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Thermal and mechanical properties of


biocomposites based on a cashew nut shell
liquid matrix reinforced with bamboo fibers

Article in Journal of Composite Materials · January 2014


DOI: 10.1177/0021998314545182

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JOURNAL OF
COMPOSITE
Article M AT E R I A L S
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Thermal and mechanical properties Reprints and permissions:
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of biocomposites based on a cashew DOI: 10.1177/0021998314545182
jcm.sagepub.com
nut shell liquid matrix reinforced with
bamboo fibers

AE Costa Júnior1, ACH Barreto1, DS Rosa2, FJN Maia1,


D Lomonaco1 and SE Mazzetto1

Abstract
Cardanol–formaldehyde thermoset resin was reinforced with raw and chemically modified fibers of bamboo
(Bambusoideae). Modified fibers were treated with alkali solutions of NaOH (5% and 10%) and bleached with sodium
hypochlorite NaClO/H2O (1:1) at 60 C–75 C. The biocomposites were fabricated with a hand lay-up technique. This
study investigated the fibers microstructure before and after alkali treatment, as the interaction between matrix and
reinforce by scanning electron microscopy. The Fourier transform infrared spectra allowed the identification of char-
acteristic stretching frequencies attributed to the methyl groups of lignin. A considerable increase in thermal stability was
observed in the materials studied, which was verified by thermogravimetric analysis and confirmed by X-ray diffraction.
The tensile tests showed that the mechanical properties (tensile modulus, tensile strength, and elongation at break) of
bamboo fibers improved after alkali treatment, as well as the increase in the biodegradation in simulated soil, showing
that the alkaline treatment acted removing the macro components of the fibers (lignin and hemicellose), making them
more susceptible to the action of microorganisms.

Keywords
Bamboo fibers and biocomposites, cashew nut shell liquid resin, biodegradability, thermomechanical properties

polymer matrix biocomposites are sisal,6 coir,7 jute,1


Introduction
and banana.8
The use of polymer matrix biocomposites reinforced by Lignocellulosic fibers are constructed of microfibrils
natural lignocellulosic fibers has had a growing devel- composed of a cellulose crystalline fraction and an
opment in recent years.1,2 The great interest of these amorphous matrix around the hemicellulose, lignin,
materials is directly related to their physical, chemical, pectin, wax, and water-soluble compounds. These
and mechanical properties such as low density, flexibil- microfibrils are oriented at different angles forming
ity, biodegradability, non-abrasivity, porosity, and the various layers that make up the microfiber.
viscoelasticity, besides the fact that they are a renew-
able natural resource of low cost and result in less wear 1
Laboratório de Produtos e Tecnologia em Processos (LPT),
on equipment during their processing when compared
Departamento de Quı́mica Orgânica e Inorgânica, Universidade Federal
with synthetic fibers.3,4 do Ceará, Brazil
Due to these excellent properties, natural fibers have 2
Universidade Federal do ABC, Centro de Engenharia, Modelagem e
been used in the textile, paper, biocomposites, and Ciências Sociais Aplicadas (CECS), Brazil
technological applications.5 Because the lignocellulosic
fibers have accessible hydroxy groups, it can react with Corresponding author:
AE Costa Júnior, Laboratório de Produtos e Tecnologia em Processos
other polar functional groups, such as those present in (LPT), Departamento de Quı́mica Orgânica e Inorgânica, Universidade
phenolic resins. Among the most important vegetable Federal do Ceará, C. P. 6021 60455-900 Fortaleza, CE, Brazil.
fiber studied and used worldwide as reinforcement in Email: eufraziojr@yahoo.com.br

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Bamboo is an abundant natural resource in many information on these composites to produce materials
regions such as Asia, India, and South America9–11 less harmful to the environment.
and has been used traditionally for construction of Cardanol, the major component of technical cashew
houses, bridges, and home utensils.12 However, in nut shell liquid (CNSL), which is obtained as
recent years, bamboo has been prominent on the inter- by-product in the industrial processing of cashew
national scene as a sustainable material, being used in (Anacardium occidentale L.), is a phenolic compound
engineering, structural supports, biocomposite design, with a long unsaturated chain substituted in the meta
being incorporated in all production chain.13 position to the hydroxyl.15 This hydrocarbon chain acts
The bamboo fibers are long with high resistance and as an internal plasticizer giving flexibility to phenolic
considered ideal for the manufacture of paper duplex resin. The polymeric matrix is result of the polyconden-
board. They are also suitable for food packaging, sation reaction between cardanol (natural phenol) and
pharmaceuticals, and reinforcements for the ideal bio- formaldehyde.
composite.14 Their high mechanical strength is guaran-
teed by fibers that represent about 60%–70% of the total
mass of stem. Bamboo is considered as a natural Experimental procedure
resource that takes less time to be renewed, and there
is no species that can compete in speed of growth and
Materials
utilization by area. It is an excellent scavenger of carbon Bamboo fibers of the family Bamboo vulgaris (100 mm
that can be used in reforestation, riparian vegetation, length, diameter 0.04 mm, and density 0.763 g/cm3)
such as protective and regenerating environment, were collected at the University Federal of Ceará
besides being used as raw material in many applications. (Brazil, 3 440 4600 latitude S and 38 340 3300 longitude
Bamboo fibers were selected in the present study as W) in September 2011. The CNSL used in this work
reinforcement materials in resol resin matrix for the was kindly provided by Amêndoas do Brasil Ltda
following reasons. First, bamboo has the fastest located in Fortaleza-Ceará-Brazil. Sodium hydroxide
growth rate among the various types of renewable nat- (99%), sodium hypochlorite (97%), formaldehyde
ural fibers. Furthermore, the cellulose fibers in bamboo (37%), ammonium hydroxide (30%),
are aligned along the length of the bamboo providing 2 -(Dimethylamino) ethyl benzoate (99%), and sodium
maximum tensile strength, flexural strength, and rigid- sulphate (99%) were obtained from Sigma-Aldrich and
ity in that direction. Another factor considered decisive used without prior treatment. Resin epoxy was
in the choice of bamboo as reinforcement material is obtained from Epoxiglass in Brazil.
the high content of cellulose (60%), responsible for the
rigidity and resistance, see Table 1.
Chemical modifications on the surfaces of natural
Chemical treatment of bamboo fibers
fibers have been widely used to improve the interaction Dried bamboo strips were dipped in NaOH solutions
between fiber and matrix. Alkali treatment is currently 5% and 10% at temperature intervals of 60 C–75 C for
used in the stage of surface modified fibers. The process 4 h, for partial removal of lignin, hemicellulose, and
consists of immersing the material in an alkaline solu- other residues (Figure 2). After this period, the fibers
tion at different concentrations. were washed with distilled water several times to
In this work, we report the use of bamboo fibers as remove sodium hydroxide excess from the surface
reinforcement and cardanol as polymeric matrix in the until the water no longer indicated any alkalinity reac-
preparation of biocomposites (Figure 1). They were tion. Subsequently, the fibers were dried in oven at
evaluated in terms of their thermal and mechanical 60 C for 24 h.
properties, as were also submitted to biodegradability Bamboo fibers obtained after alkaline treatment
tests in simulated soil, in order to gather more were dipped in NaClO 1% solution under heating

Table 1. Composition of some natural fibers.

Fiber Density (103 kg m3) Microfibril angle ( ) Cellulose (%) Hemicellose (%) Lignin (%)

Bamboo 800 2–10 60 5 32


Banana 1350 11 65 19 5
Coir 1150 30–49 43 0.25 45
Jute 1450 8.1 63 20 12
Sisal 1450 20–25 70 14 12

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Júnior et al. 3

Figure 1. Step of the preparation of biocomposites.


CNSL: cashew nut shell liquid.

Figure 2. (a) raw bamboo fiber, (b) bamboo fiber treated with NaOH 5%, and (c) bamboo fiber treated with NaOH 10%.

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(60 C–75 C) for 1 h. At this point, the fibers presented


Study of biodegradability
strong bleaching effect, being subsequently washed with The biodegradability measurements of the fibers and
distilled water to eliminate remaining chemicals and biocomposite were obtained by the mass retention tech-
dried in oven at 60 C for 24 h. The active bleaching nique. The fibers and the biocomposites were weighed
agent is the hypochlorite ion and the reactions are as and buried in simulated soil at room temperature
follows:6 (24 C). The simulated soil consisted of 23% of loamy
silt, 23% of organic matter (cow manure), 23% of sand,
NaOCl þ H2 O ! NaOH þ HOCl ð1Þ and 31% of distilled water (all wt/wt). Biodegradation
was monitored for 210 days by measuring the mass
HOCl ! Hþ þ  OCl ð2Þ retention. The buried specimens were recovered,
washed with distilled water, and dried at a room tem-
HOCl þ Hþ þ Cl ! Cl2 þ H2 O ð3Þ perature until there was no further variation in weight,
after which they were then weighed. The experiments
were done in triplicate.
Obtainment cardanol and synthesis of polymer resol
Cardanol used in the preparation of the resin was Structural characterization of the jute
obtained from technical CNSL using the following fibers and biocomposites
methodology: Technical CNSL (100 mL) was dis-
Infrared measurements
solved in methanol (320 mL), and ammonium hydrox-
ide (170 mL) was added and stirred for 30 min. Then, The infrared measurements were performed using a
the solution was extracted with hexane (1  250 mL). Spectrum 200 FTIR Spectrometer, Perkin Elmer, in
The organic phase was washed with 2.5% NaOH order to determine changes in functional groups chem-
(2  100 mL). To this solution was added HCl istry have been caused by the treatments. Prior to the
(37%, 10 mL) until pH 5. The cardanol analysis, 10 mg fibers were ground and mixed with KBr.
obtained was conditioned at a temperature of The resultant powder was pressed into transparent pel-
approximately 15 C. lets and analyzed in transmittance mode within the
The polymer resol was obtained by adding cardanol range of 4000–400 cm1.
to a solution of formaldehyde (37%) and ammonium
hydroxide (30%), in proportions of 1:2:1, under strong
magnetic stirring. The mixture remained in refluxing at
Crystallinity index
80 C for 3 h in order to complete the polycondensation. X-ray diffraction (XRD) patterns were obtained from
bamboo disks at room temperature (300 K) using a
Rigaku powder diffractometer model DMAXB. The
Preparation of biocomposite samples were pulverized and their particles were com-
The processes of biocomposites manufacturing were pacted in a cylindrical mold into disc format (Ø 1.7 cm)
reported elsewhere.1,6 The technique used in the prep- and submitted to the pressure of 111 MPa. Co-Ka tube
aration of the biocomposites was a simple hand lay-up. was operated at 40 kV and 25 mA, and the measure-
An aluminum mold (160  80  5 mm) was used. A ments were performed using the Bragg–Bretano geom-
release agent (silicone) was used to facilitate easy etry in continuous mode with a scan speed of 0.5 /min
removal of the biocomposite from the mold after and step size of 0.02 (2) in the angular range of 5 –40
curing. The resol resin was mixed with epoxy resin (2). The crystalline index of cellulose, CIr, was deter-
and catalyst 2 -(Dimethylamino)ethyl benzoate mined based on the Segal empirical method16
(Aldrich, 99%) in the proportion 0.93:1:0.03,
respectively. CIr ¼ ðI200  Iam Þ=I200 100 ð4Þ
Epoxy resin acts as a modifier agent in the poly-
mer, giving it greater flexibility and adhesion. The where I200 is the peak intensity corresponding to cellu-
epoxy resin hardened with the aid of a catalyst lose I, and Iam is the peak intensity of the amorphous
improving the thermosetting properties of material. fraction.
Bamboo fibers were cut into uniform length (35
mesh) and added to the polymer matrix, under stir-
Mechanical analysis of bamboo
ring. This mixture was transferred to an aluminum
mold previously waxed with a desmoldant agent. A Elasticity module (GPa), tensile strength (MPa), and
complete cure of the material was done in oven at rupture elongation (%) were the mechanical properties
120 C for 3 h. measured in the tensile strength. The tensile tests were

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Júnior et al. 5

carried out for five samples to each kind of fiber presents no cavities and it is covered by a layer of resi-
(untreated and chemically treated) and biocomposites, dues responsible for fibrils compression. These residues
using the INSTRON machine model 4433. The fibers protect fibers and prevent the penetration of the resin
were defibrillated and their wires were submitted to into it. This material that covers fibrils is named cuticle
mechanical measurements. The conditions for analysis and it was identified as an aliphatic wax,19 which is
were a speed of displacement of 2.0 mm/min, load of incompatible with most polymers and prevents a
100 N, and length of the fiber of 5.0 cm. It was preceded greater adhesion between reinforcement/matrix.
by an adaptation of the norm ASTM D3039, and the Figure 3(d) shows the biocomposites with natural
fibers were located in a rectangular window, with fibers of bamboo, which presented a low interaction
2.0 cm of width and 4.0 cm of length. The norm with the matrix, evidenced by limited microfibrillar
ASTM D3039 and ASTM 638 describes the test. exposure.
Figure 3(b) shows the fibers after chemical treatment
of NaOH 5%, indicating a slight difference due to the
Mechanical analysis of biocomposites
partial removal of non-cellulosic component as waxes,
Five samples of biocomposites (160  10  3 mm) were pectin, hemicellulose, lignin, etc., providing more
tested with an INSTRON, model 4433 tensile tester exposed fibrils, increasing the surface area provided
according to ASTM D638 and D3039 with a crosshead and thereafter the interaction and adhesion between
speed of 2 mm/min and a span length of 4 cm. fiber and resin. Figure 3(c) shows a slight modification
of the fiber surface after treatment with NaOH 10%. At
this concentration of alkali, a greater degree of leaching
Scanning electronic microscopy
of the surface layer of the fibers was observed, making
The morphological characterization of the bamboo them more resilient to produce a greater adherence to
fibers and the biocomposites was done by scanning the polymer matrix. The loss of the surface layer occurs
electron microscopy (SEM). This technique was used by breaking the links that bind the polymer chains pre-
to observe the surface morphology and make analysis sent in lignin and hemicelluloses due to sensitivity to
of the microstructure in both natural and chemically alkali treatment, leaving the fiber surface more
treated forms. The micrographs were obtained by an exposed.20,21 Based on these results, it is expected that
electronic microscope DSM 960 Zeiss, with 20 kV elec- the fibers subjected to a treatment with NaOH 10%
tron beam. The samples were coated with Au and would have a greater interaction with the polymer
‘‘sputter counted’’ with argon plasma model matrix.
BALZERS 5CD50. Studies by Barreto et al.1 showed a greater inter-
action between the reinforcement and matrix after
chemical treatment with 10% NaOH. Similar behavior
Results and discussion was observed in coconut fibers when used as reinforce-
The physical and mechanical properties of biocompo- ment of biocomposites derived from natural rubber.20
sites reinforced with natural fibers depend on the inter- The same behavior was observed for Rosa et al.7 who
action of components present in the region of the investigated the interaction between starch/ethylene
interface reinforcement/matrix. The magnitude of this vinyl alcohol copolymers/coir biocomposites. As a con-
interaction can be improved by surface modification, sequence, greater reinforcement/matrix interaction was
whose purpose is to increase the hydrophilicity, disper- observed due to improvement of the surface adhesion.
sion, mobility, and adherence of the fibers. Figure 3(e) and (f) illustrate this behavior for the bio-
The chemical treatment with NaOH was chosen composites reinforced with bamboo fibers undergoing
based on satisfactory results obtained for other fibers, treatment with NaOH 5% and 10%, respectively.
where the physical and mechanical properties of fibers The XRD patterns of the bamboo fibers untreated
were optimized to be used as reinforcement in biocom- and treated with NaOH are shown in Figure 4. The
posites.1,17 Bamboo fiber as reinforcement in biocom- major peaks observed for all fiber samples are at 2
posites has improved mechanical properties after diffraction angles of 18.2 and 26.0 . They are repre-
different treatments.18 The removal of non-cellulosic sented by 101 and 002 planes, attributed to the crystal-
components of the surface layer increases adhesion line phase of cellulose type I (ICDD PDF50–2241).22
between fibers and resin, providing greater stabilization Table 2 shows the crystallinity index calculated accord-
of the fiber–matrix bond. ing to the Segal et al.16 empirical method.
Figure 3 shows the SEM images obtained for ana- The crystallinity index increased for all treated sam-
lyses of the surface of bamboo fibers treated, non- ples, especially for the ones treated with NaOH 10%
treated, and their biocomposites. Figure 3(a) illustrates (48.28%). This increase could be related to the partial
the morphology of the untreated fiber surface, which removal of non-cellulosic compounds: lignin,

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Figure 3. The scanning electron microscopy for bamboo fibers: (a) raw, (b) treated with NaOH 5%, and (c) treated with NaOH 10%
and their biocomposites (d), (e), and (f), respectively.

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Júnior et al. 7

hemicellulose, and waxes. The surface modification of ester in pectin and wax.25 The disappearance of the
the bamboo fiber after alkaline treatment was also peak around 1253 cm1, which represents the C–O
observed by SEM, as shown in Figure 3. stretching in lignin, probably indicates its degradation
Figure 5 shows Fourier transform infrared spectra after alkaline treatment.26
(FTIR) spectra for untreated and treated bamboo strip. The spectral region between 1050 cm1 and
Bands frequencies and their corresponding functional 1500 cm1 (between the dashed lines) represented in
assignments are consistent with the literature values for Figure 5(a) is relative to lignin. In this spectral range
lignocellulosic fibers.23,24 The spectrum shows the main was observed a slight change in raw bamboo, when
absorption modes between 400 and 2000 cm1. A band compared with chemically modified fibers (Figure 5(b)
between 1660 cm1 to 1740 cm1, characteristic of the and (c)). This variation in the spectra suggests that,
stretching frequency of C ¼ O groups, was observed, despite the alkali treatment does not completely
which can be attributed to the presence of carboxylic remove lignin, it still caused changes in the groups on
fibers surface. These results agreed with those observed
in the analysis by XRD analysis, where the amorphous
area (Iam) corresponds mainly to the presence of this
component in the fibers. The peak around 1735 cm1,
which represents the C ¼ C axial stretching belonging
to hemicellulose, pectin and waxes, disappeared after
treatment with NaOH 5% and 10%, suggesting that
these components were partially removed.6,27

Figure 5. Infrared spectroscopy of bamboo fiber: (a) raw,


Figure 4. XRD of the bamboo fibers: (a) raw, (b) treatment (b) treatment with NaOH 5%, and (c) treatment with NaOH
with NaOH 5%, and (c) treatment with NaOH 10%. 10%.

Table 2. Mechanical properties and crystallinity index of treated and untreated bamboo fibers.

Maximum Breaking Breaking Elongation Elasticity Crystallinity


Fiber tensile (MPa) tensile (MPa) load (N) (%) modulus (GPa) index (%)

Raw 84 84 164 2.05 4.1 22.97


NaOH 5% 174 174 250 4.82 4.6 45.53
NaOH 10% 212 212 358 3.98 5.3 48.28

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Table 2 shows the results of mechanical properties of observed.31 XRD results corroborated the behavior
the bamboo fibers before and after chemical treatment. demonstrated in this test, which revealed an increase
All fibers subjected to tensile tests showed higher resist- in the crystallinity of the fiber after chemical treatment,
ance and percentage of elongation than other lignocel- providing higher resistance of the material due to the
lulosic fibers such as jute, sisal, and banana, whose high content percentage of cellulose. Therefore, mech-
average stretch is 1.5%, 0.7%, and 0.6%, respectively.28 anical properties of fibers depend on the chemical com-
According to data showed in Table 2, there was an position and their internal structure.
increase in the mechanical properties of fibers after the The thermogravimetric analyses (TG) and its deriva-
chemical treatment. An increase in the failure stress of tives (DTG) curves under nitrogen atmospheres for
107% and 152% for the fibers treated with NaOH 5% bamboo fibers untreated and treated with NaOH solu-
and 10%, respectively, was observed when compared to tions are shown in Figure 7. In both samples, a progres-
raw fibers. The results are associated to cellulose con- sive loss of mass at a temperature below 100 C was
tent of bamboo fiber (60%) and confirmed by the XRD observed, which was associated with the release of
data, which shows an increase of crystallinity index water.32 The decomposition of lignocellulosic compounds
after alkali treatment.29 (hemicellulose, cellulose, and lignin) for all bamboo fibers
The mechanical properties of biocomposites were showed only one distinct peak to raw fibers and two peaks
evaluated for the influence of the chemical treatment to treated fibers with 5% to 10% in the DTG curves.
employed in the reinforcement. Similarly, the biocom- At temperatures between 100 C and 400 C, mass
posites that showed the best performances were those losses of 64.90, 67.38, and 67.95% in samples of raw
reinforced with fibers treated with NaOH 10%, see bamboo, treated with NaOH 5%, and 10%, respect-
Figure 6. According to Gomes et al.,30 upon alkaline ively, were observed. These corresponded to the thermal
treatment, there was a partial removal of the fiber com- decomposition stage of the fiber macrocomponents.
ponents due the rupture of ester linkages between poly- Lignocellulosic fibers degrade in several steps.33 The
uronic acid and lignin, increasing the index crystallinity hemicellulose part degrades at about 240 C–310 C,
after alkali treatment. Accordingly, the fiber becomes whereas the cellulose part degrades in the range of
less dense and more rigid, increasing the fibrils strength 310 C–360 C and the lignin has been shown to degrade
as observed for fibers with lower lignin content and in wide temperature interval (200 C–550 C).6
hemicelluloses contents. In Figure 7, it is also noted that the chemical treat-
The results obtained from these tests are consistent ment improved thermal stability of the fiber, character-
with the literature.30 After chemical treatment, a signifi- ized by an increase in initial temperatures of
cant increase in the mechanical properties of fibers was degradation. An increase in the initial degradation

Figure 6. Tensile strength of biocomposites reinforced with bamboo fiber untreated and treated with NaOH solutions.

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Júnior et al. 9

Figure 7. TG/DTG of raw and treated bamboo fibers in inert atmosphere.

Table 3. Parameters obtained from TG/DTG curves of white and colored cotton fibers at N2 atmospheres:
temperature range of thermal degradation, mass losses, and mass residue at 800 C.

Atmosphere Temperature Temperature Mass Residue


Fiber (10 C min1) maximum ( C) range ( C) loss/(%) (%)

Raw N2 315 275–400 55 22


NaOH 5% N2 330 283–400 67 15
NaOH 10% N2 340 291–400 68 13

temperature (284.0 and 291.0 C) in samples treated Initial temperature of degradation, the maximum
with NaOH 5% and 10% respectively, compared with temperatures of the thermal decomposition, mass loss
the fibers in their natural state (275.5 C), can be seen. involved, and the residual mass at 800 C were deter-
Similar results were found by Maheswari et al.,34 who mined from TG/DTG (Figure 7) and are shown in
investigated the thermal behavior of the tamarind Table 3. The bamboo fiber treated with NaOH 10%
fruit fibers. began to decompose at higher temperature than the

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other fibers samples analyzed. Despite the increase in the biocomposites, under inert atmosphere (N2), are
alkali concentration, it caused a small increase in the shown in Figure 8. Weight loss associated with the
initial temperature of pyrolysis (from 283 C to 299 C) moisture present in the fibers, which is justifiable con-
under these conditions, in addition to a greater mass sidering the temperature used in the curing process, was
loss, indicating that chemical treatment was more not observed in all samples. The thermogravimetric
appropriate with NaOH 10%. This result can be justi- curves of the biocomposites showed two main degrad-
fied if we associate the degradation to the amorphous ation stages. The first event occurred in the temperature
regions of the fibers as a function of crystallinity. range between 250 C and 380 C, and this process cor-
Bamboo fibers treated with NaOH 10% showed a responds to the simultaneous degradation of pectin,
higher crystallinity index, resulting in a greater hemicellulose, and cellulose.
amount of waste degradation process, thus justifying A second stage occurred at intervals between 400 C
a higher mass loss.35 and 450 C, characteristic of the degradation of cross-
The thermal analysis is an important technique for linking between the polymer chains. At temperatures
the characterization of polymers, since the good ther- above 450 C occurred the decomposition of the final
mal stability observed in these materials allows several products of the fibers and the polymeric matrix.
technological applications. The TG and DTG curves of During these stages, a slight increase in the maximum

Figure 8. TG/DTG of biocomposites reinforced with raw and treated bamboo fiber in inert atmosphere.

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Júnior et al. 11

degradation temperature (DTG curve) from 400 C to where the bamboo fiber treated with NaOH 10% solu-
421 C for the biocomposite reinforced with raw and tion was more affected than others.37 This happened
chemically modified (10% NaOH) fibers, respectively, due to an increase in surface area, as observed by
was also observed. These results demonstrate that the SEM, caused by the partial removal of the fiber con-
thermal properties of the bamboo biocomposites stituents such as hemicellulose, pectin, fat, and lignin.
improved considerably after the chemical treatment of Similar behavior was also observed for the biocom-
the fibers. posite supported with bamboo fiber (treated and
Figure 9 shows the loss of weight of the biocom- untreated). In 30 days, there was an increase in the
posites and fibers (non-treated and treated with alka- mass of the biocomposites of 6.09%, 5.10%, and
line solution) exposed to microorganisms in simulated 3.04% for the samples reinforced as raw fiber and
soil during 210 days. The results showed that the treated with NaOH solution of 5% and 10%, respect-
biodegradability of the lignocellulosic fiber is depend- ively. The biocomposite samples reinforced with raw
ent on the applied treatment. It was observed that bamboo fiber and treated showed different degree of
raw bamboo fiber and treated with NaOH 5% pre- biodegradation with weight loss after 30 days of
sented an increase of mass at the initial stages of the analyses.
experiment (3.03% and 1.05% for raw and treated In general, the biodegradability studies showed that
fibers, respectively), which could be attributed to the raw bamboo fiber and the biocomposite reinforced
the absorption of water.32,36 This behavior was not with this fiber was more resistant to the action of the
observed for the sample treated with NaOH 10% due microorganisms due to the presence of more lignin and
to significant decrease of macroconstituents (lignin hemicelluloses contents. In the plant tissue, lignin acts
and hemicellulose) that present hydrophilic hydroxyl as a reinforcing reinforcement, like cement between the
groups. fibers. The association between lignin and hemicellulose
In general, the fibers treated with NaOH (5% and forms a protective barrier against microorganism’s
10%) demonstrated higher weight loss caused by the attackers.
biodegradation induced by the action of microorgan-
isms. This loss of weight was caused by enzymes pro-
duced by microbial population in the simulated soil,
Conclusions
The chemical treatment directly affected the thermal
and mechanical properties and consequently the adhe-
sion between matrix and fiber, as observed in SEM,
where the alkaline treatment caused exposure of the
cellulose structures. The XRD showed that chemical
treatment increased the crystalline fraction due to par-
tial removal of amorphous components. The FTIR was
important to observe the main groups function and its
variations as function of treatment. This modification
was important to improve the adhesion fiber matrix in
the biocomposites and resulted in materials more
homogeneous, resistant to thermal decomposition and
higher mechanical resistance.
Beyond these results, the biodegradation tests
showed that alkaline treatment rendered a composite
more susceptible the microorganism’s action, especially
the composite reinforced with fibers treated with NaOH
10%, which revealed a higher mass loss in simulated
soil. In general, we can conclude that the composites
produced in this study, obtained from a raw material
derived from biomass (CNSL) have a greater bio-
degradability compared to composites reinforced with
synthetic fibers.

Funding
Figure 9. Biodegradation of bamboo fibers after and before This work was supported by FUNCAP, CAPES, and CNPq
treatment, in simulated soil. (Brazilian agencies).

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Conflict of interest
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