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https://doi.org/10.1007/s12633-019-00275-6
ORIGINAL PAPER
Abstract
In this research, the PLA- biocomposite and PLA- hybrid biocomposites were prepared with twin screw extruder, two-roll mill,
and compression molding method. The PLA based bio-composites are fabricated with 30% of treated aloevera fiber and 0, 1, 2
and 3 wt% nanoclay filler. The influence of MMT clay on thermal, mechanical and barrier properties of PLA-biocomposite and
PLA-hybrid biocomposites has been studied. The PLA-hybrid biocomposites thermal, mechanical and water resistance proper-
ties are increased with adding of MMT clay. However, 1 wt.% MMT included PLA-hybrid biocomposites exhibits increased
tensile, flexural, impact and abrasion resistance properties than PLA- biocomposite, the improvements 5.72, 6.08, 10.43, and
45.71% respectively are observed. The PLA-bio and hybrid biocomposites showed higher tensile modules 25.76, 18.84, 31.53
and 32.30% respectively, and flexural modules 61.42, 60.95, 66.66 and 79.04% respectively, than pure- PLA. The results TGA
analysis depicted that inclusion of MMT clay can improve the decomposition temperature of the PLA-biocomposites. The
addition of 3 wt.% MMT clay can improve the PLA- biocomposite decomposition temperature from 295 to 299o C in T 10%
likewise 338 to 350o C in T 75%. SEM analysis discloses that, MMT clay not only improves micro-structure and also it acts as a
load transfer mechanism. The Physical barrier properties and biodegradability results show that water resistance of biocomposites
improved and biodegradability decreased due to adding of MMT clay.
Keywords Polylactic acid . Aloevera fiber . NaOH treatment . Montmorillonite clay . Thermo- mechanical . Physical barrier and
biodegradability properties
more dissimilar fibers in a common polymer matrix or rein- At present, nano particles or fillers such as organically
forced with polymer blends [16–18], and it offers most modified montmorillonite(OMMT) and montmorillonite
attracting potential application in non structural, semi structur- (MMT) nanoclay getting higher consideration as they possess
al and structural industrial sectors [19]. the potential tendency to modify extensively the thermal, me-
Hybrid technology creates the new revolution in the area of chanical and functional properties of both thermoplastic and
material science showing the most high-tech advanced com- thermoset polymers [32, 33]. The various nano clay are pyro-
posites. The adding of nano particles demonstrates remarkable phyllite, organo clay, hectorite, saponite and nontronite
enhancement in the thermal, mechanical, physical thermo- nanoclay, montmorillonite (MMT) nanoclay; among these
mechanical properties due to perfect distribution, a high spe- montmorillonite (MMT) nanoclay is the most commonly used
cific ratio and effective polymer filler interaction [13, 20]. layer silicate in polymer composites due to its high strength,
In the different types of natural resources, plant fibers low cost, high aspect ratio and high modulus [33, 34].
are low cost, low density, easy to handle and comparable Several systems are being considered for get better proper-
mechanical properties over synthetic fibers [21]. Among ties and diminish of PLA cost. The produced PLA-
the plant based fibers, aloevera fiber is identified as most biocomposites has established to be a successful technique
important one for biocomposites study because of its to attain ideal properties [1, 35–38]. Some scientists are
availability, acceptable specific strength and low cost. achieving the preferred properties through hybridization
Aloevera plant (Aloe barbadensis Miller) also called me- method like addition of fillers and or natural fibers into the
dicinal plant and it is widely used in food, cosmetic and conventional polymers or plastics [39, 40]. Chaitanya et al.
pharmaceutical or drugs industries since thousands of [24] have reported that treatment and 30% fiber content en-
years [22]. Aloevera plants were widely cultivated in hanced mechanical and thermal properties of the PLA/
India, Florida, South Texas, United States i.e. South aloevera fiber biocomposite. N Saba et al. [19] investigated
California, Africa, South and Central America, Australia, and compare the morphological and mechanical properties of
Iran and Caribbean [23]. Its look like a sisal plant, but in OPEFB/kenaf/epoxy, OMMT/kenaf/epoxy and MMT/kenaf/
reality different in nature; these are easily cultivated and epoxy hybrid composites. Q Meng et al. [41] experimented
low maintenance plant, and ability to stay alive through the effects of nanoclay on mechanical and thermal properties
hard weather circumstances in a rocky terrain and pro- of PLA/clay/wood nanocomposites. V Sajna et al. [42] devel-
vides economic benefit [24]. Aloevera gel was extracted oped the banana/PLA/nano clay hybrid green nanocompos-
from the leaves and leaving the outer shell (residue). The ites. M Kaiser et al. [43] studied the effects of process routes
fibers extracted from these leftover leaf shells by using on morphological, mechanical and thermal properties of PLA/
retting method and are at currently use in small textile kenaf/ nanoclay biocomposites. E.Jalalvandi et al. [44] have
industry in southern India [25]. researched the influence of MMT clay on mechanical, water
Chemical or surface modification methods can decrease the absorption, biodegradability and physical barrier properties of
aloevera fiber disadvantages like hydrophilic nature, low ther- starch/PLA hybrid biocomposites. M.N Azmi et al. [45]
mal resistance, durability, low water resistance and poor com- analysed the optimum concentration of MMT clay in kenaf-
patibility between polymer and fiber. In case of plant fibers, PP/PLA-MMT clay hybrid biocomposites. P Ramesh et al.
the presence of lignin, wax, pectin and hemicelluloses are [46] investigated mechanical properties of PLA/treated kenaf
expected to hinder the edge bonding between the polymer fiber/MMT clay hybrid biocomposites.
and fiber. Chemical modification for fiber is general technique Every one of the above researchers some have attempted to
to reduce moisture absorption and improves the adhesion be- determine appropriate hybrid-composites with preferred prop-
tween the hydrophobic polymer matrix and hydrophilic natu- erties. It is the evident from literature review that no one has
ral fibers [26]. In several cases, it is potential to make compat- tried to combine PLA, treated aloevera fiber (TAF) and mont-
ibility between the two materials by introducing maleic anhy- morillonite (MMT) clay. So far investigators knowledge this
dride and silane type coupling agent, which can reduce the is the first article on PLA/TAF/MMT clay hybrid
water absorption in the composites [27]. The various chemical biocomposite prepared via compression molding method.
modification methods such as alkaline, peroxide, acetylating, The PLA/TAF biocomposite and PLA/TAF hybrid
silane and benzoylation treatments have been studied in the biocomposites having total 30 wt.% of TAF loading by weight
past [26]. Among them, alkaline treatment (NaOH) is inex- together with 1, 2 and 3 wt.% MMT clay loading in PLA/TAF
pensive, easy and effective method when compared to other hybrid biocomposites are fabricated by twin screw-extruder-
methods. Alkaline method expected to remove lignin, wax compression molding method.
and pectin on the fiber as well roughen the surface, facilitating The main objective of this article is to investigate the
superior interlocking and adhesion between the polymer and effect of MMT clay loading on mechanical, morphologi-
fiber [28–30]. The NaOH concentration, immersion time and cal, thermal, physical barrier and biodegradability proper-
temperature influence the properties of composites [31]. ties of PLA/TAF biocomposite and PLA/TAF/MMT clay
Silicon
hybrid biocomposites. The results are also compared with temperature profile were set to 78 rpm and 155o C to 190o C
PLA/TAF biocomposite and virgin PLA in order to devel- respectively. Then, compounded pellets are kept in oven for
op biodegradable hybrid biocomposites with improved dry at 80 °C for 4 h. After drying, the compound pellets are
performance characteristics. pre-melted at 185 °C in a counter rotating two roll mill internal
mixer through a revolve speed of 50 rpm. Afterwards, the
compounded pellets are processed through compression
2 Experimental molding machine. During the process, keep the temperature
185 °C and 30 ton force applied (up stroke); then compacted at
2.1 Materials 165 °C bar pressure for 30 min followed by cool under pres-
sure. When the mold temperature reached at 90o C the platens
In this research pellet formed 3052D PLA with 1.24 g/cm3 at are opened from press; then composite sheets (200 mm X
specific gravity, 145-160o C of melting temperature and 55-60o 200 mm X 3 mm) are removed from platens and cut to desired
C of glass transition material acquired from Nature Tech. The form for tensile, flexural, impact, abrasion resistance,
aloevera fiber supplied through Go-Green Products, India. The thermogravemetric analysis, water absorption and biodegrad-
NaOH was supplied by SR-Scientific Chemicals, Tirupati, AP ability evaluations. The same procedure is followed for prep-
in India. The 1-3 mm long chopped fibers are used. The 1.01 g/ aration of bio and hybrid biocomposites. Virgin- PLA sheet is
cm3 density MMT clay (Nanomers® I.31PS) by modifying produced through two roll mill- compression molding.
onium ion, powder formed with ≤20 μm sized is procured from
Sigma-Aldrich at Bangalore, India. It contains 0.5–5 wt% 2.2.3 Mechanical Characterizations
aminopropyltriethoxysilane, and 15 to 35 wt% octadecylamine.
Tensile test of PLA-biocomposite and PLA-hybrid
2.2 Methods biocomposites is carried out by Instron-3369 Universal
Testing Machine-USA according to ASTM D638 at 25o C.
2.2.1 Fiber Surface Modification Speed of cross head is 10 mm/min. Flexural test of
biocomposites also performed through the same UTM
The NaOH treatment method is applied for aloevera fiber i.e.50KN load and 50 mm span length according to ASTM
surface modification. The pellet formed Sodium hydrox- D790–03 at 18o C. Impact test of biocomposites are finding
ide (NaOH) was provided by S.R.S. Chemicals at through Izod testing machine according to ASTM D256 at
Tirupati, India. Aloevera fibers are covered with water 18 J load. Abrasion resistance test is carried out by abrasion
in 6% NaOH solution for 3 h at room temperature. The machine according to ASTM D1044 standards for 100 cycles.
aloevera fibers then bathe with flowing distilled water.
The pH value kept 7 as constant. Afterwards, the treated 2.2.4 Morphological Characterizations
fibers kept in oven at 100o C for 8 h.
JSM-IT500 scanning electron microscope (SEM) (Japan
2.2.2 Preparation of PLA- Hybrid Biocomposites Electronics Optic Limited, USA) was used to examine the
break surface of tensile fracture specimens. The gold coating
The produced composites formations were tabulated in is coated to samples through vacuum sputter coater.
Table 1 Prior to fabrication of sample PLA, TAF and MMT
clay were held in oven at 110o C for 1 h. The PLA, TAF and 2.2.5 Thermal Characterizations
MMT clay are physically pre-mixed and then compounded
through (ZV 20 model) twin-screw extruder. Screw diameter The PLA-biocomposite and PLA-hybrid biocomposites ther-
and L/D ratio were 21 mm and 40, respectively. For mal stability is carried out through TGA (Thermogravemetry
compounding of all PLA-composites, screw speed and analysis) by Perkin Elmer instrument. The samples (5–30 mg)
P PLA 100 0 0
A PLA-30TAF 70 30 0
A1 PLA-30TAF-1MMT 69 30 1
A2 PLA-30TAF-2MMT 68 30 2
A3 PLA-30TAF-3MMT 67 30 3
Silicon
70 9
8
Impact strength, kJ/m2
acid/polycaprolactone nanocomposites enhanced higher me- biocomposite (A1) tensile and flexural modules are improved
chanical properties than 3% MMT-PLA/ polycaprolactone, 18.84% and 60.95% respectively than virgin- PLA (P). The
5% MMT-PLA/ polycaprolactone and 7% MMT-PLA/ addition of treated fiber and MMT into PLA the tensile and
polycaprolactone nanocomposites. flexural modulus was expected increment, since introduced
The PLA-biocomposites, PLA-hybrid biocomposites ten- stiffer materials or reinforcement into the polymers [52–54].
sile and flexural modulus are plotted in Figs. 4 and 5. The Similar trend observed in previous studies [55]. El-Shekeil
PLA-biocomposite (A) flexural and tensile modules are pro- et al. [56] studied that the treatment and fiber content influ-
gressively increased with addition of TAF. The PLA- ences the tensile and flexural moduli [57]. Adversely, as
biocomposite (A) and PLA- hybrid biocomposites (A1, A2 shown Figs. 1, 2 and 3 impact, tensile and flexural strength
and A3) have greater flexural and tensile modules than (P) are detrimental with natural filler. As example, the PLA/TAF
virgin PLA. PLA-biocomposites (A) flexural and tensile mod- biocomposites impact strength is decreases from 56.69 to
ules are improved 61.42 and 26.15% respectively than virgin- 50.39 kJ/m2; the flexural strength is reduced from 104.16 to
PLA (P). Additionally, 1 wt.% MMT/PLA/TAF hybrid 94.76 MPa; the tensile strength is diminished from 57.06 to
53.88 MPa. According to Yang et al. [58] and Ismail et al. [59]
4 this diminish is recognized due to the irregular shapes, fiber
inability, stresses transferred (support from matrix), micro-
3.5 voids and various processing procedures [60].
Tensile modulu, GPa
properties by having micro-voids and agglomerations forma- bending and fiber pullouts (Fig. 7c). The voids and agglom-
tions; these are reduced both fiber-PLA bonding and load erations are formed due to higher load of MMT clay.
transfer capacity; similar mechanism observed in previous Addition of 3 wt.% MMT clay -PLA/TAF hybrid
study [61, 62]. The nano clay content plays a vital role in biocomposites demonstrates more number of agglomera-
improved performance of PLA-hybrid biocomposites, the tions, micro-voids, fiber bending and pullouts (Fig. 7d)
lowered content enhanced higher mechanical properties. These failure mechanisms of PLA- biocomposite and PLA-
hybrid biocomposites are confirmation for enhancement of
3.1.1 Abrasion Resistance mechanical properties. For example, the adding of 1 wt.%
MMT clay -PLA/TAF hybrid biocomposite reveals superior
Performed PLA- biocomposite and PLA- hybrid mechanical properties (Figs. 1, 2, 3, 4 and 5) which indicates
biocomposites abrasion resistance results are shown in better bonding agent among by the sequence of fiber-nano-
Fig. 6. It is obvious that 1% MMT clay biocomposite (A1) matrix that leads to superior load transfer capacity (Fig. 7b).
shows higher abrasion resistance than other. The 1% clay im-
proves the bonding between PLA and TAF; it is evident from 3.3 Thermal Characterization or TGA Analysis
mechanical and morphological results. After more than 1%
MMT clay affects the abrasion resistance of biocomposites. Thermal stability of PLA- biocomposite and PLA- hybrid
Previously the similar effect was observed in previous work biocomposites were investigated by thermo gravimetric anal-
[63]. The mechanical results followed the same trend. ysis (TGA). Figure 8 shows PLA-biocomposites and PLA-
hybrid biocomposites of the TGA curve. The hybridization
improved thermal stability of biocomposite as evidenced from
3.2 Morphological Properties Thermo gravimetric curve. The 10 and 75% weight loss tem-
peratures [47] set as base line for analyzing thermal stability of
Figure 7a–d shows the PLA- biocomposite and PLA- hybrid PLA-biocomposites and PLA-hybrid biocomposites. The T10
biocomposites structures. Multiplicities of failure mecha- and T75% of PLA- hybrid biocomposite improved 295o C to
nisms such as fiber pullouts, fiber-matrix debonding, voids, 299o C and 338o C to 350o C (Table 2). The decomposition
agglomerations, matrix failure and fiber rupture are ob- takes place in three-stages. In the primary stage moisture evap-
served. The TAF/PLA biocomposites (Fig. 7a) shows some oration occurred up to 150o C and in second phase due to
de-bonding between the fabrics and matrix, pullouts. The l i g n i n , c e l l u l o s e a n d h e m i c e l l u l o s e s . F i n a l l y,
adding of 1 wt.% MMT clay PLA/TAF biocomposites depolymerisation of PLA, MMT clay takes place. The virgin
(Fig.7b) illustrates fine bonding agent between fibers to ma- PLA thermal stability diminishes with adding of natural fiber.
trix by the bonding of fiber-nano-matrix. In the same way Generally, common trend was the polymer thermal stability
the 2 wt.% MMT clay based PLA-hybrid biocomposites decrement with adding of natural fiber [47, 64, 65]. For PLA-
shows uneven surface, small voids, agglomeration, fiber biocomposite (A) and PLA- hybrid biocomposites (A1, A2
and A3) 10% mass loss were degraded at 295, 296, 299 and
5 299 respectively. About 75% weight loss at 338, 342, 344 and
350 respectively. For 10 and 75% weight loss the pure PLA
degrades at 327 and 3580 C respectively.
4
Weight Loss, mg
Fig. 7 SEM images of (a) A, (b) A1, (c) A2 and (d) A3 biocomposites
period. At the beginning period, the water absorption for biocomposites. The water resistance increased maximum with
all samples are improved significantly and then reached to continuous adding of MMT clay. This phenomenon attributed
equilibrium. The Fig. 9 demonstrates for all specimens because of fiber treatment and MMT clay presence in PLA/
that, water gain percentage is increased with increasing TAF biocomposites; the clay act as barrier medium and it
of submerging time. The virgin PLA water barrier proper- restricts flow of water into biocomposites in all path way, thus
ty decreased with adding of TAF. resultant in lower water uptake as described in the literature
However, the incorporation of MMT clay effectively raises [69–71]. As consider the effect of MMT clay on water resis-
the water resistance for clay-filled TAF/PLA hybrid tance of hybrid biocomposite, the 3 wt.% MMT contained
hybrid biocomposite (A3) exhibited excellent water resistance
120
12
4 Conclusions
10
Water absorption, %
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Publisher’s Note Springer Nature remains neutral with regard to
reinforced poly (lactic acid) composites: evaluation of the
jurisdictional claims in published maps and institutional affiliations.
physicomechanical and morphological properties. J Appl Polym
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