Egyptian Journal of Petroleum 27 (2018) 775–783

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Egyptian Journal of Petroleum

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Review

Effect of fiber treatment on flexural properties of natural fiber reinforced

composites: A review
Mohit Sood a,⇑, Gaurav Dwivedi b
a
Department of Mechanical Engineering, KC College of Engineering, Punjab, India
b
Department of Mechanical & Automation Engineering, Amity School of Engineering, Amity University, Noida, Uttar Pradesh, India

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

Article history: Fiber treatments and coupling agents have been applied by composites researchers to improve the func-
Received 6 June 2017 tionality in the flexural loading of natural fiber reinforced composites. This paper reviews how fiber treat-
Revised 5 November 2017 ments upshot to flexural strength and modulus of natural fiber composites during 2000–2016. Chemical
Accepted 12 November 2017
treatments improved fiber interface bonding with matrix and impart more strengths to composites.
Available online 20 November 2017
Coupling agents also ameliorate flexural properties and the combination of treatments is equally super-
cilious. The negative impact of fiber’s physical treatments on flexural properties of natural fiber compos-
Keywords:
ites also reviewed. Eventually, a number of perspectives have been concluded with the hope that our
Natural fibers
NaOH
work will succor to further betterment in flexural strength of natural fiber composites.
Matrix Ó 2017 Egyptian Petroleum Research Institute. Production and hosting by Elsevier B.V. This is an open
Coupling agent access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Composites

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 775
2. Composition of natural fibers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 776
2.1. Chemical treatments for natural fibers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 776
3. Characterization of flexural properties of natural fiber composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 776
4. Analysis of effect of chemical treatment on flexural property of polymer fiber composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 776
5. Conclusion and perspectives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 782
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 782

1. Introduction main reasons behind the use of cellulose fibers as a constituent

of the natural fiber composites [3]. A variety of natural fibers are
The reinforcement of the cellulose fibers into polymer matrix available in the nature such as flax, hemp, jute, sisal, isora, ferula,
has become an attractive research topic for the researcher over okra, ferula, coir is used as reinforcement in the polymer matrix
the previous decades. Materials from this type of combinations [4–7]. Many automotive industries are using cellulose fibers to
have been studied for find a suitable replacement of synthetic replace conventional fiber like glass and carbon for reinforcement
fibers with cellulose fiber [1,2]. No harmful effect on the environ- into polymer matrix [8,9]. Along with number of benefits of natural
ment and their specific properties are main causes that attract fibers as reinforcement, there are some drawbacks associated with
the interest of researcher toward natural fiber composites. Low- these natural fibers. Natural fibers are not so much stable at ele-
cost production, less energy consumption and vast availability, vated temperature. These have moisture absorption capacity that
biodegradability, low density and high specific strength are the restricts them for moisture milieu applications [10]. It also leads
dimension instability problem for fiber composite [11]. The cause
of this is hidden in the structure of the natural fiber. Cellulose,
Peer review under responsibility of Egyptian Petroleum Research Institute. hemicellulose, pectin, and lignin are main constituents of the nat-
⇑ Corresponding author.
ural fiber. The rich hydroxy-1 group give a strong affinity to natural
E-mail address: msood04@gmail.com (M. Sood).

https://doi.org/10.1016/j.ejpe.2017.11.005
1110-0621/Ó 2017 Egyptian Petroleum Research Institute. Production and hosting by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
776 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783

fibers toward moisture and make them hydrophilic in nature [12]. hemicellulose mostly find in the primary wall of the fiber as shown
On other hand, matrix are mainly polymers like polypropylene, in Fig. 1. An aromatic structured matter called lignin is of amor-
polyvinyl chloride, polylactic acid, which are water repellent in phous in nature. Pectin is constituted with polysaccharides. In
nature [11,13]. Due to the hydrophilic nature of natural fibers addition of these, a little amount of organic and inorganic sub-
and hydrophobic nature of polymer matrix leads a poor interface stances is also present on the natural fiber which is responsible
bonding between these two. The mechanical properties of the for color, odor and decay resistance and abrasive nature of natural
composites deteriorate due to poor bonding between the natural fibers [12,19]. Compositions of some of the natural fibers are
fiber and polymer matrix [12,13]. The surface of the natural fiber mentioned in Table 1.
scan easily modified to change their hydrophilic nature [9]. A num-
ber of chemical treatments are available that can be used to 2.1. Chemical treatments for natural fibers
enhance the functionality of natural fiber polymer composites by
improving the compatibility between the fiber and matrix [14]. Chemical modification of the natural fibers is a process of per-
Apart from the chemical treatments, there is a number of physical manently altering the nature of fiber cell walls by grafting poly-
treatments are used to improve the interface bonding between mers on the surface of fibers. It may happen also with bulking or
natural fiber and the polymer matrix. Physical structure and sur- cross-linking within the fiber cell wall. The different chemical
face properties of fibers can be altered by physical treatments can be used for surface treatment of natural fibers are enlisted in
but by chemical [15]. Different types of chemicals are used for Table 2. The chemical modification provides more dimensional sta-
the treatment of natural fiber. Most of the treatments used on nat- bility, reduce water absorption capacity and give resistance to fiber
ural fibers are alkali treatment. This treatment removes the lignin, against fungal decay [20].
wax, and oil covering part of natural fibers and increases the
roughness of the surface of fibers. This leads a better interlocking
3. Characterization of flexural properties of natural fiber
of fibers with its polymer matrix [16]. Along with these chemical
composites
treatments, reactive coupling agents are also added to explore
more additive groups on fiber surface that enhance coupling of
For evaluation of the flexural properties viz. strength and mod-
fiber with matrix [17]. Flexural properties are an essential require-
ulus, samples of the composites are mostly prepared according to
ment for structural members and glass and carbon fiber reinforced
ASTM D 760 standard [8]. This test is performed mainly on the uni-
composites are replacements of steel reinforcement. But the
versal testing machine (UTM) by three-point bending technique
requirement of environment-friendly material gaining popularity
[11,21]. The three-point bending technique is a material testing
these days [18]. To make natural fiber reinforced composites mate-
method which evaluates modulus of elasticity in bending, flexural
rials a good option for as a structural member, it is required that
stress and flexural strain when the material sample is set up as a
these composites should show a humongous strength under flexu-
simply supported beam under two supports and a load is applied
ral loading. For good flexural strength, natural fiber composites
at a point shown in Fig. 2. For three-point bending test, crosshead
should have good interface bonding between fiber part and matrix
speed recommended 2 mm/min [12].
part. Different chemical treatments used on natural fibers from last
decades (2000–2016) and their effect on flexural properties of
composites have been reviewed which can edify further possibili- 4. Analysis of effect of chemical treatment on flexural property
ties of enhancements of natural fiber reinforced composites. of polymer fiber composites

Nopparut et al. [1] fabricated composites from 20 wt% of

2. Composition of natural fibers pineapple fibers reinforced into nylon matrix. Treatments were
used on pineapple fibers were alkali and silane. Both flexural
Flora based natural fibers are composed of cellulose, hemicellu- strength and flexural modulus were evaluated. Results showed
lose, lignin, pectin and waxy materials. Cellulose is the major that both treatments increased the flexural strength and flexural
constituent of the natural fiber which provides strength, stability, modulus as compared with untreated pineapple fiber composites.
and stiffness to the fibers. Another branched polymer which is On the comparison between treatments, Silane-treated fiber

Fig. 1. Structural constituent of natural fiber cell [96].

 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783 777

Table 1
Constituents of natural fibers [19].

Fibers Cellulose (wt%) Lignin (wt%) Hemicellulose (wt%) Pectin (wt%) Wax (wt%)
Cotton 82.7 0.7–1.6 5.7 – 0.6
Flax 71 2.2 18.6–20.6 2.3 1.7
Palf 70–82 5–12 – – –
Hemp 70.2–74.4 3.7–5.7 17.9–22.4 0.9 0.8
Ramie 68.6–76.2 0.6–0.7 13.1–16.7 1.9 0.3
Sisal 67–78 8–11 10–14.2 10 2
Jute 61–71.5 12–13 13.6–20.6 2.3 1.7

Table 2
Chemical treatments for plant fibers.

Name of treatment Chemical(s) used Chemical Strength of chemical Ref.

Structure
Benzoylation Treatment Benzoyl Chloride C7H5ClO – [48]
Cyclohexane modification Cyclohexane/Ethanol C6H12/C2H6O 1:1 vol/vol [97]
Alkali treatment Sodium Hydroxide NaOH 5%, 10%, 15% [41,98]
Fluorocarbon treatment Perigurard UFC 50 g/L [99]
Silicon treatment Perisoft MSA 20 g/L [99]
Isocyanate treatment Carbon Tetrachloride and dibutyl tin CCl4 and – [100]
dilaurate C32H64O4Sn
Peroxide treatment Benzoyl peroxide or Dicumyle C14H10O4 or 6% solution in acetone [100]
peroxide C18H22O2
Permanganate treatment Potassium Permanganate KMnO4 0.005% in acetone [100]
Acetylation treatment Siliane SiH4 5 wt% in methanol [101]
Treatment with flexible epoxy resin Flexible epoxy resin 1 g resin:200 ml acetone [102]
Sulfuric acid treatment Sulfuric acid H2SO4 1.0% (wt/vol) [103]
Etherification Dodecane bromide, NaOH, Isopropanol C10H21Br, C3H8O 12 ml Dodecane bromide into Isopropanol [104]
solution
Modification with maleic anhydride Maleic anhydride C4H2O3 20 wt% solution into acetone [105]
Stearic acid treatment Stearic acid C18H36O2 1% solution in ethyl alcohol. [106]
Modification with Alkyl ketene dimer Alkyl ketene dimer 3–5% Alkyl ketene dimer in n-hexane [107]
Treatment with Ethylenediaminetetra acetic EDTA C10H16N2O8 Solution of 5 g/l [108]
acid (EDTA)

composites was 16.7% more than that of untreated coir/epoxy fiber

composites. The alkali treatment significantly improved the flexu-
ral strength of composites. Punyamurthy et al. [11] treated abaca
fiber with benzene diazonium chloride and reinforced into
polypropylene matrix for fabrication of composites. Along with
chemical treatments a coupling agent also used. The study clearly
mentioned that the flexural strength of benzene diazonium chlo-
ride composites was higher than that of untreated fiber compos-
ites. Treated composites with coupling agent alone showed
64.91% hike in flexural strength than that of untreated composites.
This treatment and coupling agent extirpated the external fiber
surface and exposed more cellulose content for better fiber-
matrix bonding which led higher strength of treated composites
Fig. 2. Schematic diagram of three-point bending [12].
than untreated fiber composites. Yousif et al. [12] tested the flexu-
ral properties of kenaf fiber reinforced epoxy composites. The
fibers were treated with 6% NaOH solution. The results showed
composites were stronger than that of alkali treated fiber composites. that reinforcement of treated kenaf fibers increased 36% flexural
This was because Silane-treated composites gave higher aspect strength of composites while untreated fiber composites enhanced
ratio than NaOH treated composites. Silane treatment could brakes only 20% of the flexural strength This was due to enhancement on
down large bundle structure of fibers into smaller fibrils more than interface bonding by chemical treatment. Bamboo particle/polyvi-
NaOH treated fibers hence aspect ratio increased as an area of the nyl chloride composites were fabricated by Qian et al. [13] and
interface. Scalici et al. [7] treated Arundo leaf fiber with plasma effect of hydrothermal treatment was investigated on flexural
treatment and reinforced into the epoxy matrix. Fiber composites strength of composites. The treatment improved the flexural
samples were tested by three-point bending technique. From the strength maximum up to 39.75 MPa. Fiore et al. [15] investigated
outcomes of the quasi-static flexural properties, it was revealed the effect of NaOH treatment on kenaf fiber/epoxy composites.
that the flexural modules and flexural strength of treated fiber They evaluated that all composites showed higher flexural moduli
composites were more than that of untreated Arundo fiber/Epoxy than neat epoxy resin. Alkali treatment enhanced the flexural
composites samples at all fiber loadings and length. Yan et al. [8] properties of composites. Alkali treatment gave more positive
investigated the effect of alkali treatment on mechanical properties impact on flexural strength as compared to the flexural modulus
of coir fiber reinforced epoxy composites. After analysis of results, of fiber reinforced composites. Manalo et al. [16] investigated the
it was found that the flexural strength of treated coir fiber/epoxy effect of NaOH treatment and elevated temperature on mechanical
778 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783

properties of bamboo fiber reinforced polyester composites. They flexural strength of ramie/PLA composites increased by addition
found that then composites treated with 6% NaOH had highest of 3% maleic anhydride as compare to untreated ramie/PLA com-
flexural modulus and 25% higher than that of untreated fiber com- posites. A similar trend was showed by data of flexural modulus.
posites. It was also evaluated that this hike in moduli of composites But further increase in maleic anhydride leaded reduction in both
was due to better interface bonding between fiber and matrix part. flexural strength and flexural modulus. Yemele et al. [31] used hot
Yu et al. [22] fabricated Ramie/polylactic acid composites with water treated and untreated black spruce and trembling aspen
diisocyanates as a compatibilizer. They added three different vari- bark fibers and reinforced into high density polyethylene matrix
ants of diisocyanates as a compatibilizer. Flexural strength of trea- with addition of maleic anhydride as coupling agent and lubri-
ted fiber composites was more than that of untreated fiber cants. There was not much difference between flexural modulus
composites. The cause of this was mentioned as improvement in of elasticity and flexural modulus of rupture but less than that of
interface adhesion between ramie and polylactic acid. Zhu et al. the untreated samples in case of black spruce bark fiber. Both mod-
[23] used alkali, acetylation, silane, and enzyme treatments for flax ulus significantly decreased as compared to untreated trembling
fibers and reinforced into mimosa tannin resin. The results showed aspen fiber composites. Hot water treatment removed extractives
that NaOH and Acetylation treatments increased flexural strength from fibers which deteriorate fiber properties that led reduction
by 14.6% and flexural modulus by 6.3% than untreated fiber com- in flexural properties. Vekateshwaran et al. [32] fabricated com-
posites. Apart from the improvement in flexural properties enzyme posites with banana fibers and reinforced into epoxy matrix. The
treatment reduced the flexural strength and modulus by 18.2% and fiber was treated with NaOH solution at different concentrations.
11.7% respectively. The enzyme treatment led severe dissolution of They found that flexural strength of the treated fiber composites
hemicellulose as an interfibrillar matrix which reduced fiber prop- was more than untreated fiber composites because alkali treat-
erties. Srisuwan et al. [24] modified woven sisal fibers by 2% solu- ment of fibers removed the hemicellulose, lignin, and other impu-
tion of NaOH and silane treatment performed on pretreated fibers. rities, from fiber and led enhancement in fiber-matrix bonding,
These treated fibers were reinforced into the modified epoxy resin. fiber wetting characteristics and bonding [33]. It was also evalu-
The flexural modulus of all composites was higher than neat epoxy ated that 1% NaOH solution gave best flexural strength than other
blend matrix. The reinforcement of silanized sisal fibers into blend concentrations of treatments. Shanmugum et al. [34] reinforced
matrix further improvement showed into flexural modulus. The alkali treated Palmyra Palm leaf stalk (PPLSF) and jute fibers into
increasing in flexural modules was continuous with an increase unsaturated polyester matrix. Flexural modulus and strength of
in reinforcement. Prabu et al. [25] treated the banana fibers with hybrid composites increased by 19% and 56% respectively by addi-
NaOH and silane. Along with treatment, 8% of red mud particles tion of treated fibers into polyester matrix. Mir et al. [35] prepared
were added to manufacture banana fiber/polyester composites. polymer matrix composites by reinforcement of coir fibers into
After evaluation of the flexural strength of composites with polypropylene matrix. Raw coir fibers were treated with chromium
untreated fiber with red mud showed the highest reading. Treated sulfate and sodium bicarbonate. It was evaluated that treated fiber
fibers composites with red mud showed less flexural strength. On composites provided more flexural strength and modulus than that
comparison of NaOH and silane treatments, silane treated fiber of untreated fiber composites at all fiber loadings. The treatment
composites showed more strength with red mud addition which time of 3 h provided better strength than 5 h treated fiber compos-
gave better interlocking with the matrix. Bakar et al. [26] evaluated ites. But in case of flexural modulus 5 h. treatment time was better
the effect of grafting with methyl methacrylate of kenaf fibers on than treatment time for 3 h. Fernandes et al. [36] evaluated the
flexural properties of polyvinyl chloride/ethylene vinyl acetate. effect of use maleic anhydride as coupling agent with or without
The grafted fiber composites showed better flexural modulus than sisal fiber treated with NaOH reinforced into Cork-polyethylene
that of ungrafted fiber reinforced of polyvinyl chloride/ethylene composites. Improvement in fiber-matrix composites was evalu-
vinyl acetate composites. This was due to better interlocking ated by alkali treatment. Flexural strength with alkali treated sisal
between fiber and matrix. Ferreira et al. [27] used electron beam fiber with coupling agent increased 98% and modulus increased by
radiation treatment on piassava fibers and reinforced into high- 33% as compared to unreinforced cork-polyethylene composites.
density polyethylene matrix. Glycidyl methacrylate (2.5% and 5%) Jang et al. [37] investigated the effect of pretreatment of seaweed
also added as crosslinking agent. The flexural strength of electron in seaweed/polypropylene composites. The seaweed of two type
beam radiation treated composites reduced as compared to brown algae and green algae treated with bioethanol, biodiesel
untreated fiber composites. But in case of flexural modulus non–ir- and biomethane. Flexural strength of the treated seaweed/
radiate composites showed hike in modulus as compared with polypropylene composites was less than alone polypropylene
neat high-density polyethylene. On other hand irradiate compos- matrix at all loading values. All three treatments did not show
ites showed equal and greater flexural modulus as compared to any positive results. In case of modules at 40 wt% of seaweed load-
irradiate high density polyethylene. Ozerkan et al. [28] treated date ing and sulfuric acid treated composites showed highest modulus.
palm fibers with NaOH and Ca(OH)2 and reinforced into cement Mamun et al. [38] used microfiber obtained from wheat husk, Rye
mortar matrix. The study indicated that reinforcement of the trea- husk and softwood and treated with enzymes. Treated fibers were
ted fibers imparts higher flexural strength to composites. Schirp reinforced into polypropylene (PP) and polylactic acid (PLA)
et al. [29] manufactured composites samples from wood particles, matrix. A coupling agent maleic anhydride was used with
wood flour and thermo-mechanical pulp (TMP) of wood reinforced polypropylene. Unmodified wheat husk/PP composites showed
into high density polyethylene matrix. Wood particles and TMP are less flexural modulus and flexural as compared to enzyme treated
treated with Emulsifiable methylene diphenyl diisocyanate and maleic anhydride treated composites. Enzyme treated wheat
(EMDI), Phenol based resin (PF), Hydrowax and Korlan. The study husk/PP composites were best in modulus. Similar trend was seen
evaluated that flexural strength with TMP fibers not improved as in Rye husk/PP composites. In case of treated wheat husk and Rye
compared wood flour reinforced composites when maleic anhy- husk reinforced PLA composites showed more flexural modulus
dride used as coupling agent. Flexural strength of phenol-based and flexural strength than untreated composites. Yan et al. [39]
resin treated composites was not improved. Only EMDI treatment used noil hemp fibers (NHF) and scotched hemp fibers (SHF) with
was successful which increased flexural strength of composites. maleic anhydride coupling agent and reinforced into polypropy-
Flexural modulus of composites reduced with every treatment. lene (PP) matrix. Flexural strength of SHF/PP (30 wt%) composites
Yu et al. [30] investigated the effect of maleic anhydride as cou- increased when 2.5% coupling agent is added and in case of SHF/
pling agent on ramie fiber/polylactic acid (PLA) composites. The PP composites flexural strength increased relentlessly when
 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783 779

coupling agent increased by 0–5%. Liu et al. [40] treated rice straw alkalization, acetylation, and silane treatment on hemp fiber rein-
with NaOH and hot water and reinforced into corn-based adhesive. forced polyester composites. Among of the all treatments 8% NaOH
Flexural strength was maximum at 10 wt% of starch mass when treated hemp fiber composites showed best flexural strength and
hot water treated corn starch used and NaOH treated showed min- modulus as compared to untreated and other chemical treated
imum strength as compared with untreated composites. Similar composites. Between silanzied and acetylated fiber composites
trend was observed in case of flexural elastic modulus. Hemsri acetylated composites gave better flexural strength and modulus.
et al. [41] treated coconut fibers sodium hydroxide and silane Swapan et al. [48] tested the effect of alkali and silane treatment
and reinforced into matrix of wheat gluten. All treated fiber com- on hemp fiber reinforced polylactide (PLA) and unsaturated polye-
posites showed high maximum flexural stress than untreated fiber ster composites. It was found that the flexural strength of the
composites. Maximum flexural strength was highest in alkali untreated fiber composites was less than all treated fiber compos-
silane treated coconut fiber composites and lowest in silane trea- ites at 20% and 30% fiber loading. Alkali-treated fiber composites
ted coconut fiber composites but higher for untreated composites. gave best flexural strength than silane treated and alkali + silane
Alkali-treated coconut fiber composite showed also more maxi- treated composites at all fiber loadings. Similar trend was observed
mum flexural stress than untreated fiber composites. Asumani in case of flexural modulus. In case of hemp/unsaturated polyester
et al. [42] treated kenaf fibers with alkali treatment and silane (UPE) composites alkali + silane treated composites gave best flex-
treatment and composites fabricated by reinforcing into ural strength and modulus at all fiber loadings. In this case fiber
polypropylene matrix. 5% alkali treated composites gave highest treatment enhanced flexural properties also. This could be
flexural strength at 30 wt% fiber loading. In case of alkali-silane explained by attribution of more enhancement in interfacial bond-
treated fiber composites they gave highest flexural strength at ing between alkali + silane fiber and unsaturated polyester than a
30 wt% fiber loading with 6% NaOH strength. Both gave more single treated fiber composites as shown in Fig. 3.
strength than untreated fiber composites. Sreenivasan et al. [43] Sever et al. [49] used jute fiber sand modified by alkali, micro
treated Sansevieria cylindrical fibers (SCF) with alkali, benzoyl per- emulsion silicon, and fluorocarbons. Composites fabricated with
oxide, potassium permanganate and stearic acid and reinforced treated and untreated fibers. All treated fibers composites gave a
into polyester matrix. Flexural strength showed more in treated hike in flexural strength and modulus as compared with untreated
fiber composites as compared to untreated fiber composites. Max- fiber composites. In a comparison of all treated composites, fluoro-
imum flexural strength obtained from potassium permanganate carbon treated fiber composites had highest flexural strength. But
treated composites. Singha et al. [44] reinforced Agave fibers (Long in case of flexural modulus silicon treated fibers composites were
fibers, particle and short fibers) into polystyrene matrix. Fibers performed better than other treated composites. Rokbi et al. [50]
were modified with graft copolymerization of methacrylate treated Alfa fibers with alkali treatment and reinforced into the
(MMA) with ceric ammonium nitrate as catalyst. The composites polyester matrix. Treated fiber composites provided highest flexu-
treated with showed higher flexural strength at all fiber types ral strength as compared with untreated Alfa fiber composites. 10%
and fiber loading than untreated fiber composites. Best flexural NaOH led 60% hike in flexural strength and 62% hike in modulus.
strength was obtained from treated particle reinforced composites. Marques et al. [51] reinforced recycled newsprint fibers into
Goriparthi et al. [45] used jute fiber and alkali, peroxide, perman- polypropylene matrix along with Fusabond P-613, Polybond 3002
ganate and silane treatments were performed and reinforced into (P1) and Polybond 3200 (P2) coupling agents which were different
polylactic acid (PLA) matrix. Flexural strength and modulus of forms of maleic anhydride grafted polypropylene (MAH-PP) cou-
the treated fiber composites was more than that of the untreated pling agent. Flexural stress and modulus of modified composites
fiber composites. Among of the all treatments Silane treatment found higher at all fiber loadings as compared with neat
gave the highest flexural properties. From other three treatments polypropylene matrix and uncoupled fiber matrix composites.
alkali treatment had lowest flexural strength and modulus evalu- Polybond 3200 (P2) coupling agent provide best flexural stress at
ated but more than untreated fiber composites. Huang et al. [46] 50% fiber loading. Flexure modulus did not improve at large extent
used mechanical activation treatment on sugarcane bagasse fibers by coupling agents. At 10% fiber loading both strength and modu-
and then treated with aluminate coupling agent. For composites, lus decreased by use of Polybond 3200 (P2) and Polybond 3002
both treated and untreated fibers were reinforced into polyvinyl (P1) coupling agent as compared with uncoupled fiber composites.
chloride (PVC) matrix. Both treated composites first mechanically Mylsamy et al. [52] analyzed flexural properties of alkali treated
modified without coupling agent and other coupling agent treated Agave fiber reinforced epoxy composites. Results showed that flex-
without mechanically modified showed 49% more flexural strength ural strength increased from 10 to 15% by reinforcing treated agave
than unmodified composites. Kabir et al. [47] studied the effect of fiber into composites as compared with untreated fiber composites.

Fig. 3. SEM micrograph of flexural tested fractured surfaces (a) UPE/Silane treated (b) UPE/Alkaline + Silane treated [48].
780 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783

A similar type of increment was observed in flexural modulus of of flax fiber reinforced polypropylene composites. In case of flexu-
composites. Hossain et al. [53] modified jute fibers with alkali, ral behavior, 2% zein treated flax fiber composites gave more than
acetic acid, dewaxing and detergent washing and reinforced into double flexural strength as compared with untreated fiber compos-
bipole matrix. The flexural strength and modulus of treated fiber ites at 30% fiber loading. Lui et al. [63] modified jute fibers 2%
composites were higher than untreated fiber composites. Further NaOH, 2 + 5% NaOH and c-methacryloxypropyltrimethoxy silane
improvement was observed when Nanoclay added. Use of 4% Nan- coupling agent and reinforced into poly(butylene succinate)
oclay provided highest flexural strength and 3% Nanoclay addition matrix. After evaluation of flexural strength and modulus, all trea-
provided the highest modulus. Nam et al. [54] Reinforced poly ted fibers composites provided higher values as compared with
(butylene succinate) matrix with coir fibers. The fiber treatment untreated fibers composites at all fiber loadings. Among of the all
was carried out by alkali treatment. Results showed that at all fiber treatments, at 20% fiber loading coupling agent treated fiber com-
loading alkali treated fiber composites provided higher flexural posites gave highest flexural strength and modulus. Rahman et al.
strength and modulus as compared with untreated coir fiber rein- [64] treated abaca fibers with benzene diazonium salt and rein-
forced composites. At 25% fiber loading treated fiber composites forced into polypropylene matrix. Flexural strength and modulus
gave highest flexural properties. Sever et al. [55] treated jute fibers of treated fiber composites found more than that of the untreated
with oxygen plasma treatment and reinforced into high-density fiber composites at all fiber loadings. Highest flexural strength and
polyethylene matrix. Two type LF-plasma system and RF-plasma modulus calculated at 25% fiber loading of treated abaca fibers
system used for modification of jute fibers. Flexural strength of reinforced composites. Sangthong et al. [65] used sisal fibers for
treated fiber composites found higher than untreated fiber com- reinforcement into unsaturated polyester matrix. Fibers were trea-
posites apart from composites treated with LF plasma system at ted with admiceller polymerization (Methyl methacrylate) and
90 W. Cerqueira et al. [56] investigated the effect of chemical treat- flexural properties evaluated. Untreated fibers composites per-
ment on sugarcane bagasse reinforced polypropylene composites. formed lowest in case of flexural strength and modulus when com-
Fibers treated with 10% sulfuric acid solution followed by 1% NaOH pared with treated fiber composites.0.1% treated sisal fibers at 30%
solution. Reinforcement of treated fiber improved flexural proper- fiber loading showed highest flexural strength and similar trend
ties of treated fiber composites as compared with untreated fiber followed by modulus. Seki et al. [66] used jute fibers and reinforced
composites. Goulart et al. [57] studied the effect of coupling agent into unsaturated polyester and epoxy resin. Fibers were treated
in flexural properties of palm/polypropylene composites. 2% maleic with alkali and followed with oligomeric siloxane treatment. Both
anhydride polypropylene coupling agent enhanced flexural alkali-treated and siloxane treated jute fibers composites gave
strength from 22.6 MPa to 24.4 MPa and similarly, modulus hiked higher flexural modulus and strength as compared with untreated
from 641.2 MPa to 738.7 MPa. Xie et al. [20] used glutaraldehyde jute fiber reinforced unsaturated polyester and epoxy composites.
(GA) and 1,3-dimethylol-4,5-dihydroxyethyleneurea (DMDHEU) In case of jute/epoxy composites, siloxane treatment provided
as a treatment for wood particles and reinforced into polypropy- highest strength and modulus as compared with alkali treated
lene matrix. Flexural modules increased by 8.6% and 12% when composites. Same highest strength and modules found with silox-
treated with GA and 0.2 M of DMDHEU respectively as compared ane treatment in jute/polyester composites. Sreekumar et al. [67]
to untreated samples. Reduction in flexural strength observed used treatments like alkalization, heating at 100 °C, benzoylation,
when fibers treated with respective chemicals. The main culprit silanization and permanganate treatment on sisal fibers and rein-
in this case was increase in the concentration of chemical strength forced into polyester matrix. By evaluation of flexural strength
that led further reduction in flexural strength. Bledzki et al. [58] and modulus both were lowest in case of untreated sisal fiber com-
fabricated composites by reinforcing abaca fibers into polypropy- posites. Permanganate treated sisal fibers composites showed
lene matrix. These fibers were modified with fungamix natural highest flexural strength than other treatments and silane treated
enzymes. Maleic anhydride grafted polypropylene (MAPP) cou- sisal fiber composites gave highest modulus at same fiber loading.
pling agent also used to modify these fibers. Another type naturally Benzoylation gave lowest strength and modules among all treat-
treated (elephant dung) abaca fibers used to fabricate composites. ments. Huda et al. [68] fabricated laminated composites from
Flexural strength of all treated fiber composites hiked as compared kenaf fibers and reinforced into polylactic acid (PLA) composites.
with untreated fiber composites. Among of all treated composites, Modification of fibers were done with alkalization and silane treat-
MAPP treated composites showed highest flexural strength. Funga- ment. The flexural strength of the treated fiber composites treated
mix treated fiber composites gave little less strength than previ- with chemicals gave high flexural strength as compared with
ously mentioned composites. Elephant dung treated fiber untreated fiber composites but less than the strength of pure PLA
composites had lowest flexural strength but were more than that matrix due to poor interface bonding between fibers and matrix.
of untreated fiber composites. Islam et al. [59] investigated alkali Flexural modules showed opposite trends. Alkali + silane treated
treatment effect on hemp fiber reinforced polylactic acid (PLA) kenaf fiber composites showed highest flexural modules as com-
composites. In case of flexural strength, align alkali treated long pared with untreated fiber composite and neat PLA matrix. Luz
fiber composites gave the highest strength as compared with et al. [69] developed cellulose and cell-lignin sugar cane bagasse
untreated fiber composites and neat PLA matrix. Same fashion fiber/polypropylene (PP) composites and effect of acetylation was
observed in case of flexural modulus. John et al. [60] treated kenaf studied by obtaining flexural strength. Strength of 10% and 20%
fiber with a coupling agent Zein (2%) and reinforced into fiber weight untreated cellulose/PP composites was more than
polypropylene. After evaluation of flexural strength and modules, acetylated treated cellulose fiber composites at given fiber loading.
treated fibers composites gave higher values as compared with Similar detrimental effect found in treated cell-lignin fiber com-
untreated fiber composites. Haque et al. [61] used coir and palm posites. Rahman et al. [70] fabricated jute fiber polypropylene
fibers and reinforced into polypropylene matrix. Both fibers were composites. For reinforcement jute was oxidized treated. Compos-
treated with benzene diazonium salt. At all fiber loadings treated ites with oxidized jute reinforced had higher flexural strength than
coir fibers, composites showed highest flexural strength as com- that of untreated jute/polypropylene composites at all fiber load-
pared with untreated coir fiber composites. In case of palm fiber ings. Sgriccia et al. [71] used kenaf fibers and hemp fibers and
composites, treated palm fibers composites performed well as cured with oven and microwave and reinforced into epoxy matrix.
compared to untreated fiber composites. Between two treated fiber Both curing treatments showed similar trends in flexural modulus
composites coir fiber composites gave the highest strength. John in kenaf and hemp fiber composites. Both fibers were treated with
et al. [62] studied the effect of zein as coupling agent modification alkali, silane and alkali + silane and reinforced into epoxy matrix
 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783 781

and composites were cured with microwave and oven. From all of performed better than short fiber treated composites and treated
composites, silane treated kenaf fiber composites with microwave kenaf/CNSL composites showed highest flexural properties. Liu
cured provided highest flexural modules and silane treated hemp et al. [82] studied the influence of alkali treatment on Indian grass
fiber composites with microwave treated showed lowers modules. reinforced soya protein based biocomposites. Flexural strength of
Vilay et al. [72] reinforced bagasse fibers into unsaturated polye- composites increased with reinforcement of treated fiber and solu-
ster. Bagasse fibers were treated with NaOH and acrylic acid. tion concentration as compared with untreated grass fiber com-
Acrylic acid treated fiber composites showed best outcomes in posites. It was highest when 10% NaOH used for 4 h. on fibers.
terms of flexural strength and modulus as compared with Flexural modules of treated grass fiber composites did not increase
untreated and NaOH treated bagasse/unsaturated polyester com- by large amount as compared with untreated fiber composites.
posites at all fiber loadings. Highest strength and modulus Weyenberg et al. [83] reinforced flax fibers into epoxy matrix
observed at 20% fiber loading with acrylic treated composites. and investigate effect of chemical treatments like alkali, diluted
Kim et al. [73] studied effect of maleic anhydride grafted epoxy, acetone and silane. Out of the all treatments the combina-
polypropylene (MAPP) coupling agents (polybond-3510, tion of alkali and diluted epoxy gave highest flexural strength
polybond-3200, G-3003, E-43 and bondyram-1004) on wood flour and modulus. This combination of treatment enhanced 40% longi-
and rice husk flour/polypropylene composites. Flexural strength of tudinal flexural strength and 60% stiffness but strength and stiff-
non-treated composites declined as compared with treated flour ness increased by 200% and 500% in transverse fiber loading.
composites. From the two reinforcements wood flour reinforced Cantero et al. [84] fabricated composites with flax fibers and flax
composites with polybond-3200 MAPP compatibilizer showed pulps by reinforcing into polypropylene matrix .Maleic anhydride
highest flexural strength. Weyenberg et al. [74] reinforced treated (MA), maleic anhydride grafted polypropylene (MAPP) and vinyl
and untreated flax fibers into epoxy resin. For treatment NaOH 1%, trimethoxy silane (VTMO) treatments performed to improve inter-
2% and 3% solution strength used. NaOH treatment increased flex- face bonding between fibers and matrix. Only 5% and 10% MA-
ural strength and modules as compared with untreated flax fiber treated fiber composites showed higher flexural modulus than
composites. At 1% of NaOH both strength and modules was highest. untreated flax fiber composites. Treatment with MAPP and VTMO
Kaddami et al. [75] used acetic acid and maleic anhydride to mod- reduced this strength. In case of flax pulp treated composites only
ify palm fibers and reinforced into polyester and epoxy matrix. 5% MA-treated pulp flax composites enhanced flexural modulus.
Flexural modulus of unmodified palm fiber/epoxy composites Any treatments did not show any improvement in flexural strength
was lower than treated fiber composites. But in case of polyester of flax fiber composites but 5% and 10% MAPP flax pulp/polypropy-
based composites modification of palm fibers reduced flexural lene showed highest flexural strength as compared with strength
modulus of composites. Kuan et al. [76] reinforced wood flour with of other composites. Escamilla et al. [85] grafted poly methyl
and without treatment into linear-low density polyethylene methacrylate (PMMA) and poly butyl acrylate (PBA) with hene-
(LLDPE). Silane-treated fiber composites performed well than quen fibers and reinforced into PMMA and poly styrene-co-
untreated composites. At 30% fiber loading silane treated fiber acrylonitrile (SAN) matrix polymer. Both type of composites
composites gave highest flexural strength. Arbelaiz et al. [77] man- showed less flexural modulus as compared with grafted fiber rein-
ufactured flax fiber/polypropylene. Modification of fiber performed forced composites. Relative flexural strength of PMMA-g-
through maleic anhydride (MA), silane, peroxide, maleic anhydride henequen/PMMA composites found more than untreated and
grafted polypropylene (MAPP) and alkalization. MAPP and alkaliza- PBA grafted henequen/PMMA composites. Similar behavior
tion increased flexural strength as compared with untreated com- described by PMMA-g-henequen/SAN composites. Marcovich
posite. On other hand MA and silane treated composites showed et al. [86] modified wood flour with maleic anhydride and NaOH
very little increment in flexural strength as compared with and reinforced into unsaturated polyester matrix. Flexural strength
untreated flax/polypropylene composites. On using of combination and modulus of untreated treated wood flour composites was
of MA + peroxide and silane + peroxide modifications both gave higher than treated wood flour composites. Ray et al. [87] rein-
higher flexural modulus and strength as compared with untreated forced alkali treated jute fibers into vinyl ester resin. 4 h NaOH
fiber composites. Maleic anhydride and peroxide was best combi- treated fiber composites gave highest flexural strength and com-
nation for treatment of flax fiber to enhance flexural properties. pared with untreated composites at all fiber loadings. Highest flex-
Franco et al. [78,79] reinforced short and continuous henequen ural modules given by 4 h. NaOH treated jute/polyester composite
fibers into polyethylene matrix. Alkali and silane coupling agent at 35% fiber loading. Rout et al. [88] fabricated coir/polyester com-
and its combination used of fiber for treatments. These treatments posites Coir is treated with alkali, bleaching and acrylonitrile graft-
also enhanced flexural strength of the short and fibers composites ing. 5% NaOH treated, bleached at 65 °C and 10% acrylonitrile coir/
than those composites which fabricated from untreated fibers. polyester composites showed highest flexural strength. Gassan
From all three treatments. Silane-treated short fiber composites et al. [89] treated jute fibers with corona discharge and ultra-
showed highest flexural strength. Similar trend was followed in violet rays and reinforced into epoxy matrix. It was concluded that
continuous henequen fiber composites. Both strength and modulus under optimum treatments conditions 30% increment of flexural
in transverse and longitudinal fiber loading with treated fiber com- strength was achieved. Khalil et al. [90] prepared carbon black
posites was higher than untreated fiber composites. Aziz et al. from bamboo stem, coconut shell, and oil palm empty fiber bunch
[80,81] conditioned long and short hemp and kenaf fibers with and reinforced into epoxy matrix. Both flexural strength and mod-
0.6 M NaOH and reinforced into polyester resin. All treated fiber ules was observed at peak when epoxy reinforced with coconut
composites showed higher flexural strength and modulus than shell and carbon black. Alvarez et al. [91] applied acetylation and
untreated fiber composites. Composites with long treated kenaf alkalization on sisal fibers and reinforced into MasterBi-Y polymer.
fibers provided highest flexural modulus and strength as compared Composites treated with 5% wt/vol gave highest flexural proper-
with other treated fiber composites. Compared with long fiber ties. Arbelaiz et al. [92] reinforced short flax fibers bundle into
composites, both flexural strength and modulus of short fiber com- polypropylene composites and maleic anhydride grafted
posites was low. again, treated long and short hemp and kenaf polypropylene (MAPP) as E43 and G3003 used as compatibilizer.
fibers and treated with 6% NaOH solution and reinforced into At 60% fiber loading and 10 wt% of G3003 flax/polypropylene com-
cashew nut shell liquid (CNSL) resin. Strength and modulus of long posites showed highest flexural strength but modulus was found
and short treated fibers composites was more than that of highest when 5 wt% E43 coupling agent used. Yu et al. [93] rein-
untreated fibers composites. All long treated fibers composites forced ramie fibers into polylactic acid (PAL) matrix. The ramie
782 M. Sood, G. Dwivedi / Egyptian Journal of Petroleum 27 (2018) 775–783

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