/N ratio (dB)
1 43 20 30 55 250 6.0833 64.3172
2 43 30 45 65 355 2.9167 70.7023
3 43 40 60 75 420 2.5000 72.0412
4 43 50 90 85 600 1.2500 78.0618
5 54 20 45 75 600 2.5625 71.8267
6 54 30 30 85 420 3.8750 68.2346
7 54 40 90 55 355 22.625 52.9082
8 54 50 60 65 250 20.250 53.8715
9 65 20 60 85 355 4.5263 66.8851
10 65 30 90 75 250 1.6842 75.4721
11 65 40 30 65 600 5.1053 65.8396
12 65 50 45 55 420 13.2632 57.5471
13 76 20 90 65 420 36.7143 48.7033
14 76 30 60 55 600 32.4762 49.7687
15 76 40 45 85 250 11.5238 58.7681
16 76 50 30 75 355 30.7143 50.2532
S. Kumar et al. / Materials and Design 32 (2011) 22602268 2265
Table 5
ANOVA table for erosion rate.
Table 6
Results of the conrmation experiments for erosion rate.
Fig. 8. Effect of erodent size on the erosion wear rate of the composites (at constant From SEM observations of eroded surfaces, it appears that com-
impact velocity: 54 m/s, impingement angle: 60 and stand-off distance: 65 mm). posites under consideration exhibit several stages of the erosion
Fig. 9. Correlation between erosion rate (Er) and loss modulus (E00 ) of carbon bre reinforced vinyl ester composites.
S. Kumar et al. / Materials and Design 32 (2011) 22602268 2267
and material removal process. First, there is local removal of resin the bres to the erosive environment, as seen in Fig. 10a and b.
material from the impacted surface; which results in exposure of The erosion rate data shown in Table 4 (Experiment no. 1) supports
0
30 1.5kX 300 3.0kX
(a) (b)
(c) (d)
(e) (f)
(g) (h)
Fig. 10. SEM micrograph of carbon bre reinforced vinyl ester resin composites.
2268 S. Kumar et al. / Materials and Design 32 (2011) 22602268
this observation. The micrograph further reveals that the impact of resistance of the composites besides the bre content. The opti-
solid sand particles onto the matrix renders the matrix prone to mum conditions for maximization of erosion resistance have been
breakage via the formation of cracks transverse to bre-length. found to be at an impingement angle of 60, impact velocity of
These cracks across the bre are caused by bending due to the im- 65 m/s and erodent size of 420 lm whereas from material compo-
pact of these particles on the unsupported bres. Bending is possi- sition point of view the maximum wear resistance is observed in
ble because the matrix resin surrounding and supporting the bres the composite with 30 wt.% of carbon bres. Design of experiment
have been removed. But on further increase in impact velocity (DOE) approach based on Taguchi method has been found to be
(54 m/s) under similar bre loading (20 wt.%), it can be seen from successful for parametric optimization of erosion performance
Fig. 10c and d that, when impacting at low angles, the hard erodent with respect to experimental/operational and material variables.
particles can penetrate the surfaces of the samples and cause mate- The successful predictions have also been reconrmed by conduct-
rial removal by micro-cutting and/or micro-ploughing. The matrix ing analysis of variance (ANOVA) and conrmation experiments on
is randomly grooved and cratered with local material removal un- a randomly selected set of operational variables. Wear surface
der 54 m/s impact velocity (see Table 4, Experiment no. 5). morphology has revealed that erosion process involved different
Further continuation of erosion by sand particle impacts re- mechanisms depending on the type and arrangement of bre con-
sulted in damage to the interface between the bres and the resin tent in the matrix. For short carbon bre composite, severe deteri-
matrix. This damage is characterized by the separation and detach- oration of both bre and matrix, micro-ploughing in the matrix,
ment of broken bres from the resin matrix, as shown in Fig. 10e transverse shearing and stripping have been observed whereas
and f. The observed behaviour of these materials can be attributed brillation, composite de-bonding, bre pull-out, and bre-frac-
to the following mechanism. It is well known that the bres in ture were found out to be the characteristic features of carbon bre
composites subjected to particle ow, undergo breakage when damage. A direct correlation between erosive wear rate and loss-
subjected to bending. Thus, there is a local removal of resin mate- modulus inverse (E001 ) irrespective of the bre concentration has
rial from impacted surface, which results in the exposure of the - been observed. Such a resemblance of the two different material
bres (see Table 4, Experiment no. 7). This causes intensive de- performance aspects conceptually demonstrates a mechanistic
bonding and breakage of the bres, which are not supported by interrelation between the response of the composites to erosion
the matrix. The observed erosion damage is characterized by expo- conditions and to thermo-mechanical loading situations.
sure of carbon bres, brematrix de-bonding, multiple bre
cracking and material removal. Plastic deformation, melting of ma- References
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