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Composites Part B
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a r t i c l e i n f o a b s t r a c t
Article history: Identifying novel natural fibers/fabrics with proper properties as reinforcement material is a new
Received 15 October 2014 challenge in the field of bio-composites. Hence, the aim of this paper is to study the possibility of using a
Received in revised form natural fabric extracted from Manicaria saccifera palm as a novel reinforcement in composites. This fabric
12 December 2014
was extensively characterized by chemical composition analysis, infrared spectroscopy (FTIR) analysis,
Accepted 28 December 2014
Available online 10 January 2015
morphological studies (SEM), thermo-gravimetric analysis (TGA) and physical /mechanical properties
studies. From SEM analysis it was identified globular protrusions spread uniformly over the fiber which
could help the mechanical interlock with the resin. As well, Manicaria fabric showed good thermal
Keywords:
Manicaria saccifera fabric
stability, low density, low moisture content and good tensile properties. Further, their properties are
A. Fabrics/textiles comparable to most natural cellulose fabrics and some synthetic fabrics, such as fiber glass fabrics.
B. Mechanical properties Manciaria saccifera fabric showed to be a suitable candidate as natural reinforcement material for the
B. Thermomechanical development of bio- composite.
© 2015 Elsevier Ltd. All rights reserved.
1. Introduction hemp [15,16]; sisal [17,18]; ramie [19]; kenaf [20,21]; bamboo
[22,23]; oil palm [24]; and coir fibers [25], among others. However,
Over the last years, the depletion of petroleum resources, and as the spectrum of these fibers is narrow, the identification of new
the increasing environmental regulations, have stimulated the natural fibers/fabrics has turned into an active research challenge in
research on composite materials made of renewable, recyclable, the bio-composites materials community. For example, in the last
and biodegradable resources [1,2]. For instance, cellulose-based years fibers/fabrics such as: Arundo donax L. [26]; Cissus quad-
fibers/fabrics are being used as reinforcement elements in bio- rangularis [27]; Abelmoschus esculentus [28]; Ferula communis [29];
composites, as they display several advantages in contrast to con- Cynara cardunculus L. [30]; Althaea officinalis L. [31]; Sansevieria
ventional reinforcement materials: low cost, low density, accept- ehrenbergii [32]; Prosopis juliflora [33]; and Polyalthia cerasoides
able specific strength, good thermal and acoustic insulating [34], have been suggested as interesting alternatives to reinforce
properties [3,4]. Still, their mechanical properties are intrinsically novel composites.
dependent on factors such as the origin and maturity of the plant as As the large variety of plants present in nature offers a moti-
well as the processing method implemented for its extraction [5]. vating opportunity to identify new fibers/fabrics, a research chal-
Therefore, a proper understanding of their overall mechanical lenge is to find sustainable resources for the development of bio-
behavior is one of the challenges in working with such fibers/ composites. For example, amongst the natural diversity of Latin
fabrics. America, Manicaria saccifera palm is an interesting renewable
Even though cellulose-based reinforced composites have been source for manufacturing green composites as different parts of it
widely studied during the last decades [6,7], researchers have are used by indigenous inhabitants as sources for house thatches
centered their attention to a few natural fibers/fabrics with the and sails (leaves); hats (bracts); food and drink (fruits and seed-
demonstrated potential to effectively reinforce either thermo- lings); medicines (fruits and leaves); and sago (trunk) [35e37].
plastic or thermoset polymer matrices: flax [8e11]; jute [12e14]; Among those, pouch-like bracts of closely woven texture (termed
natural fabric), which temporally cover the entire inflorescence and
the pendant infructescence (see Fig. 1), are a promising source to
* Corresponding author. create new composites [38]. Hence, this work presents a systematic
E-mail address: emaranon@uniandes.edu.co (A. Maranon). study of this natural fabric extracted from the Manicaria saccifera's
http://dx.doi.org/10.1016/j.compositesb.2014.12.033
1359-8368/© 2015 Elsevier Ltd. All rights reserved.
A. Porras et al. / Composites Part B 74 (2015) 66e73 67
Fig. 1. a) Manicaria saccifera palm [55]. b) Manicaria bract and Manicaria fabric. c) Fabric optical micrograph. d) Fabric SEM micrograph.
bracts as a possible reinforcement in composites. This study in- dry weight. A Sartorius ED2245 analytical balance and a Thermo-
cludes fabric's chemical composition analysis; Fourier Transform lyne muffle furnace type 6000 were used for the experiment.
Infrared (FTIR) spectroscopy; morphology (SEM); Thermo-
Gravimetric Analysis (TGA); and physical/mechanical properties. 2.2.2. Extractives content
To determine waxes, fats and surface resins of the fabric, the
2. Experimental methodology extractives content test was carried out following the TAPPI T204
method. Before the test, the fabric sample was oven dried at 105 C
2.1. Material and milled then into a sufficient length to pass a screen of 0.40 mm.
The extraction process was performed by boiling 5 g of the fabric
Manicaria saccifera bracts (Fig. 1(b)), of a length between 0.8 m with ethanol-benzene mixture (1:2, v/v) in a Soxhlet apparatus for
and 1.2 m, were collected manually by a native community of the 5 h. After, the solvent mixture was evaporated, and the weight of
Choco Region in Colombia. Bracts are made of brown fibrous ma- the residual part was determined. Extractives content was calcu-
terial constituted of numerous inter-crosslinked fibers as shown in lated based on the percentage of the extract dry weight to the fabric
Fig. 1(c). Due to its particular weaving design, resembling a fabric, it dry weight.
is not possible to extract a single fiber for testing as they are all
interlocked, displaying several points of bifurcation (Fig. 1(d)). 2.2.3. Lignin content
Therefore, this research is limited to the characterization of the Lignin content was determined based on the TAPPI T222 pro-
natural fabric as a whole. cedure. An extractives free sample (2.0 g, previously dried) was
treated with 72% (w/w) sulfuric acid for 2 h. During this time the
sample was macerated and stirred with a glass rod to assure
2.2. Chemical composition complete solution. After that, the material was diluted with water
to give a mixture containing 3% of sulfuric acid. Once the dilution
Chemical analysis of the Manicaria saccifera fabric was performed was completed, the system was boiled for 4 h with a constant
according to ASTM standards procedures and TAPPI methods, even volume to coagulate the lignin. Then, the coagulate material was
though TAPPI procedures were proposed for wood and pulp. Spe- allowed to settle after cooling, and the insoluble lignin was filtered
cifically, ash, extractive, lignin, and cellulose content were deter- (glass vacuum filtration assembly), washed (hot water >90 C),
mined. Samples were taken from five locations of the bract in order oven-dried (105 C), cooled, and weighed. The lignin content was
to characterize its complete behavior along the natural fabric. The calculated based on the percent of filtered solid weight to the initial
reported property was the average values of the tested samples. dry weight of test specimen.
cellulose was the remaining fraction in the solution. During the first the width, and the weights were measured to the nearest 0.1% of its
oxidation, the beta plus gamma cellulose, the dissolved fraction, mass using an analytical balance Sartorius ED2245 model. One
was measured, and alpha-cellulose was determined as an undis- hundred specimens were tested.
solved fraction by difference between the total pulp specimen
(100%) and the dissolved fraction. Then, in the second oxidation, 2.6.4. Volumetric density
the gamma-cellulose was determined. Finally, the beta-cellulose The density of the fabric was measured by displacement method
was found by the difference between the first and the second with ethyl alcohol analytical grade, as immersion liquid, using the
oxidations. ASTM D792 standard. A precision weighing balance, Sartorius
ED2245 model, was used to weight the samples. Weights of seventy
2.3. Spectral analysis five specimens were measured to the nearest 0.1 mg.
Fourier Transform Infrared spectroscopy (FTIR) was carried out 2.7. Mechanical properties
on Manicaria fabric. For this analysis, the fabric was powdered and
mixed with KBr. Then, very thin films were prepared using a Manicaria fabrics were tensile tested according to the ASTM
manual press machines, Maekawa model BRM-32. IR spectra of the D5035 method using a universal mechanical testing machine, Ins-
samples were recorded using the Nicolet 3810 FTIR spectropho- tron model 3367, equipped with a load cell of 30 kN. Standard
tometer in the frequency range 4000e500 cm1. Three replicas conditions in the testing room were 23 ± 1 C and 60 ± 5% RH.
were tested. Fabric specimens prepared by the cut strip method
(25 mm 150 mm) were characterized in longitudinal directions,
2.4. Morphology the preferential growth direction of the fibers. Tensile tests were
performed at a gauge length of 75 mm and a crosshead speed of
Surface morphology of Manicaria fabric was studied by scanning 10 mm/min to keep a constant time-to-break at 20 ± 3 s. Wood tabs
electron microscopy (SEM). Specimens were observed using Joel were used to prevent gripping damage by machine clamps. One
scanning electron microscopy (SEM), model JSM-6490LV. Prior to hundred specimens were tested to obtain average tensile proper-
the analysis, samples were coated with a thin layer of gold to ties. Taking into account that the fabric have many void regions, the
achieve good conductivity using a Dentom Vacuum Desk IV appa- cross sectional area, used to convert load into stress, of the speci-
ratus. In addition, the Energy Dispersive X-ray Spectroscopy (EDS) mens were calculated using an effective width. The concept was
technique was used to identify elements in the sample. Ten samples proposed by relating the experimental area with the density of the
were observed in both the longitudinal (inner and outer surface) fabric in order to determine the width specimen without void areas,
and the transverse section. assuming a homogeneous and continue solid (see Fig. 2(a)). The
effective width (We) was determined by equation Eq. (1), which
2.5. Thermal properties involves the mass (m), length (l), thickness (t), and density (r) of the
sample.
To analyze the thermal stability of Manicaria fabric the Ther-
mogravimetry (TG) technique was used. Tests were carried out m
We ¼ (1)
using the TA Instruments Q600 thermogravimetric analyzer and l$t$r
platinum sample pans. Measurements were conducted from
ambient temperature to 600 C at a heating rate of 10 C/min in a
2.8. Statistical analysis
nitrogen atmosphere. Samples weights were approximately be-
tween 8 mg and 10 mg. To verify the reproducibility of the obtained
Specimens for physical and mechanical measurements were
mass loss curves, two sample runs were performed under the same
taken from five locations of the bract in order to characterize the
experimental conditions. An approximate overlapping of the curves
complete behavior along the natural fabric. As it is shown in
was considered as a suitable test.
Fig. 2(b), the first (S1) and last sections (S5) were the tip and base of
the Manicaria bract, respectively. The properties found throughout
2.6. Physical properties
the study were expressed as means standard deviations. To estab-
lish if there is statistically significant difference between the mean
2.6.1. Moisture content
properties from one section to another, statistical significance was
Moisture content was measured according to ASTM D1348
analyzed using analysis of variance-one way (ANOVA). To this
standard using method B, where the specimen was weighed
purpose, a p-value of p < 0.01 was considered statistically signifi-
outside of the oven. Fabric samples were dried in an oven at 105 C
cant with a 99.0% confidence level.
until a constant weight was reached. The moisture content was
calculated from the change in weight of the oven dried sample to
the net dry sample. A total of fifty samples were tested.
Table 1
Chemical composition of Manicaria fabric at selected sections.
Component (%) S1 S2 S3 S4 S5
observed in the surface of the fabric at different levels magnifica- literature [24], the silica bodies could help the mechanical interlock
tions. Fig. 4(a) (30) shows that most of the fabric is covered by this with the resins when it is used as reinforcement in polymeric
epidermis. Fig. 4(b) (500) illustrates that the epidermis has small matrix composites. As well, when the silica bodies are dislodged a
holes on the surface that are called stomata, through which the perforated crater is left, which would enhance penetration of ma-
plant cells can breathe [8]. At higher magnifications, Fig. 4(c) trix during composite fabrication. This results in better fiber-matrix
(1000) shows that the fabric is constituted by fibers that are interfacial adhesion.
covered with lignin, impurities, waxy layer and fatty acid, too. In general, the SEM study revealed that the longitudinal surface
This substance on the fabric surface contributes to an ineffective of the fabric varies from outer to inner surface in terms of the
fiber to polymer matrix bonding and poor surface wetting. There- amount of lignin, wax, fat, resin, and impurities found. At the outer
fore, surface modification treatments are recommended to improve surface, the fibers are more condensed by this material than the
the adhesion properties with the matrix. Among chemical treat- inner surface. This is attributed to the fact that Manicaria fabric is
ments, mercerization or alkaline treatment is one of the most the material that encloses the flowers of the palm tree, and only the
common, effective, and low cost procedures applied on natural fi- outer surface of the fabric is permanently exposed to the environ-
bers. This treatment removes a certain amount of lignin, wax and ment (e.g sun, rain, dust, pollution, impurities). However, the
impurities covering the surface of the fiber. As well, it leads to in- microstructure of fiber is the same in both inner and outer surface.
creases surface roughness and the amount of cellulose exposed on The transverse section of Manicaria fiber is shown at different
the fiber resulting in better mechanical interlocking [46]. Several magnifications in Fig. 4(gei). The single fiber cross section has a
scientific works have reported that mechanical and thermal prop- polygonal shape, and the traditional morphology of a fiber consti-
erties of the composites are enhanced significantly by this treat- tuted by the epidermis, cell wall, and the lumen are present
ment. For example, Yan et al. [47] and Yan and Libo [48] reported an (Fig. 4(g)). Also, the lumen varies in size but its shape is usually
improvement of flax fabric/epoxy polymer interfacial adhesion by well-defined. The fiber is actually a bundle of hollow sub-fibers that
alkali treatment. are linked together by means of middle lamella, which consist of
Longitudinal section SEM images of the inner surface view at hemicellulose and lignin (Fig. 4(h)). As is reported in the literature
increasing magnifications are shown in Fig. 4(dee). In Fig. 4(d) [7,17], the cell walls are reinforced with spirally oriented cellulose
(30) is easier to observe that Manicaria fabric is a fibrous material, in a hemi-cellulose and lignin matrix. These helical windings of
and it is constituted by cross-linked fibers. In fact, it is noticed that cellulose microfibrils are shown at high magnification in Fig. 4(i).
one fiber can bifurcate into two new ones. As well, globular pro-
trusions are also found in great number on the fiber strand 3.4. Thermal properties
(Fig. 4(e), 1000), and the EDS analysis identified globular pro-
trusions as silica bodies, which are spread uniformly over the fiber Knowing the thermal stability of natural fibers is an important
(Fig. 4(f), 5000). In the outer surface the protrusions are covered aspect in the development of natural fiber thermoplastic compos-
by impurities and lignin. Similar protrusions were also reported for ites because the molding processing temperature is limited by this
other fibers extracted from palm tree [49]. According to the parameter. Therefore, thermal decomposition characteristics of
Fig. 4. SEM micrographs of Manicaria fabric. Longitudinal outer surface (aec). Longitudinal inner surface (def). Cross section (gei).
A. Porras et al. / Composites Part B 74 (2015) 66e73 71
Table 3
Physical and mechanical properties of Manicaria fabric at selected sections.
Property S1 S2 S3 S4 S5
Moisture content (%) 9.86 ± 1.05 9.77 ± 1.19 9.67 ± 0.91 9.55 ± 0.96 8.95 ± 1.05
Water absorption (%) 70.27 ± 3.92 71.44 ± 3.68 72.99 ± 4.77 73.08 ± 3.30 74.17 ± 2.93
Area density (g/m2) 583.30 ± 138.21 472.38 ± 89.57 401.20 ± 71.52 371.79 ± 105.20 366.31 ± 127.51
Volumetric density (g/cm3) 1.07 ± 0.05 1.04 ± 0.05 0.99 ± 0.08 0.95 ± 0.09 0.84 ± 0.12
Strength e Load per width (cN/m) 391.08 ± 133.40 381.82 ± 136.96 315.86 ± 116.99 287.77 ± 141.65 254.88 ± 139.06
Fracture stress (MPa) 70.85 ± 14.50 81.67 ± 16.27 75.58 ± 15.71 69.59 ± 15.26 54.98 ± 11.79
Young's modulus (GPa) 2.20 ± 0.53 2.42 ± 0.44 2.29 ± 0.36 2.05 ± 0.44 1.81 ± 0.36
Specific fracture stress (MPa/g$cm3) 65.97 ± 13.50 78.66 ± 15.67 76.46 ± 15.90 73.60 ± 16.14 65.75 ± 14.10
Specific modulus (GPa/g$cm3) 2.05 ± 0.49 2.33 ± 0.43 2.31 ± 0.37 2.17 ± 0.47 2.16 ± 0.43
Failure strain (%) 4.97 ± 1.39 5.39 ± 2.14 5.24 ± 0.98 5.30 ± 1.36 5.42 ± 1.70
72 A. Porras et al. / Composites Part B 74 (2015) 66e73
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