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http://dx.doi.org/doi:10.1016/j.ijbiomac.2014.03.013
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5-3-2014
7-3-2014
Please cite this article as: K.R. Rajisha, L.A. Pothan, Z. Ahmad, S. Thomas,
Preparation and Characterization of Potato Starch Nanocrystal Reinforced Natural
Rubber Nanocomposites, International Journal of Biological Macromolecules (2014),
http://dx.doi.org/10.1016/j.ijbiomac.2014.03.013
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Nanocomposites
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*Corresponding author:
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Sabu Thomas, Centre for Nanoscience and Nanotechnology, Mahatma Gandhi University,
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Abstract
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Potato starch nanocrystals were found to serve as an effective reinforcing agent for natural rubber
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(NR). Starch nanocrystals were obtained by the sulfuric acid hydrolysis of potato starch granules.
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After mixing the latex and the starch nanocrystals, the resulting aqueous suspension was cast into
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film by solvent evaporation method. The composite samples were successfully prepared by varying
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filler loadings, using a colloidal suspension of starch nanocrystals and NR latex. The morphology of
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the nanocomposite prepared was analyzed by Field Emission Scanning Electron Microscopy
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(FESEM) and Transmission Electron Microscopy (TEM). FESEM analysis revealed the size and
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shape of the crystal and their homogeneous dispersion in the composites. The crystallinity of the
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nanocomposites were studied using XRD analysis which indicated an overall increase in crystallinity
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with filler content. The mechanical properties of the nanocomposites such as stress-strain behaviour,
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tensile strength, tensile modulus and elongation at break were measured according to ASTM
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standards. The tensile strength and modulus of the composites were found to improve tremendously
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with increasing nanocrystal content. This dramatic increase observed can be attributed to the
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formation of starch nanocrystal network. This network immobilizes the polymer chains leading to
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1. Introduction
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Nanocomposite materials find considerable interest recently among researchers and industrialists.
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Synthetic nanomaterials lack easy processability, biocompatibility, and biodegradability and hence
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superior thermal, barrier and mechanical properties can be synthesized from biopolymer and
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nanosized reinforcements. They are formed by the combination of natural polymers and inorganic
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nanocomposites, which involve synthetic polymers, these biohybrid materials exhibit improved
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inherent to the biopolymers, biocompatibility and biodegradability, open new prospects for these
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hybrid materials with special incidence in regenerative medicine and environment friendly materials
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field closely related to significant topics such as biomineralization processes, bioinspired materials,
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multifunctionality represents a promising research topic that takes advantage of the synergistic effect
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of biopolymers with inorganic nanometer-sized solids. Raw materials often used for these new
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nanostructured composites are natural polymers; clay and nanowhiskers of chitin and cellulose. A
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possible source of inspiration for the design of new high performance bionanomaterials is due to the
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Starch is an abundant biopolymer, which is totally biodegradable. Starch nanocrystals obtained from
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starch have been used as fillers in polymeric matrices leading to desired reinforcing effect [2-4].
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During the last decade, nano-material derived from natural polymers have been used as
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reinforcement in polymers and have been named as green bionanocomposites [5]. Many research
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works published in the area of starch based bionanocomposites show the relevance on this topic in
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the current scenario of polymer research [6-9]. Chitin, cellulose and starch are the crystalline
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residue that can be obtained from different natural polysaccharides with a uniform structure after
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acidic or alkaline hydrolysis. These nanoparticles from different sources have different geometrical
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Similar to conventional
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The properties
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characteristics. For example, the nanocrystals obtained from cellulose [10] and chitin [11] have a
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rod shaped structure while that of starch have a platelet shaped structure[12].
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However, nanocrystals from polysaccharides have the limitation of being hydrophilic and hence are
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usually the weakest point in a biocomposite, which results in the poor performance of the final
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composite . In order to improve the compatibility between the reinforcing phase and the polymer
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matrix, the nanoparticles can be physically or chemically modified [12]. An effective method for
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chemical modification is to graft polymer chains from the matrix directly onto the surface of
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interphase between polysaccharide phase and the polymer matrix phase can improve interfacial
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adhesion. In addition, entanglements between grafted and ungrafted polymer chains are expected to
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occur if the molar weight is high enough. By this approach, nanocomposite materials with high
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materials for nanocomposite preparation are starch and cellulose, but an increasing attention is also
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given to the application of the other biopolymers such as chitin and chitosan [14].
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Starch is a well-known polymer naturally produced by plants in the form of granules which can
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be obtained mainly from maize, potatoes, corn, and rice. The properties of these starch granules
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vary from plant to plant, but are generally composed of , amylose (in most cases about 20% of the
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granule), and amylopectin. Amylose that builds up to 1535% of the granules in most plants, is a
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branched molecule, with (14) linked D-glucose backbones and exhibits about 5% of (16)-
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linked branches, which have a profound effect on the physical and biological properties. Amylose is
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semi crystalline and soluble in hot water while amylopectin is insoluble in hot water. During its
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biodegradation, starch undergo enzyme-catalysed acetal hydrolysis where the - 1,4 link in
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The focus of this work is to process nanocomposite materials consisting of natural rubber filled with
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potato starch nanocrystals which is completely biodegradable and thereby replacing the
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conventionally used .carbon black (manufactured by burning oil or natural gas in controlled
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conditions).
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reinforcing agents to replace carbon black in rubber compounds. Recently, Novamont (Novara,
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Italy), working in partnership with Goodyear Tire and Rubber, has developed tires using
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nanoparticles derived from corn starch, partially replacing the conventional carbon black and silica
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used in making tires. This patented innovation, called Biotred, not only presents environmental
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advantages but also reduces the rolling resistance of tires [16]. Many attempts have been reported to
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blend polysaccharide nanocrystals with polymeric matrices [17-20]. The resulting nanocomposite
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materials display outstanding mechanical properties and thermal stability. For example, starch
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nanocrystals consist of crystalline nanoplatelets about 68 nm thick with a length of 2040 nm and a
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width of 1530 nm [20]. They have been used as a new kind of fillers, showing interesting
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nanocrystals constitute another possible filler for natural rubber which can have an admirable
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Starch nanocrystals, the nanoscale biofiller derived from native starch granules, have been
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nanocrystals, special platelet-like morphology, strong interfacial interactions, and the percolation
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In the past decades, research works were focused on the development of other
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In the present work, a new nanocomposite based on natural rubber filled with potato starch
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nanocrystals was prepared. The nanocrystals were characterized by TEM and XRD. By varying the
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weight percentage of starch nanocrystals in the NR matrix the surface morphology, swelling
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behavior, and crystallinity of the various composites were investigated. The mechanical properties
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2. Experimental
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2.1 Materials
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Natural rubber latex was kindly supplied by Rubber Research Institute of India (RRI, Kottayam,
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India). It contained spherical particles of natural rubber with an average diameter around 1 m, and
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the dry rubber content determined was about 60 wt %. The density of dry NR, was 1.4g cm-3, and it
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contained ~98% of cis-1,4-polyisoprene. Potato starch powder was purchased from Luba chemicals,
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Mumbai.
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microorganisms) etc needed for the preparation of starch nanocrystals were obtained from local
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sources.
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Potato starch nanocrystals were prepared by sulfuric acid hydrolysis of native potato starch powder.
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About 36g of potato starch granules were mixed with 250 ml of 36N H2SO4 for 5 days at 40oC, with
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a stirring speed of 100 rpm. The aqueous suspension was washed by successive centrifugation with
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distilled water until neutrality (confirmed by litmus paper testing). At this stage, starch suspension
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can be believed to be broken into nanocrystals, which changes the refractive index of the solution
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which is evident from the opaque nature of the suspension. The dispersion was completed by a
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Other chemicals like 36N H2SO4, BaCl2, sodium azoture (protectant against
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further 10 min ultrasonic treatment in a B12 Branson sonifier. The resultant aqueous suspension
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constituted of starch fragments with a homogenous distribution in size. The solid fraction of this
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The aqueous suspension of potato starch nanocrystal and the NR latex were mixed in various
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proportions at ambient temperature using a mechanical stirrer (IKA-RW 28). The mixing was
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carried out for 15 minutes to ensure uniform dispersion. Then the mixture was kept for 1 hour in
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order to ensure homogenization and also for the sedimentation of impurities. The mixture was
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stored under vacuum and stirred on a rotavapor for 10 minutes in order to degass the mixture and to
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avoid the formation of irreversible bubbles during water evaporation. The films with uniform
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thickness were obtained by casting on a glass mold and was evaporated at 40oC in a ventilated oven
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for 4-6 hours and then heated at 60oC under vacuum for 2 hrs. The resulting films were conditioned
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at room temperature in desiccators containing P2O5 Fig. 1 shows the flow chart of the preparation
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method adopted.
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InsertFig.1.
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The weight fractions of the sample and their compositions are listed in Table .1.
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Insert Table 1
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3. Characterization Techniques
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The morphology of the nanocrystals was investigated by means of TEM (JEM-2100HRTEM). The
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micrographs were obtained in point to point resolution 0.194 nm, operating at an accelerating
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voltage of 200 kV. The suspension was placed on a 300 mesh Cu grid (35 mm diameter).
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Morphology of the composites was studied using field emission scanning electron microscopy. A
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FESEM, CARC-ZEISS, SUPRA40 UP was used to observe the morphology of starch nanocrystal
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and different starch nanocomposite. The films were sputter coated with platinum to ensure
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X-ray diffraction patterns were taken by using Ni- filtered Cu-K radiation (=0.154 nm) by Bruker
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D8 Advanced X-Ray Diffractometer. The latex nanocomposite samples were scanned in step mode
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by 1.5% min scan rate in the range of 2< 12. The specimens of 11cm films were used for the
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analysis.
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Tensile tests: The non linear mechanical properties of the samples were studied using Universal
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Testing Machine in accordance with ASTM D 412- 2002. Dumbbell shaped specimens 5 mm wide ,
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8 mm long and about 1 mm thick were used for tensile measurements. The tensile curves obtained
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were analyzed for strain at break and modulus. The tests were conducted at a crosshead speed of
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500 mm/ min at ambient temperature. The mechanical properties of nano filled latex composites
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The kinetics of water absorption was determined for all compositions. The specimens were films
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with dimensions around 10100.2 mm3. The films were thin enough to ensure unidirectional
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diffusion. After immersion in water, samples were removed at different times, wiped with filter paper to
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remove surface water and weighed with an analytical balance with 0.1mg resolution. Water induced
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dimensional changes were measured with a micrometer having an accuracy of 0.1mm. The water
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Equation1
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mo and mt are the weights of the sample before and after a time t of immersion, respectively
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Water diffusion coefficient (D) of the nanocomposites was calculated using equation(2)
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Equation2
where, D
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The morphological analysis of starch nanocrystal was done using x-ray diffraction analysis and
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transmission electron microscopy. The XRD pattern displayed two weak peaks at 2 =11.0, double
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peak at 2 =14.16 and 2 =19.5 and a strong peak at 2 =22.19 and 2 =25.88 (Fig.2).From the
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XRD data, it was observed that the diffraction patterns recorded for the lyophilized sample of pure
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potato starch nanocrystal displayed a typical A-type amylose with X-ray diffraction patterns at 2
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with the first peak around 15, the second peak near 18, and the third main reflection around 23.
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A comparative study of the XRD peaks of native starch with prepared starch nanocrystals were also
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conducted. From the diffractograms, both the native potato starch and hydrolysed potato starch
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show the characteristic peak at 18 and 23. But these two peaks are more prominent in the
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diffractogram of potato starch nanocrystal and this indicates the very high extent of crystallinity in
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starch nanocrystals.
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Insert Fig. 2
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The TEM analysis of potato starch nanocrystals lead to the image shown in Fig. 3a. The presence of
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nanocrystal particles is evidenced by the small dark spots (a few spots are encircled to highlight
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them). From the TEM image, the average diameter of the nanocrystals is found to be 3 nm which
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can be confirmed from the particle size analysis (Fig 3b). The samples were found to be free of
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aggregation and impurities as per the TEM observation. Thus the method used to synthesize
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nanocrystals does not create impurities. Nanocrystals of the same of nanometers range (920
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Insert Fig. 3
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The morphology of the NR/starch nanocrystal material were determined from field emission
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The distribution level of the filler within the matrix was evaluated by observing the FESEM image
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of the surface fractured films. Fig. 4a and 4b show the nanocomposite films of NR nanocomposite
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dispersion of starch nanocrystals which appears like white dots can be observed.
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distribution of the nanocrystal in the matrix is clearly seen for the compositions. Such an even and
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A uniform
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uniform distribution of the filler in the matrix is essential for obtaining optimum properties. As the
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filler loading is increased the nanocrystals show a tendency to agglomerate which can be observed in
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Fig. 4(b) image. The particle size of the nanocrystal was observed to be in the range 12nm and it is
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Insert Fig.4
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The
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diffractograms of unfilled natural rubber and pure potato starch nanocrystal films have also been
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shown for comparison. The diffraction pattern recorded for a film of pure potato starch nanocrystals
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obtained by pressing freeze-dried nanocrystals displays typical peaks of A-type amylose allomorph.
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It is characterized by two weak peaks at 2 = 10.1 and, a strong peak at 18.2, and a strong peak at
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23.5. The natural rubber film (NR100) displays a typical behavior of a fully amorphous polymer. It
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is characterized by a broad hump located around 2 = 18.By adding starch nanocrystals, the
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peaks corresponding to A-type amylose allomorph become stronger and stronger. This shows that
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an increase of the starch content results in an increase of the global crystallinity of the composite
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material. Furthermore, X-ray analysis confirmed that the processing by casting and evaporation at
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The starch nanocrystal obtained from sulfuric acid hydrolysis was very promising reinforcing
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material for polymer nanocomposites because of their high stiffness and strength Studies on the
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reinforcing effect of starch nanocrystals with other fillers like clays, organoclays, carbon black, fly
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ash, and chitin whiskers in natural rubber matrix reports that starch nanocrystal is a good substitute
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for carbon black, as it can induce a reinforcing effect in terms of stiffness, strength and elastic
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behavior. These nanocomposites from renewable resources have the added advantages such as, low
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cost, easy availability, good biocompatibility, and ease of modification chemically and
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mechanically.
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The tensile behavior of the potato starch nanocrystal reinforced with NR latex nanocomposite
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films was analyzed at room temperature. Figure 6 shows the stress-strain curves of starch- natural
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rubber composite with increasing starch content. It is found that stress increases regularly with
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strain till the sample breaks. As the filler loading is increased the tensile strength as well the
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modulus increases remarkably. The sharp increase in the tensile strength of the NR nanocomposites
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with addition of the filler shows the reinforcing effect of starch nanocrystal.
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InsertFig.6.
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The elongation at break of the nanocomposites was found to be decreased from a value
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of 1351 for the neat rubber to 536 when 20wt% of the starch nanocrystals were added. Tensile
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modulus of the nanocomposites also was improved significantly with filler loading. In Fig. 7,
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the tensile modulus of the NR/ potato starch nanocrystal composites is plotted as a function of
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starch content. From the graph it is clear that tensile modulus also increases in almost linear fashion.
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Insert Fig 7
The reinforcing effect of the starch nanocrystals strongly depended on their ability to form a
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rigid three-dimensional network, resulting in strong interactions such as hydrogen bonds between the
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filler. Tensile test experiments give clear evidence for the presence of a three-dimensional network
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within the nanocomposites samples. In higher concentration, there is more number of possible
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polymerfiller interactions which enhances the reinforcement. The schematic representation given
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in Fig. 8 shows the possible presence of a three-dimensional network within the nanocomposites.
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Even though an agglomerated morphology was observed at 10wt% nanocrystal loading the property
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of the nanocomposites were not affected adversely. Thus, a modification of dispersion method used
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can possibly give a better dispersion that can result in a further improvement of properties and will
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The swelling behavior of the composite samples after immersion in distilled water were plotted as a
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function of time. Swelling studies of samples with a filler loading from 5 to 20 wt % were carried out.
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The diffusion of water molecules was found to be strongly influenced by the microstructure of the
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nanocomposites and a clear trend is observed with respect to the starch content.
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For all the compositions the water uptake increases tremendously at its first zone (below
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20 hrs) and then reaches a maximum. After reaching the maximum point, there is a
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decrease for the next 5 hours. On further soaking there is a slight decrease with respect to
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time and reaches at equilibrium. The diminution of water uptake may be due to the partial
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release or leaching of starch nano particles in water. The further increase in water uptake with time
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may be due to the migration of starch nanocrystals towards the aqueous phase during
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swelling. During the exposure of this starch nanocrystals to water, starch domains
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gets swollen, and the interface between filler and NR matrix weakens which can create
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free volumes and thereby inducing an increase in swelling rate by the phenomenon
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known as overshooting effect. This has already been reported for polystyrene-co-butyl acrylate
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InsertFig.9
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Diffusion coefficient (D) of NR composites calculated using equation (2) is given in table 2. It was
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observed that the water diffusion coefficient (D) increases continually as the wt % of starch
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nanocrystals is increased. It may be due to the formation of a continuous polar network of starch
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nanocrystal within the NR matrix which seems to favor the swelling of the films by water. The
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increase in the water diffusion coefficient can be explained as, due to the pathways created by the
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networks and also due to hydrogen bonding. Increased starch content results in more absorption of
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water.
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nanocrystals within the NR matrix is due to the interaction between the starch
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Insert Table 2.
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From the water swelling behavior given in Fig.9 it can be observed that the unfilled NR matrix
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displays the lowest swelling and on addition of nanocrystals induces an increase in water diffusivity.
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Diffusion coefficient increases roughly and linearly. This can be explained based on the formation
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of a continuous polar network of starch nanocrystals within the NR matrix. The network seems to
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favor the swelling by water. The polar network of starch nanocrystals within the NR matrix due to
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the interaction between the starch nanocrystals and polymeric chains is represented (Fig.8). The
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Conclusion
Potato starch nanocrystals appeared to be an effective reinforcing agent for natural rubber.
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Starch nanocrystals were obtained after sulfuric acid hydrolysis of potato starch granules (filler).
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TEM observations confirmed that the crystals extracted from potato starch granules via acid
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hydrolysis are in the nanometer dimensions. Nanocomposite material were obtained by casting and
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evaporating a mixture of NR latex and aqueous suspension of potato starch nanocrystal. Four
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different compositions were prepared with different wt % of filler for the matrix.
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dispersion of the filler into the polymer matrix is one of the key parameters for obtaining excellent
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mechanical properties. Wide-angle X-ray analysis showed that the processing by casting and
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evaporation at 40C did not affect the crystallinity of starch nanocrystal. The diffractograms revealed
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that, by adding starch nanocrystals into NR resulted in an increase of the global crystallinity of the
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composite material. The mechanical properties of the prepared composite materials were studied
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through tensile testing. The reinforcing effect of the prepared nanocrystals thus appears to be an
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excellent nanofiller for NR latex and have the potential for replacing conventional polymer
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composite and nanocomposite which are a real threat to the environment. The overall improvement
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References
FESEM
The homogenous
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cold acid hydrolysis and ultrasonication . Carbohydrate Polymers :98 (2013) 295 301
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9. H.-Y. Kim, J.A Hanb, D.K Kweonc, J.D Parkd, S.T Lima, .Effect of ultrasonic treatments on
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11. Y. Lu, L. Weng, L. Zhang. Morphology and properties of soy protein isolate thermoplastics
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14. P. J. Jenkins, A.M. Donald, The effect of acid hydrolyis on native starch granule structure,
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13. W. Thielemans, M. N. Belgacem, and A. Dufresne, Starch nanocrystals with large chain
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15. T. Materne, F. Corvasce, and P. Leitz, European patent no. EP0995775A1, 2000
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(2005) 37833792.
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doi:10.1155/2011/573687
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25. A. Dufresne . Natural rubber green nanocomposites. In: Ranimol S, Thomas S, editors.
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cr
Sample
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Table 1
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Table(s)
(dry wt%)*
100
95
NR90
NR100
Starch
content
(dry wt%)
90
10
NR85
85
15
80
20
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NR 80
NR95
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*Dryrubbercontentof100mgNRlatexfoundtobe60gm.
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NR95
1.65
NR90
1.42
NR85
us
0.08
0.40
1.31
0.95
0.56
1.38
1.01
1.12
0.61
1.48
3.24
1.81
0.63
1.50
3.97
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1.23
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NR80
0..38
1.35
NRfilm
Weightof
Diffusion
sampleat
coefficient
infinity(M)
(D)(cm2s1)
(gm)
an
Nanocomposites Thicknessof
Angleof
Samples sample (h)
linear ()
(vol%)
(mm)
cr
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Figure(s)
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starch nanocrystal
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60
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2 Theta
potato starch
Figure 2.X-ray diffraction patterns of starch nanocrystals and potato starch powder
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Figure 3.a)TEM micrograph of starch suspension b) Particle size distribution of (~50 counts)
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Figure 7. (a) Tensile strength, (b), tensile modulus and (c) elongation at break,for starch
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nanocrystals/NRnanocomposite
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Figure9.WateruptakeofNR/starchnanocrystalcomposites
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