Some of the common conducting polymers and their conductivity [29].
\\n\\n
Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\\n\\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
Note: Edited in March 2021
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'IntechOpen is proud to announce that 191 of our authors have made the Clarivate™ Highly Cited Researchers List for 2020, ranking them among the top 1% most-cited.
\n\nThroughout the years, the list has named a total of 261 IntechOpen authors as Highly Cited. Of those researchers, 69 have been featured on the list multiple times.
\n\n\n\nReleased this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\n\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
Note: Edited in March 2021
\n'}],latestNews:[{slug:"intechopen-signs-new-contract-with-cepiec-china-for-distribution-of-open-access-books-20210319",title:"IntechOpen Signs New Contract with CEPIEC, China for Distribution of Open Access Books"},{slug:"150-million-downloads-and-counting-20210316",title:"150 Million Downloads and Counting"},{slug:"intechopen-secures-indefinite-content-preservation-with-clockss-20210309",title:"IntechOpen Secures Indefinite Content Preservation with CLOCKSS"},{slug:"intechopen-expands-to-all-global-amazon-channels-with-full-catalog-of-books-20210308",title:"IntechOpen Expands to All Global Amazon Channels with Full Catalog of Books"},{slug:"stanford-university-identifies-top-2-scientists-over-1-000-are-intechopen-authors-and-editors-20210122",title:"Stanford University Identifies Top 2% Scientists, Over 1,000 are IntechOpen Authors and Editors"},{slug:"intechopen-authors-included-in-the-highly-cited-researchers-list-for-2020-20210121",title:"IntechOpen Authors Included in the Highly Cited Researchers List for 2020"},{slug:"intechopen-maintains-position-as-the-world-s-largest-oa-book-publisher-20201218",title:"IntechOpen Maintains Position as the World’s Largest OA Book Publisher"},{slug:"all-intechopen-books-available-on-perlego-20201215",title:"All IntechOpen Books Available on Perlego"}]},book:{item:{type:"book",id:"525",leadTitle:null,fullTitle:"Optoelectronics - Devices and Applications",title:"Optoelectronics",subtitle:"Devices and Applications",reviewType:"peer-reviewed",abstract:"Optoelectronics - Devices and Applications is the second part of an edited anthology on the multifaced areas of optoelectronics by a selected group of authors including promising novices to experts in the field. 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Much work has focused on the construction of nanocomposites due to the structural enhancements in physico-chemical properties, and functionality for any given system [1-6]. The physico-chemical enhancements result from the interaction between the elements being near the molecular scale. Nanocomposite materials have also received interest for tissue engineering scaffolds by being able to replicate the extracellular matrix found
However, the major obstacle concerning the electrically conducting polymers has been the difficulty associated with the processing of them [11]. To overcome this problem, most researchers have electrospun conducting polymers by blending them with other spinnable polymers, compromising the conductivity of the nanocomposite fibres [12-16]. Blending of conducting polymers with other polymers positively affects the properties of the resultant nanocomposite fibres. In addition, sometimes for making benefid from condicting polymers and the specific properties of them we can have just a small thib coating of the polymer on the surface of nanocomposite.
\n\t\t\tThe term of “Tissue Inducible Biomaterials” has been recently applied based on the principles of biology and engineering to design nanocomposite scaffolds that restore, maintain or improve the general function of damaged tissues. To gain tissue induction activity and assist tissue regeneration, the nanocomposite scaffolds need to be designed based on nanostructural properties, surface modifications or incorporation of molecules into them. Among different approaches and materials for the preparation of scaffolds, get benefit from conducting polymers seems to be more interesting and promising. Electroconductive polymers exhibit excellent electrical properties and have been explored in the past few decades for a number of applications. In particular, due to the ease of synthesis, cytocompatibility, and good conductivity, some kind of conducting polymers have been extensively studied for biological and medical applications. Different forms of conducting polymers such as polypyrrole (PPy), polythiophene (PT), polyaniline (PANI), poly(3,4-ethylenedioxythiophene) (PEDOT) etc. are used in our daily life due to their uniqe properties which can be applied in different applications. These materials have a conjugated π electron system with “metal-like” electrical conductivity. Due to the rich chemistry of conducting polymers, they have attracted the attention of many researchers and leading to the publication of thousands of papers. The most important property of conducting polymers is their electrical conductivity, so the first approach is to study their electrical-related biological behaviors. Neurons are well known for the membrane-potential-wave style signal transduction. Hence, early studies were focused on the electrical stimulation to the neuron cells using conducting polymers as electrodes. The results showed that the electric conducting polymers can be used as biological electrodes and the neuron growth can be enhanced under an electrical field.
\n\t\t\tUsing conducting polymers in nanocomposite scaffold design is relatively new in tissue engineering applications [17]. It has been demonstrated that these conducting nanocomposites are able to accept and modulate the growth of different cell types [18] including endothelial cells, [19] nerve cells [20] and chromaffin cells [21]. It has been demonstrated that using conducting nanocomposite scaffolds are most promissing in nerve tissue engineering. These electroconductive polymers have been recognized as potential nanocomposite scaffold materials to electrically stimulate tissues for therapeutic purposes in tissue engineering scaffolds. Based on the literature search within the last decade, the present chapter summarized the strategy of electroconductive nanocomposite scaffolds for tissue engineering and regenerative medicine purposes.
\n\t\tConducting polymers are a special class of materials with electronic and ionic conductivity [22]. The structures of the widely used conducting polymers are depicted in Fig. 1 [23]. These polymers have immense applications in the fields of drug delivery, neuroprosthetic devices, cardiovascular applications, bioactuators, biosensors, the food industry and etc.
\n\t\t\t\tOne of the first electrically conducting polymers, polypyrrole (PPy) was introduced in the 1960s, but little was understood about this polymer at that time [24]. In 1977, a research team reported a 10 million-fold increase in the conductivity of polyacetylene doped with iodine as the first inherently conducting polymer [25,26]. Unlike polyacetylene, polyphenylenes, are known to be thermally stable as a result of their aromaticity [27]. Polyheterocycles, such as PPy, polythiophene (PT), polyaniline (PANI), and poly(3,4-ethylenedioxythiophene) (PEDOT), developed in the 1980s, have since emerged as another class of aromatic conducting polymers that exhibit good stabilities, conductivities, and ease of synthesis [28]. Table 1 shows a list of different conducting polymers and their conductivities [29].
\n\t\t\t\tChemical structures of various conducting polymers
Conducting polymers have an inherently unstable backbone, resulting from the formation of alternate single and double bonds along with the monomer units during polymerization. The delocalized π bonding electrons, produced across the conjugated backbone, provide an electrical pathway for mobile charge carriers which are introduced through doping. Consequently, the electronic properties, as well as many other physicochemical properties, are determined by the structure of the polymer backbone and the nature and the concentration of the dopant ion [30].
\n\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Polyacetlene (PA) | \n\t\t\t\t\t\t\t200-1000 | \n\t\t\t\t\t\t\tn,p \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Polyparaphenylene (PPP) | \n\t\t\t\t\t\t\t500 | \n\t\t\t\t\t\t\tn,p | \n\t\t\t\t\t\t
Polyparaphenylene sulfide (PPS) | \n\t\t\t\t\t\t\t3-300 | \n\t\t\t\t\t\t\tp | \n\t\t\t\t\t\t
Polyparavinylene (PPv) | \n\t\t\t\t\t\t\t1-1000 | \n\t\t\t\t\t\t\tp | \n\t\t\t\t\t\t
Polypyrrole (PPy) | \n\t\t\t\t\t\t\t40-200 | \n\t\t\t\t\t\t\tp \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Polythiophene (PT) | \n\t\t\t\t\t\t\t10-100 | \n\t\t\t\t\t\t\tp \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Polyisothionaphthene (PITN) | \n\t\t\t\t\t\t\t1-50 | \n\t\t\t\t\t\t\tp | \n\t\t\t\t\t\t
Polyaniline (PANI) | \n\t\t\t\t\t\t\t5 | \n\t\t\t\t\t\t\tn,p \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Some of the common conducting polymers and their conductivity [29].
Typical monomer structures used to fabricate Poly(3,4-ethylene dioxythiophene), Poly(hydroxymethyl- 3,4-ethylenedioxythiophene) and Poly(3-alklythiophene) [
Conjugated aliphatics, including polyacetylene, and benzene derivatives such as PANI, have been largely ruled out for biomedical applications due to their oxidative degradation in air and the cytotoxic nature of their by-products. Although recent research has shown that the emeraldine salt of PANI (EPANI) can be successfully fabricated in a biocompatible form [31,32], modern biomedical conducting polymers are typically composed of heterocyclic aromatics, such as derivatives of thiophene and pyrrole [33,34]. Specifically, PEDOT and PPy have been widely studied for their superior environmental and electrochemical stability [35-37]. Fig. 2 shows the chemical structure of various thiophene derivatives including EDOT, EDOT-MeOH and 3-alkylthiophene [30].
\n\t\t\tFor biomedical approaches, sometimes we need to modify the outer surface of the materials to induce special features. Conducting polymers can be also modified to enhance the functionality of nanocomposites. The surface modifications of conducting polymers have some concerns including:
\n\t\t\t\tEnhancement of the charge transport of carriers between the implant and tissue
Mediating the large difference in mechanical modulus
Improvement of biodegradation
Decreasing the impedance to enhance the sensitivity of the recording site
Cell response enhancement
Bioactivity enhancement
Surface modification and functionalization of conducting polymers with different biomolecules or dopants has allowed us to modify them with biological sensing elements, and to turn on and off different signalling pathways required for cellular processes. In this way, conducting polymers can show significant enhancement in cell proliferation and differentiation. Thus, conducting polymers provides an excellent opportunity for fabrication of highly selective, biocompatible, specific and stable nanocomposite scaffolds for tissue engineering of different organs [39,40].
\n\t\t\tA range of applications for conducting polymers are currently being considered, such as the development of tissue-engineered organs [41], controlled drug release [42], repaire of nerve chanels [43], and the stimulation of nerve regeneration [44]. In addition, electrically active tissues (such as brain, heart and skeletal muscle) provide opportunities to couple electronic devices and computers with human or animal tissues to create therapeutic body–machine interfaces [45]. The conducting and semiconducting properties of this class of polymers make them important for a wide range of applications. The important properties of various conducting polymers and their potential applications are discussed in Table 2 [23].
\n\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tHighly conductive Opaque Brittle Amorphous structure \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tbiosensors drug delivery bioactuators Nerve tissue engineering Cardiac tissue engineering Bone tissue engineering | \n\t\t\t\t\t\t
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tGood electrical conductivity Good optical property | \n\t\t\t\t\t\t\tBiosensors Food industry | \n\t\t\t\t\t\t
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tA semiflexible rod polymer Requires simple doping/dedoping chemistry Exists as bulk films or dispersions High conductivity up to 100 S/cm \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tBiosensors Drug delivery Bioactuators Nerve tissue engineering Cardiac tissue engineering \n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tHigh temperature stability Transparent conductor Moderate band gap Low redoxpotential conductivity up to 210 S/cm | \n\t\t\t\t\t\t\tBiosensors Antioxidants Drug delivery neural prosthetics | \n\t\t\t\t\t\t
Properties and applications of some common conducting polymer [23]
Generally, polymers with loosely held electrons in their backbones can be called conducting polymers. Each atom on the backbone has connection with a
One of the most important challenges of nanocomposite scaffolds based on conducting polymers is their inherent inability to degrade in the body, which may induce chronic inflammation [49]. Hence, belending of conducting polymers with biodegradable polymers seems to solve the problem. PPy and PANI are the most importan conducting polymers for tissue engineering, and they are important in terms of their biocompatibility and cell signaling especially for nerve tissue engineering [24].
\n\t\t\tPPy is among one of the first conducting polymers that studied a lot for its effect on the behaviour of cells. This material has been reported to support cell adhesion and growth of different cells [50]. This conducting synthetic polymer has numerous applications in tissue engineering and drug delivery. Recently, Moroder
Fluorescence microscopy of PC12 cells at 10× and 40× magnification after undergoing different electrical stimuli treatment regimens for 48h
PANI is an oxidative polymeric product of aniline under acidic conditions and is commonly known as aniline black [52]. The exploration of PANI for tissue-engineering applications has progressed more slowly than the development of PPy for similar applications. However, recently there has been more evidence of the ability of PANI and PANI variants to support cell growth [53]. Recently, Fryczkowski
Although PPy and PANI have been the most extensively conductive polymers for tissue engineering and regenerative medicine, recently the potential of polythiophene conductive polymer for tissue engineering have been approved. This polymer has received significant attention due to a wide range of promising electronic and electrochemical applications [55,56]. PEDOT can be considered as the most successful polythiophene due to its specific characteristics [57-65]. PEDOT can also be considered as the most stable conducting polymer currently available because of not only high conductivity but also unusual environmental and electrochemical stabilities in the oxidized state [57-60]. Recently, Bolin
Recent studies on the application of conductive materials showed that piezoelectric polymeric materials can also be considered for tissue engineering applications. Piezoelectric polymeric materials can generate surface charges by even small mechanical deformations [67]. Poly(vinylidenefluoride) (PVDF) is a synthetic, semicrystalline polymer with piezoelectric properties that can be potentially used for biomedical application due to their unique molecular structure [107]. An electrical charged porous nanocomposite could be a promising approach for a number of tissue engineering applications. Reported data on piezoelectric polymeric nanocomposites showed that after electrical stimulation, cellular interaction and tissue growth might be improved [68].
\n\t\t\t\tConfocal micrograph top view
Conductive polymers exhibit attractive properties such as ease of synthesis and processing [69]. The unique properties of this type of materials have recently given a wide range of applications in the biological field. Research on conductive polymers for biomedical applications expanded extrimly in the 1980s, and they were shown via electrical stimulation, to modulate cellular activities (e.g. cell adhesion, migration, DNA synthesis and protein secretion) [70-73]. Since then many studies have been done on nerve, bone, muscle, and cardiac cells. The unique characteristics of conducting polymers have been shown to be useful in many biomedical applications, specially tissue engineering nanocomposite scaffolds and drug delivery devices [74]. In comparison to other conductive materials for biological applications, conducting polymers are inexpensive, easy to synthesize, and versatile. In addition, conducting polymers permit control over the level and duration of electrical stimulation for tissue engineering applications.
\n\t\t\ta) dexamethasone-loaded electrospun PLGA, (b) hydrolytic degradation of PLGA fibres leading to release of the drug and (c) and (d) electrochemical deposition of PEDOT around the dexamethasone-loaded PLGA fibre slows down the release of dexamethasone. (e) PEDOT nanotubes in a neutral electrical condition. (f) External electrical stimulation controls the release of dexamethasone from the PEDOT nanotubes. By applying a positive voltage, electrons are injected into the chains and positive charges in the polymer chains are compensated. (g) Cumulative mass release of dexamethasone from: PLGA nanoscale fibres (black squares), PEDOT-coated PLGA nanoscale fibres (red circles) without electrical stimulation and PEDOT-coated PLGA nanoscale fibres with electrical stimulation of 1 V applied at the five specific times indicated by the circled data points (blue triangles). (h) UV absorption of dexamethasone-loaded PEDOT nanotubes after 16 h (black), 87 h (red), 160 h (blue) and 730 h (green). [
Developing novel drug-delivery systems will open up new applications that were previously unsuited to traditional delivery systems. The use of conducting polymers in drug delivery is an excellent approach due to their biocompatibility and their possibility of using them in
The triple layer device (polypyrrole(ClO4\n\t\t\t\t\t\t\t-)/non-conducting and adherent polymer/polypyrrole(ClO4\n\t\t\t\t\t\t\t-)) and its macroscopic movement produced as a consequence of volume change in the polypyrrole films. (a) A current flows and the left polypyrrole film acting as the anode is swelled by the entry of the hydrated counter ions (ClO4\n\t\t\t\t\t\t\t-). Simultaneously, the right film acting as the cathode contracts and shrinks because of the expulsion of the counter ions. These volume changes and the constant length of the non-conducting film promote the movement of the triple layer towards the polypyrrole film that is being contracted. (b) By changing the direction of the current, the movement takes place in the opposite direction. The muscle works in LiClO4 aqueous solution [
Bioactuators are devices that are used to create mechanical force, which in turn can be used as artificial muscles. The phenomenon of change in the volume of the conducting polymers scaffold upon electrical stimulation has been employed in the construction of bioactuators. In artificial muscle applications, two layers of conducting polymers are placed in a triple layer arrangement, where the middle layer comprises a non-conductive material [81]. When current is applied across the two conducting polymers films, one of the films is oxidized and the other is reduced. The oxidized film expands owing to the inflow of dopant ions, whereas the reduced film expels the dopant ions and in the process shrinks, as depicted in Fig. 6 [81]. Conducting actuators have many features that make them ideal candidates for artificial muscles, including that they:
\n\t\t\t\tcan be electrically controlled,
have a large strain which is favourable for linear, volumetric or bending actuators,
possess high strength,
require low voltage for actuation (1 V or less),
can be positioned continuously between minimum and maximum values,
work at room/body temperature,
can be readily microfabricated and are light weight, and
can operate in body fluids [82].
The essential properties of conductive polymers desired for tissue engineering and regenerative medicine are conductivity, reversible oxidation, redox stability, biocompatibility, hydrophobicity, three-dimensional geometry and surface topography. Conductive polymers are widely used in tissue engineering due to their ability to subject cells to an electrical stimulation. Studies have addressed cell compatibility when a current or voltage is applied to PPy. An advantage offered by conducting polymers is that the electrochemical synthesis allows direct deposition of a polymer on the surface while simultaneously trapping the protein molecules [84].
\n\t\t\t\tIn a recent study the release of NGF from PPy nanocomposites by using biotin as a co-dopant during the electrical polymerization was investigated [85]. In this research, NGF was biotinylated and immobilized to streptavidin entrapped within PPy nanocomposites doped with both biotin and dodecylbenzenesulfonate. The release of heparin from hydrogels immobilized onto PPy nanocomposites could also be triggered by electrical stimulation [86]. PVA hydrogels were covalently immobilized onto PPy via grafting of aldehyde groups to PPy and chemical reaction of these with hydroxyl groups from the hydrogel as shown in Fig. 7.
\n\t\t\t\tControlled release of heparin from poly(vinyl alcohol) (PVA) hydrogels immobilized on PPy. (A) Post-polymerization of PPy to incorporate aldehyde groups. (B) Covalent immobilization of PVA hydrogels containing heparin on PPy substrates. Controlled release of heparin was obtained by electrical stimulation of PPy [
Electrically conducting polymers have attracted much interest for the construction of nerve guidance channels. The use of conducting polymers can help locally deliver electrical stimulus. It can also provide a physical template for cell growth and tissue repair and allow precise external control over the level and duration of stimulation [87,88]. The importance of conducting polymeric nanocomposites is based on the hypothesis that such composites can be used to host the growth of cells, so that electrical stimulation can be applied directly to the cells through the composite, proved to be beneficial in many regenerative medicine strategies, including neural and cardiac tissue engineering [89].
\n\t\t\t\tRecently, Li
SEM micrographs of gelatin fibers (a) and PANi-gelatin blend fibers with ratios of (b) 15:85; (c) 30:70; (d) 45:55; and (e) 60:40. Original magnifications are 5000× for (a–d) and 20000× for (e). Figure shows the electrospun fibers were homogeneous while 60:40 fibers were electrospun with beads [
To test the usefulness of PANI/gelatin blends as a fibrous matrix for supporting cell growth, H9c2 rat cardiac myoblast cells were cultured on fiber-coated glass cover slips. Cell cultures were evaluated in terms of cell proliferation and morphology. According to Fig. 9, the results indicated that all PANI/gelatin blend fibers supported H9c2 cell attachment and proliferation to a similar degree as the control tissue culture-treated plastic (TCP) and smooth glass substrates.
\n\t\t\t\tMorphology of H9c2 myoblast cells at 20 h of post-seeding on: (a) gelatin fiber; (b) 15:85 PANI/gelatin blend fiber; (c) 30:70 PANI/gelatin blend fiber; (d) 45:55 PANI/gelatin blend fibers; and (e) glass matrices. Staining for nuclei-bisbenzimide and actin cytoskeleton-phalloidin, fibersautofluorescence, original magnification 400× [
Depending on the concentrations of PANI, the cells initially displayed different morphologies on the fibrous substrates, but after 1week all cultures reached confluence of similar densities and morphology. Taken together they suggested that PANI/gelatin blend nanocomposite fibers could provide a novel conductive material well suited as biocompatible scaffolds for tissue engineering.
\n\t\t\tTissue engineering is a new concept which is a growing area of research, in which cells are seeded on nanocomposite scaffolds and then implanted in defected part of body. Appropriate stimuli (chemical, biological, mechanical and electrical) can be applied and over a relatively short time new tissue can be formed to help restore function in the patient. The ideal scaffolds should have an appropriate surface chemistry and microstructures to facilitate cellular attachment, proliferation and differentiation. In addition, the scaffolds should possess adequate mechanical strength and biodegradation rate without any undesirable by-products. Among different materials, conducting polymers are one of the materials that can be employed to facilitate communication with neural system for regenerative purposes. In this chapter the recent methods of the synthesis of nanocomposite scaffolds using different conducting polymers was reviewed. The ability of conductive scaffolds to accept and modulate the growth of a few different cell types including endothelial, nerve, and chromaffin cells have shown a bright future in the field of tissue engineering and regenerative medicine.
\n\t\tThis review chapter book is partially based upon work supported by Air Force Office of Scientific Research (AFOSR) High Temperature Materials program under grant no. FA9550-10-1–0010 and the National Science Foundation (NSF) under grant no. 0933763.
\n\t\tIn recent years, there have been rapid growth predictions for polypropylene-based composites, due to their applications in many fields such as automotive, home appliances, and construction industries [1, 2, 3, 4, 5]. Since the last decade, several nanoparticles have been incorporated into polypropylene and other thermoplastics as reinforcements, to produce stronger and lighter polymer composites [5, 6, 7, 8, 9]. There are many different thermoplastic polymers available on the market today such as polypropylene, polyethylene, etc. Amongst these, polypropylene (PP) is one of the most widely used polymers due to the fact that it is inexpensive and offers attractive properties (rigidity, light weight, thermal and chemical stability, etc.); however, it has the disadvantage of being relatively brittle at room temperature and exhibiting poor resistance to crack propagation. Many investigations have been reported on fracture properties of polypropylene. It has thus been shown that fracture toughness of PP increases with increasing molecular weight and decreasing crystalline percentage. The temperature at brittle-ductile transition of PP has also been reported to increase with increasing crystallinity [10, 11, 12, 13]. Most properties of polymers can be altered through the addition of fillers. Recent polymer nanocomposites have been an area of intense research because of their potential applications as multifunctional and high-performance materials. These nanocomposites are fabricated by simply adding small amounts of nanoparticles in the polymer matrices. The general class of nanocomposite is the mixture of organic and inorganic materials. Significant effort is focused on the ability to obtain control of the nanoscale structures via innovative synthetic approaches. This is a rapid growing area of research and is expanding as it generates many new exciting materials with various properties. These properties of nanocomposite materials depend not only on the properties but also on their morphology and interfacial characteristics. The nanoparticles significantly enhance the mechanical properties, thermal stability, reduced gas permeability, and other physicochemical properties [14, 15, 16, 17, 18, 19] of the neat polymer. To change the properties of these composites, relatively small amounts of the nanoparticle are needed, more often the percentage by weight (0.5–5%) which results from the particles having incredibly high surface to volume ratios.
\nSince the discovery of nanoparticles, researchers are aiming to achieve a uniform particles-polymer interaction rather than the polymer-polymer or particle-particle interaction to obtain the maximum benefit. Wetzel et al. [20] incorporated various amounts of Al2O3 nanoparticles into a polymer matrix and studied the influence of nanoparticles on the flexural strength, impact energy, dynamic mechanical thermal properties, and block-on-ring wear behavior, and their results show the improvement in nanocomposites as compared to the neat polymer. Zheng et al. [21] employed high frequency ultrasonic and mechanical procedures to disperse spherical SiO2 in epoxy resin. The results indicated that with the addition of 3 wt% of SiO2 into the resin, the tensile strength improved by 114%, the stiffness improved by 13%, and the impact strength improved by 56%. Wang’s et al. [22] reported that the dispersion of TiO2 nanoparticles was coated by an acrylic acid (AA)-plasma-polymers in a glycol solution, and results indicated that the dispersion of TiO2 nanoparticles were greatly improved after AA-plasma-polymer coating. They noted that the surface energy played a vital role in the dispersion behaviors of TiO2 nanoparticles. It is an effective way to improve the dispersion of nanoparticles by changing their surface energy by plasma polymer coating. Dai et al. [23] synthesized β-SiC nanorods using the reaction of carbon nanotubes by using a mixture of Si and I2 or through the use of a volatile SiO2. In this study, there was a large quantity of β-SiC nanorods prepared which was wrapped with uniform amorphous SiO2 layers on the outside surface. The formation of β-SiC nanorod was based on the carbothermal reduction of silica xerogels with carbon nanoparticles embedded in the network, and the formation of SiO2 layer was from the reaction of decomposed SiO and O2.
\nExtrusion is one of the most widely used processing techniques for fabrication of thermoplastic polymers. It can be used as a “stand alone” machine to directly shape parts or it can also be used as a melting device that is coupled with other secondary shaping devices. The two main advantages of this process over other manufacturing processes are its ability to create very complex cross-sections and work materials that are brittle, because the material only encounters compressive and shear stresses. It also forms finished parts with an excellent surface finish [24, 25]. Extrusion is also used in the dispersion of nanoparticles to prepare polymer nanocomposites. Mohammed et al. [26] investigated the effect of SiO2 infused into nylon-6 at wt% of 0, 1, and 2, respectively, and extruded into filaments. Experimental results showed that by infusing nanoparticles into nylon −6 and extruding it increased its tensile modulus, yield strength, hardening modulus, and ultimate tensile strength. There was a 45% enhancement in tensile modulus and a 26% enhancement in ultimate tensile strength observed in the 2 wt% system while compared to the neat nylon-6. TGA results indicated more thermal stability found in the nanophased infused systems, while the DSC studies indicated a more moderate increase in Tg. Liu et al. [27] presented the effects of incorporated montmorillonite (MMT) on a surface and the bulk mechanical properties of as-synthesized polyamide-6/montmorillonite (PA6/MMT) composites that were prepared using the twin-screw extruder mixing technique. Russo et al. [28] studied the effect of multiple extrusions on nanostructure and properties of nylon 6 nanocomposites. These researchers produced nanocomposites at different silicate loadings by melt compounding and submitted to further reprocessing by using single and twin screw extruders. Rheological, morphological, and mechanical analyses were carried out on as-produced and reprocessed samples to explore the influence of the number and the type of extrusion cycles on silicate nanodispersion. The results obtained displayed that the reprocessing by single screw extruder can modify the initial morphology since the re-agglomeration of the silicate layers can occur. However, a better nanodispersion was observed in the hybrids reprocessed by twin screw extruder, which was a result of the additional mechanical stresses able to realizing a dispersive mixing that contributes to avoid re-agglomeration phenomena. The high shear stresses produced with twin screw geometry determined also a significant degradation of neat matrix, principally based on chain scission mechanism. All as-produced and reprocessed hybrids showed a substantial enhancement in tensile modulus with the adding of silicate. However, the entity of performance enhancements displayed by the reprocessed hybrids was found to be highly dependent on the degradation of both organoclay and polymer matrix as well as the silicate amount, the number, and the type reprocessing. Investigations were made by Yong et al. [29] on the effects of the coating amount of surfactant and the particle concentration on the impact strength of polypropylene (PP)/CaCO3 nanocomposites. These nanocomposites prepared with monolayer-coated CaCO3 nanoparticles had the best mechanical properties, including Young’s modulus, tensile yield stress, and impact strength because of the good dispersion of the nanoparticles in the polymer matrix, which in turn allowed them to study the effects of particle concentration on the impact strength of the nanocomposites. H-PP and E-PP, which were the low and high molecular weight PPs, respectively, were used as polymer matrices. Critical particle concentrations of 10 and 25 wt% corresponding to an abrupt increase in the impact toughness were determined for the E-PP and H-PP nanocomposites, respectively. Manolis et al. [30] observed a series of experiments which were performed on both simply supported and on-grade circular slab specimens, reinforced with different volumes of fibrillated polypropylene fibers in order to gauge its influence on the slab’s impact resistance and natural frequency. Literature survey clearly suggests that there have been studies on polymer systems infused with nanofillers, but there are no reports on combination of silicon carbide, silicon dioxide coatings infused into polypropylene. Herein, this study we report the effects of reinforcement of silicon dioxide coated silicon carbide nanoparticles in polypropylene thermal and mechanical properties.
\nThe nanoparticles used in these experiments were spherical silicon carbide, ~30 nm in diameter. The β-silicon carbide nanoparticles were purchased from MTI Corporation, Richmond CA, USA. These nanoparticles were then coated with four different types of silicon dioxide nanoparticles, colloidal (Nissan chemicals), 80 nm, and areosil (Degussa), and needle shaped SiO2 nanoparticles (Nissan chemicals). The colloidal silica solution MP-1040 was procured from Nissan Chemical Corporation. This filler is composed of 40% nanoparticles that are spherical in shape and approximately 200 nm in diameter dispersed in 60% of water. The 80 nm silica was procured from MTI Corporation Richmond CA, USA. These particles are spherical in shape having an 80 nm diameter. Areosil silica is also spherical in shape with a smaller diameter of approximately 5–15 nm and was also procured from Degussa. The other silica used was the needle shaped silica solution MP-1040 which was procured from Nissan Chemical Corporation. This filler is also composed of 40% nanoparticles and 60% water; however, these nanoparticles are irregular in shape.
\nThe matrix material used in this experiment is polypropylene procured from Chem Point. The polymer molecular weight ranged from 40,000 to 100,000, its powder diameter is approximately 20 μm, and the density of polypropylene is between 0.910 and 0.928 gr/ml. The melting point of polypropylene is 160°C with >50 isotactic crystalline structure. This type of high melting polymer can be molded or machined into structural components [31].
\nIn the first step, 250 mg of β-SiC was weighed and mixed along with 500 mg of powdered SiO2, 250 mg of pluronic F-127 and 60 ml of ethylene glycol. The reaction mixture was irradiated using high intensity ultrasound for 3 hours at 5°C under argon gas flow. This process was done for each of the two powdered types of SiO2; however for the solution types, when added to SiC nanoparticles, it was done using a weight ratio of 10:1. Upon completion of the sonication process, the silicon carbide coated silica nanoparticles were collected using a centrifuge at 12,000 rpm at 5°C for 30 min. The coated particles were washed 5 times, the first four times using distilled water and the last time with ethanol. The final step was to allow the sample to dry under vacuum for 24 hours at room temperature. Once dried, the coated nanoparticles were added to polypropylene at a ratio of 1:10 and then mixed using a Thinky mixer. The materials were placed in a special container and mixed under vacuum at 1200 rpm for 10 min. This step was done three times to ensure proper distribution of particles, before being extruded. This non-contact mixing method [32, 33] proves to be very efficient at dispersing nanofillers in polymer matrices without having any cross-contamination. This non-contact method works by independently revolving and rotating a container at various speeds in a planetary manner. As the container rotates, it experiences a number of forces that results in the material inside of the container being mixed. Centrifugal force presses the material outwards to the inner wall of the container, while other forces cause the material to move in a spiraling downwards direction along the slope of the container wall. The material then moves back to the center of the container and up to the top repeating the process and in turn mixing the sample. As the material circulates from top to bottom, it generates a kneading effect forcing trapped air out of the material.
\nIn the second phase, nanocomposites of polypropylene, silicon carbide/silicon dioxides were then extruded using a Wayne Yellow Label Top single screw extruder. The extruder has a 19 mm diameter screw, which is driven by a 2HP motor complete with a toothed timing belt for smooth speed reversal. Present are five thermostatically controlled heating zones that were used to melt the mixture before extrusion. Three of the zones were located inside the barrel and the final two were in the die zone set at respective temperatures of 340, 344, 350, 354, and 350°F. As the sample material passes through each zone, they are disintegrated into several branches and then combined again, which ensures proper distributive mixing of the nanoparticles and polypropylene. As the dispersed nanoparticles containing liquid polypropylene passes through the 10 cm long steel tube, it arrives to the die plate. As the sample passes through the extruder, it enters and completely fills the die, which in turn forms the flexure sample. The process schematic is shown in Figure 1.
\nFabrication of polypropylene/SiC/SiO2 nanocomposite.
JOEL-2010, High Resolution (Japan), Transmission Electron Microscopy (HRTEM), is used to study the size, shape, and extent of coating of SiC onto SiO2 nanoparticles. The samples were prepared by dispersing the nanoparticles in ethanol and placing a drop of the solution on a copper grid.
\nRigaku D/MAX 2100 X-Ray Diffractometer (Japan) was used to study the structural characteristics. The samples were prepared for XRD by uniformly spreading the nanoparticles on a quartz sample holder. The test samples were conducted from 0 to 80° of two theta at room temperature. Characteristics XRD diffraction patterns were collected and matched with established data from PDF files. X-ray diffraction helps to determine the crystallographic configuration of the coated nanoparticles and its nanocomposites.
\nThis surface analysis technique (2–10 nm analysis depth typically) XPS can identify elemental composition, oxidation state, and chemical bonding like covalent bonds (oxides, nitrides, etc.) by evaluating binding energy shifts. This test was done at Cornell University Dr. Jonathan Shu’s lab. The pressure in the analyzing chamber was typically 1.3 × 107 Pa under operating conditions. Photoelectrons were collected at approximately 45° from the specimen surface normal. The X-rays created photoemission electrons, and the signature of the photoemissions identified each element present in the samples.
\nThermogravimetric analysis was carried out using a Mettler Toledo (USA) TGA apparatus to find out the thermal stability of the test sample. This test is most commonly used to determine polymer decomposition temperatures, residual solvent levels, the amount of moisture content absorbed, and the amount of inorganic filler in polymer or composite material compositions. The samples were prepared by cutting the samples into small pieces, then placing 5 mg of the material in a platinum sample pan, and heating at a constant heating rate of 10°C/min from room temperature to 900°C under nitrogen atmosphere of 40 ml/min. The initial sample weight is measured at room temperature, and as heat is constantly being applied, the machine monitors the change in sample weight as a function of temperature. This result in weight loss versus temperature graphs being plotted from the data is obtained. In this case, the decomposition temperature is considered at 50% weight loss of the material.
\nDifferential scanning calorimetry (DSC) tests were carried out using a Mettler Toledo822e (USA) from 30 to 300°C at a heating rate of 5°C/min under a nitrogen atmosphere then cooled from 300 to 30°C at the same rate. These results were used in measuring the melting temperature and the crystalline temperature.
\nThree-point bending flexural tests were conducted using a Zwick Roell MTS (Germany) to evaluate the samples flexural properties. Ten samples were tested using ASTM D790-03 testing standards which are of nominal size 100 mm (length) × 12.5 mm (width) × 5 mm (thick) and a span/thickness ratio maintained at 16:1. The test were conducted at room temperature at a constant crosshead speed of 2.0 mm/min. Stress-strain plots were obtained as the load displacement data were recorded through the data acquisition system equipped with the Zwick Roell MTS machine.
\nXRD patterns were collected using a diffractometer operating in the Bragg-Brentano geometry utilizing Cu Kα radiation. The X-ray tube was operated at 40 kV and 30 mA. A 2
The SiC coated onto various SiO2 samples were analyzed to investigate the effects of ultrasonic irradiation on the nanoparticles. The XRD spectra of pure SiC can be seen below in Figure 2(a). Through the use of the Jade 6.0 software, the peaks appearing at 2θ of 35.6, 41.5, 60.0, 72.0, and 75.5° indexed as (111), (200), (220), (311), and (222), designates the crystal spherical structured Moissanite-3C SiC (JCPDS 29-1129). The XRD of silicon carbide coating onto silicon dioxide was shown in Figure 2(b)–(e), and it is evident that all of the SiC particles are crystalline in nature and all assigned to β-SiC. The background wide peak pattern is the characteristic of an amorphous SiO2 phase. In the sample, the XRD data indicate the presence of only silicon carbide and amorphous silicon dioxide. The plot has characteristic peak intensities of FWHM, and d-spacing values which can be found in Table 1. A sharp peak around 35.6° corresponds to a spacing of 2.5189 A, which is attributed to the β-SiC (111) diffraction. There was an amorphous background present around 22° which is the result of the silicon dioxide presence. Deduced from the FWHM of β-SiC (111) diffraction peak. It is evident that, compared to pure SiC, the coated SiC FWHM peaks decreased significantly. In this case, the coated nanoparticles FWHM decreased compared to the neat, which results in coating of amorphous silica. The crystallite sizes of the particles were determined using Debye-Scherrer formula and FWHM method from the 100% peak of the pattern.
\nXRD patterns of SiC and coated nanoparticles.
Sample | \n2θ at 100% intensity | \nFWHM(°) | \nFWHM at 35.6° | \n
---|---|---|---|
SiC | \n35.612 | \n0.673 | \n0.673 | \n
Colloidal | \n35.746 | \n0.389 | \n0.612 | \n
Areosil | \n35.813 | \n0.397 | \n0.604 | \n
80 nm | \n35.694 | \n0.343 | \n0.674 | \n
Needle shaped | \n35.865 | \n0.368 | \n0.652 | \n
XRD analysis of SiC and coated SiC, FWHM.
The TEM micrograph in Figure 3 shows (a) as received SiC, (b) SiC coating on colloidal silica, (c) aerosol silica coated on SiC, (d) 80 nm silica coated on SiC, and finally (e) needle shaped silica coated on SiC. Figure 3(a) shows the SiC particles are spherical and particle sizes are about 30–50 nm. Figure 3(b) represents the coating of SiC on colloidal silica where the particles of silica are about 200 nm. The SiC particles are uniformly coated on silica spheres. Figure 3(c) shows that the particles of aerosol silica is coated on SiC nanoparticles. Since the aerosil silica is amorphous and also the particle sizes are about 5 nm, it is seen on the surface of SiC. In TEM Figure 3(d) and (e) shows the SiC particles and it was very hard to see the silica because of the silica is highly transparent to the electronic bean and difficult image.
\nTEM images of (a) SiC, (b) SiC coated SiO2, (c) SiC coated areosil, (d) SiC coated needle SiO2, and (e) SiC coated 80 nm SiO2.
XPS is a surface sensitive spectroscopic tool that provides information about chemical states and concentration of elements present in a sample with the exceptions of H and He. Each characteristic peak corresponds to the electron configuration of the electrons within the atoms, e.g., 1s, 2s, 2p, 3s, etc. This method uses soft X-rays to eject electrons from inner-shell orbital. The kinetic energy, Ek, of these photoelectrons is determined by the energy of the X-ray radiation, hν, and the electron binding energy, Eb, as given by:
\nUsing this technique, the surface of SiC and SiO2 were characterized from the surface to approximately 10 nm in depth. Each element shows a characteristic set of peaks in the photoelectron spectrum at kinetic energies of the elemental composition of the surface region determined by the photon energy and the respective binding energies. Elements exhibit binding energy peaks whose relative position depends on the electronegativity of their surrounding atomic neighbors. In the case of a phase mixture where more than one bonding state exists, a particular element is expected to have various binding energies, caused by different coordination/neighbor. The intensity of the peaks is related to the concentration of the element within the sampled region.
\nAs shown in Figure 4, it displays the XPS spectra of SiC/SiO2 nanomaterials. The most distinctive peaks present are the oxygen, carbon, and silicon peaks, respectively. Using the CasaXPS software for XPS analysis, a detailed spectrum of Si 2p, C 1s and O 1s of the chemical state of each element on the surface of the nanoparticles were identified and analyzed. Analysis of such element regions were done to confirm their attachment to the surface of the silicon dioxides. Silicon (Si 2p), carbon (C 1s), and oxygen (O 1s) elements can be found at binding energies of 102.8, 284.6, and 532.0 electron volts (eV), respectively. Also in Figure 4 above, one can take a look at the as received SiC which clearly shows a Si peak, but also shows where adsorbed contaminations like oxygen and carbon were found on the top layer within about 6 nm in thickness. This observation is consistent with other researchers [34, 35] and can be a result of the absorption of atmospheric oxygen. Figure 5(a) shows the high resolution scan of the deconvoluted XPS spectra of neat SiC for Si 2p peak and C 1s on the sub-surface layer. The spectra were Gaussian fitted based on the published data of the binding energies. The spectra emission line at binding energy (BE) of 100.47 eV is associated with the SiC bonding. In addition to this, two more fitted chemical shifts were observed at BE of 98.4 and 102.9 eV, which were identified as Si° and SiO2, respectively, for the spectra of SiC for Si 2p peak.
\nXPS spectra for neat SiC and coated nanoparticles.
Deconvoluted XPS spectra for SiC for (a) Si 2p peak (b) C 1s peak.
For the spectra of SiC, the C 1s spectrum was deconvoluted into three peaks (Figure 5(b) of BE 285.5, 282.7, and 289.06eV. The peak at 285.5 eV signified the presence of carbon in the form of hydrocarbon, while the peak at 282.7 eV is due to the binding energy of carbon in the form of SiC, and in the form of carbon bonded to oxygen, this was observed at 289.06eV. The binding energy for oxygen or O 1s was found to be 532.6 eV and can be associated either with O2-Si or C-O bonding which can be a result of surface contamination. From the surface chemical composition, it can be seen that the ratio of Si/C was found to be 0.29, which is much lower than the theoretical value for pure SiC of 0.5 which clearly indicates surface contamination.
\nThe coated hybrid nanocomposites of colloidal, areosil, 80 nm, and needle shape nanocomposites were also investigated using XPS for comparison with the neat sample. The chemical composition and binding energies were tabulated and presented in Table 2. The O/Si ratios from the table obviously doubled which indicated that surface contaminant oxygen was increased when SiC was sonicated with the four different types of SiO2. The concentration of C in the near surface decreases from 65.09% for neat SiC to an average of 43.26% for sonicated SiC in SiO2. This decrease is may be removal of carbon in the form of CO2. However, it can be seen here that, the as received SiC absorb oxygen which is enough to impart strong chemical double bonding in the system.
\nSamples | \nComposition (atomic %) at the surface of nanoparticles | \nAtomic ratios of O/Si | \n||
---|---|---|---|---|
\n | Si | \nO | \nC | \n|
As received SiC | \n19.05 | \n15.86 | \n65.09 | \n0.83 | \n
Colloidal | \n20.91 | \n33.64 | \n45.45 | \n1.60 | \n
Areosil 80 nm | \n23.59 19.82 | \n34.51 37.28 | \n41.35 42.90 | \n1.46 1.88 | \n
Needle shaped | \n25.66 | \n30.97 | \n43.37 | \n1.20 | \n
Surface chemical composition of neat SiC and coated nanoparticles.
\nFigures 6–9 depict the deconvoluted XPS spectra for peaks Si 2p, C 1s, and O 1s of the coated samples of colloidal, areosil, needle shaped and 80 nm nanoparticles. For each of the nanoparticles samples made using high intensity ultrasound irradiation, there were noticeable chemical shifts in peak observed indicating the coating of SiC onto SiO2 nanoparticles that took place. This was further confirmed from the elemental concentration at the surface. These spectra could be separated into two or three peaks based on the assumption that each peak consists of the Gaussian/Lorentzian sum function. The Si(2p) peak was separated into the Si▬Si, Si▬C, and SiOx peaks, and the C(1s) peak was decomposed into the C▬Si, C▬C, C▬O▬H, and C═O peaks [34, 35, 36, 37, 38, 39]. The energy positions of these peaks are listed in Table 3. The separation of the elements is not sufficient to precisely obtain the fraction of the bond. Therefore, as a rough estimation, the fraction of the bond was obtained from the ratio of the area of each peak [40]. The FWHM of Si▬Si and Si▬C are 2.13 and 1.38 eV, respectively. The FWHM of C▬C and C═C are 2.1 and 1.2 eV, respectively. The ratio between C▬C and C═C bond concentration is 10.1.
\nBond | \nBinding energy (eV) | \n
---|---|
Si▬Si | \n99.2 | \n
Si▬C | \n100.5 | \n
O▬Si▬C | \n101.8 | \n
SiOx\n | \n103.2 | \n
C▬Si | \n283.2 | \n
C▬C | \n284.6 | \n
C▬O▬H | \n286.4 | \n
C═O | \n288.4 | \n
Binding energy of different bonds.
Deconvoluted XPS spectrum of SiC/SiO2 (colloidal) for Si 2p peak and C 1s.
The deconvoluted XPS spectrum of SiC/SiO2 (Colloidal) for Si 2p peak and C 1s is shown in Figure 5. Similar results were obtained such as, the BE of 103.35, 99.99, and 97.91 eV that were associated with SiOx, Si▬C, and Si▬Si bonding, respectively, for Si 2p. Fitted curve for C 1s also showed similar results of C▬C and C▬Si bonding occurring. The O 1s emission was also found at BE of 532.55 eV. The surface chemical composition of Si, O and C obtained from CasaXPS were 20.91, 33.64 and 45.45, respectively.
\nThe deconvoluted XPS spectrum of SiC/SiO2 (Areosil) for Si 2p peak and C 1s is shown in Figure 7. The BE was found to be 103.48 and 100.089 eV for Si 2p which are associated with SiOx bonding and Si▬C bonding, respectively. Whereas, fitted curve for C 1s at 284.76 and 282.88 eV of BE was indicating the C▬C and C▬Si bonding. The O 1s emission was found at BE of 532.55 eV, and the surface chemical composition of Si, O, and C obtained from CasaXPS were 23.59, 34.51, and 41.35%, respectively. There was evident of small amounts of Na 1s present that accounted for the remaining 0.56% of the chemical composition. This was believed to be the result of surface or apparatus contamination.
\nDeconvoluted XPS spectrum of SiC/SiO2 (Areosil) for (a) Si 2p peak and (b) C 1s.
\nFigure 8 shows the deconvoluted XPS spectrum of SiC/SiO2 (needle shape) for Si 2p peak and C 1s. The BE was found to be associated with Si▬C bonding at 100.61 eV, Si▬Si at 98.35 and 103.74 eV related with Si▬O bonding, respectively, for Si 2p. Fitted curve for C 1s was also obtained at 284.46 and 283.02 eV of BE was indicating the C▬C and the Si▬C bonding. In addition to these, the O 1s emission was also found at BE of 532.55 eV. The surface chemical composition of Si, O, and C obtained from CasaXPS were 25.66, 30.97, and 43.37%, respectively.
\nDeconvoluted XPS spectrum of SiC/SiO2 (needle shape) for (a) Si 2p peak and (b) C 1s.
\nFigure 9 depicts the deconvoluted XPS spectrum of SiC/SiO2 (80 nm) for Si 2p peak and C 1s. The BE was found to be associated with Si▬C bonding at 100.41 and 103.84 eV related with Si▬O bonding, respectively, for Si 2p. On the other hand, fitted curve for C 1s at 284.76 and 282.28 eV of BE was indicating the C▬C and the Si▬C bonding. In addition to these, the O 1s emission was found at BE of 532.55 eV. The surface chemical composition of Si, O, and C obtained from CasaXPS was 19.82, 37.28 and 42.90 respectively.
\nDeconvoluted XPS spectra of SiC/SiO2 (80 nm) for (a) Si 2p and (b) C 1s.
The observed shift in the Si 2p peak between the oxide and the carbide is consistent with the expected change in oxidation state. Additional information on the interface was obtained from the C 1s photoelectron spectrum of the nominally bare SiC, far from the interface as shown in Figure 10. The narrow second highest energy peak is the expected C 1s signal from bulk SiC [41]. From the observed chemical shifts, we can determine the ionic state of a particular species. Although the incident X-rays penetrate deep into the sample, only electrons emitted from a thin surface layer are detected. The electron escape depth for Si, C, and O ranges from 2.0 to 2.5 nm [42].
\nXPS overlay of O 1s binding energy for SiC and the coated nanoparticles.
Differential scanning calolimetry (DSC) is a thermoanalytical technique by which the energy absorbed or emitted by the material as a function of temperature or time is measured. In present case, we have studied the extruded-polymer nanocomposites to determine the thermal transitions such as the melting (Tm) of a crystalline polymer as shown in Figure 11. The DSC data are presented in Table 4.
\nDSC melting curve of neat PP and nanocomposites.
The curve shapes of the neat material and nanocomposites are very similar, with only slight differences in the leading edge of the melt peak, indicating that the neat structure has little effect on the overall phase structure of the material. Above the melting temperature of about 160°C, the polymer is subject to a thermal degradation that is both dependent on time and on temperature. Adding nanoparticles allow the start of the degradation process to shift toward higher temperatures. The increase of the melting temperature of neat PP to PP + SiC was 161.43–166.12°C. Correlation has also been drawn between orientation (crystal perfection) and the DSC melt peak temperature [43].
\nThe crystallization peak temperatures are shown below in Figure 11; they follow the same order as the melt peak temperatures, with the neat pp material being more easily crystallizable. Preliminary isothermal crystallization studies at 116°C of neat polypropylene also show a similar trend. A decrease in the crystallization temperature after introduction of the filler indicates that a higher undercooling of the melt is necessary for the crystallization to occur. Such behavior may be the result of the strong influence of the SiC/SiO2 nanoparticles on the chain dynamics (lower chain mobility). It has been shown that the crystallization rate increases as both molecular weight and molecular weight distribution increase [44].
\nSeveral authors have seen multiple melting peaks in polypropylene, and there is the suggestion of multiple crystalline forms in the polypropylene [33, 44, 45]. It is alternatively suggested that the low temperature melting is caused by a less perfect crystalline order and not from different crystal phases [46]. With very sharp crystallization peaks, it is likely that the low temperature phase is induced at the crystallization temperature. Similar phenomena have been observed for isothermal crystallization [47] and this probably explains the difference in peak temperature between the nanocomposites. It is also plausible that the different polymer fractions do not co-crystallize simultaneously, and that the lower temperature melts is due to morphological effects. It is possible that the higher melt temperature of neat PP implies the molecular weight of the nanocomposites is greater than the neat PP (Table 4).
\nSample | \nMelting temperatures (°C) | \nCrystallization temperatures (°C) | \n
---|---|---|
Pure PP | \n161.43 | \n113.72 | \n
Neat areosil | \n165.48 | \n111.12 | \n
Neat 80 nm | \n163.16 | \n112.83 | \n
Neat needle shape | \n165.60 | \n111.31 | \n
PP + SiC | \n161.51 | \n116.80 | \n
Coated areosil | \n166.12 | \n113.20 | \n
Coated colloidal | \n162.84 | \n113.54 | \n
Coated 80 nm | \n163.70 | \n111.72 | \n
DSC melting and crystallization temperature chart.
The applications of TGA are to determine the absorbed moisture content, residual solvent levels, the amount of inorganic filler in a polymer, and in this case the degradation characteristics of the coated nanocomposites in terms of their induction time. The weight loss of a polymer as a function of temperature is commonly determined by this technique. Weight loss of a polymer due to thermal degradation is an irreversible process. Such thermal degradation is largely related to oxidation whereby the molecular bonds of a polymer are attacked by oxygen molecules. Figure 12 is the TGA graph of extruded neat silicon carbide coating with polypropylene and extruded samples of coated nanoparticles with polypropylene. The TGA data are presented in Table 5.
\nTGA curves of neat and SiC/SiO2 reinforced polypropylene nanocomposite.
Sample | \nTd (°C) | \nT50 (°C) | \n% Temperature increase | \n
---|---|---|---|
Pure PP | \n369.78 | \n436.06 | \n— | \n
Neat areosil | \n452.94 | \n488.59 | \n12.0 | \n
Neat 80 nm | \n469.68 | \n496.34 | \n13.8 | \n
Neat needle shape | \n464.94 | \n493.48 | \n13.1 | \n
PP + SiC | \n453.67 | \n483.60 | \n10.9 | \n
Coated areosil | \n454.06 | \n486.11 | \n11.4 | \n
Coated colloidal | \n446.79 | \n487.50 | \n11.7 | \n
Coated 80 nm | \n447.71 | \n482.39 | \n10.6 | \n
Parameters obtained from TGA curves.
In the present study, TGA results show that 50% of the total weight loss is considered as the structural destabilization point of the system. It is a common practice to consider 50% weight loss as an indicator for structural destabilization. From Figure 12, it is evident that the neat sample is stable up to 436.06 °C, whereas the coated nanocomposites minimum stabilization temperature is at 482.39°C which is a 10.6% increase. The maximum temperature increase was 13.8% and stabilization occurred at 496.34°C for the neat 80 nm sample. The reason for this increase in the thermal stability is due to the increase in cross-linking of the coated nanoparticles in the presence of polypropylene and having minimum particle to particle interaction.
\nThis may be due to the presence of silicon carbide nanoparticles which are high heat absorbing materials compared to neat polypropylene, which can be the reason for having such a positive impact on improving the decomposition temperature. One can also assume that the nanoparticles were well dispersed and were not acting as impurities in agglomerated form due to the increase. Another probable reason for the observed behavior could be the lower mobility of the polymer chains due to strong interaction with the nanofiller. Thermal degradation of polypropylene begins with formation of the free radicals, which further induce chain fragmentation processes [48]. Volatile oligomers that are formed which are responsible for the mass loss will be partially prevented which results in the whole degradation process to shift towards a higher temperature.
\nThe flexure test method measures behavior of materials subjected to simple beam loading. It produces tensile stress in the convex side of the specimen and compression stress in the concave side which creates an area of shear stress along the midline.
\nFlexure stress-strain curves for neat polypropylene and the nanocomposites are shown in Figure 13. The flexural test data are presented in Table 6. From the graph, it is evident that flexural strength and modulus slightly increases with the addition of coated SiC/SiO2 nanofillers with respect to the neat polymer. In the table, we see that coated colloidal contributed the maximum percent change in stiffness at 40.5%, while the coated 80 nm contributed to a maximum strength percent change at 24.6%, and the greatest toughness percent change which was at 92.4%. Although these were the highest values observed, it is still evident that overall, all of the samples performed greater than the neat PP sample.
\nStress-strain curve from flexure results.
The reason for such change in stiffness of the matrix is due to ultrasound irradiation which enhances the homogeneity. The ultrasound irradiation helps in molecular mixing of these components together and the formation of coated reactive particles which ultimately leads to increase the cross-linking in the polymer when mixed. The decrease in mobility of the cross linking in polymer gives better mechanical properties with an optimum amount of nanofiller addition. Surface area also played an important role in the significant increase in that the spherical spatial distribution and low weight ratio of the nanofillers enhance the homogeneity of the reaction. The nanocomposites exhibit ductile fracture and the elongation at break increased with the increase of the nanoparticle content (Table 6).
\nSample | \nStrength (MPa) | \n% Strength change | \nModulus | \n% Modulus change | \nStrain (%) | \n% Increase in toughness | \n
---|---|---|---|---|---|---|
Pure PP | \n33.97 | \n— | \n1.16 | \n— | \n7.09 | \n— | \n
Neat areosil | \n35.82 | \n5.4 | \n1.31 | \n12.9 | \n6.83 | \n13.2 | \n
Neat 80 nm | \n37.50 | \n10.3 | \n1.42 | \n22.4 | \n6.65 | \n22.4 | \n
Neat needle shape | \n39.76 | \n17.0 | \n1.48 | \n27.5 | \n6.61 | \n27.5 | \n
PP + SiC | \n38.88 | \n14.4 | \n1.45 | \n25 | \n6.50 | \n25 | \n
Coated areosil | \n39.26 | \n15.5 | \n1.49 | \n28.4 | \n6.29 | \n30.1 | \n
Coated colloidal | \n41.65 | \n22.6 | \n1.63 | \n40.5 | \n6.48 | \n41.5 | \n
Coated 80 nm | \n42.33 | \n24.6 | \n1.28 | \n10.3 | \n7.29 | \n92.4 | \n
Mechanical properties from flexure test.
The samples were prepared using high intensity ultrasound irradiation to coat SiC onto SiO2 nanoparticles. This process has been introduced as an efficient way to disperse SiC onto SiO2 nanoparticles, and by extruding these samples with polypropylene, it increases its mechanical properties. XRD analysis confirmed that the samples were crystalline with an amorphous background present. The TEM analysis revealed that the SiC nanoparticles were uniformly dispersed over the entire surface of the SiO2 nanoparticles. It also indicated a minor growth in the size of the nanoparticles after ultrasonic irradiation. XPS spectrographs revealed the chemical composites found in the samples. It also verified the surface coating through the shifts in binding energies. The crystallization of the polypropylene polymer matrix was also affected by the presence of the coated nanoparticles. DSC testing indicated that the crystallization and the melting temperatures increased with increasing filler content. Through DSC, it can be seen that by adding nanoparticles, it allows the start of the degradation process to shift toward higher temperatures. The increase of the melting temperature of neat PP to PP + SiC was 161.43–166.12°C. A decrease in the crystallization temperature after introduction of the filler indicates that a higher undercooling of the melt is necessary for the crystallization to occur. The TGA data showed that the neat sample is stable up to 436.06°C, whereas the coated nanocomposites minimum stabilization temperature is at 482.39°C which is a 10.6% increase. The maximum temperature increase was 13.8% and stabilization occurred at 496.34°C for the neat 80 nm sample. The coated nanocomposites had profound effects on the PP properties. The flexure test results showed that the flexural strength and modulus slightly increases with the addition of coated SiC/SiO2 nanofillers with respect to the neat polymer.
\nThe authors acknowledge the financial support of NSF-RISE # 1459007, NSF-CREST#1735971 and NSF-MRI-1531934 grants.
\nThe authors declare no conflict of interest.
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',metaTitle:"Horizon 2020 Compliance",metaDescription:"General requirements for Open Access to Horizon 2020 research project outputs are found within Guidelines on Open Access to Scientific Publication and Research Data in Horizon 2020. The guidelines, in their simplest form, state that if you are a Horizon 2020 recipient, you must ensure open access to your scientific publications by enabling them to be downloaded, printed and read online. Additionally, said publications must be peer reviewed. ",metaKeywords:null,canonicalURL:null,contentRaw:'[{"type":"htmlEditorComponent","content":"Publishing with IntechOpen means that your scientific publications already meet these basic requirements. It also means that through our utilization of open licensing, our publications are also able to be copied, shared, searched, linked, crawled, and mined for text and data, optimizing our authors' compliance as suggested by the European Commission.
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\n\nMetadata for all publications is also automatically deposited in IntechOpen's OAI repository, making them available through the Open Access Infrastructure for Research in Europe's (OpenAIRE) search interface further establishing our compliance.
\n\nIn other words, publishing with IntechOpen guarantees compliance.
\n\nRead more about Open Access in Horizon 2020 here.
\n\nWhich scientific publication to choose?
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I am also a member of the team in charge for the supervision of Ph.D. students in the fields of development of silicon based planar waveguide sensor devices, study of inelastic electron tunnelling in planar tunnelling nanostructures for sensing applications and development of organotellurium(IV) compounds for semiconductor applications. I am a specialist in data analysis techniques and nanosurface structure. I have served as the editor for many books, been a member of the editorial board in science journals, have published many papers and hold many patents.",institutionString:null,institution:{name:"Sheffield Hallam University",country:{name:"United Kingdom"}}},{id:"54525",title:"Prof.",name:"Abdul Latif",middleName:null,surname:"Ahmad",slug:"abdul-latif-ahmad",fullName:"Abdul Latif Ahmad",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"20567",title:"Prof.",name:"Ado",middleName:null,surname:"Jorio",slug:"ado-jorio",fullName:"Ado Jorio",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Universidade Federal de Minas Gerais",country:{name:"Brazil"}}},{id:"47940",title:"Dr.",name:"Alberto",middleName:null,surname:"Mantovani",slug:"alberto-mantovani",fullName:"Alberto Mantovani",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"12392",title:"Mr.",name:"Alex",middleName:null,surname:"Lazinica",slug:"alex-lazinica",fullName:"Alex Lazinica",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/12392/images/7282_n.png",biography:"Alex Lazinica is the founder and CEO of IntechOpen. After obtaining a Master's degree in Mechanical Engineering, he continued his PhD studies in Robotics at the Vienna University of Technology. Here he worked as a robotic researcher with the university's Intelligent Manufacturing Systems Group as well as a guest researcher at various European universities, including the Swiss Federal Institute of Technology Lausanne (EPFL). During this time he published more than 20 scientific papers, gave presentations, served as a reviewer for major robotic journals and conferences and most importantly he co-founded and built the International Journal of Advanced Robotic Systems- world's first Open Access journal in the field of robotics. Starting this journal was a pivotal point in his career, since it was a pathway to founding IntechOpen - Open Access publisher focused on addressing academic researchers needs. Alex is a personification of IntechOpen key values being trusted, open and entrepreneurial. Today his focus is on defining the growth and development strategy for the company.",institutionString:null,institution:{name:"TU Wien",country:{name:"Austria"}}},{id:"19816",title:"Prof.",name:"Alexander",middleName:null,surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/19816/images/1607_n.jpg",biography:"Alexander I. Kokorin: born: 1947, Moscow; DSc., PhD; Principal Research Fellow (Research Professor) of Department of Kinetics and Catalysis, N. Semenov Institute of Chemical Physics, Russian Academy of Sciences, Moscow.\r\nArea of research interests: physical chemistry of complex-organized molecular and nanosized systems, including polymer-metal complexes; the surface of doped oxide semiconductors. He is an expert in structural, absorptive, catalytic and photocatalytic properties, in structural organization and dynamic features of ionic liquids, in magnetic interactions between paramagnetic centers. The author or co-author of 3 books, over 200 articles and reviews in scientific journals and books. He is an actual member of the International EPR/ESR Society, European Society on Quantum Solar Energy Conversion, Moscow House of Scientists, of the Board of Moscow Physical Society.",institutionString:null,institution:{name:"Semenov Institute of Chemical Physics",country:{name:"Russia"}}},{id:"62389",title:"PhD.",name:"Ali Demir",middleName:null,surname:"Sezer",slug:"ali-demir-sezer",fullName:"Ali Demir Sezer",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/62389/images/3413_n.jpg",biography:"Dr. Ali Demir Sezer has a Ph.D. from Pharmaceutical Biotechnology at the Faculty of Pharmacy, University of Marmara (Turkey). He is the member of many Pharmaceutical Associations and acts as a reviewer of scientific journals and European projects under different research areas such as: drug delivery systems, nanotechnology and pharmaceutical biotechnology. Dr. Sezer is the author of many scientific publications in peer-reviewed journals and poster communications. Focus of his research activity is drug delivery, physico-chemical characterization and biological evaluation of biopolymers micro and nanoparticles as modified drug delivery system, and colloidal drug carriers (liposomes, nanoparticles etc.).",institutionString:null,institution:{name:"Marmara University",country:{name:"Turkey"}}},{id:"61051",title:"Prof.",name:"Andrea",middleName:null,surname:"Natale",slug:"andrea-natale",fullName:"Andrea Natale",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"100762",title:"Prof.",name:"Andrea",middleName:null,surname:"Natale",slug:"andrea-natale",fullName:"Andrea Natale",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"St David's Medical Center",country:{name:"United States of America"}}},{id:"107416",title:"Dr.",name:"Andrea",middleName:null,surname:"Natale",slug:"andrea-natale",fullName:"Andrea Natale",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Texas Cardiac Arrhythmia",country:{name:"United States of America"}}},{id:"64434",title:"Dr.",name:"Angkoon",middleName:null,surname:"Phinyomark",slug:"angkoon-phinyomark",fullName:"Angkoon Phinyomark",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/64434/images/2619_n.jpg",biography:"My name is Angkoon Phinyomark. I received a B.Eng. degree in Computer Engineering with First Class Honors in 2008 from Prince of Songkla University, Songkhla, Thailand, where I received a Ph.D. degree in Electrical Engineering. My research interests are primarily in the area of biomedical signal processing and classification notably EMG (electromyography signal), EOG (electrooculography signal), and EEG (electroencephalography signal), image analysis notably breast cancer analysis and optical coherence tomography, and rehabilitation engineering. I became a student member of IEEE in 2008. During October 2011-March 2012, I had worked at School of Computer Science and Electronic Engineering, University of Essex, Colchester, Essex, United Kingdom. In addition, during a B.Eng. I had been a visiting research student at Faculty of Computer Science, University of Murcia, Murcia, Spain for three months.\n\nI have published over 40 papers during 5 years in refereed journals, books, and conference proceedings in the areas of electro-physiological signals processing and classification, notably EMG and EOG signals, fractal analysis, wavelet analysis, texture analysis, feature extraction and machine learning algorithms, and assistive and rehabilitative devices. I have several computer programming language certificates, i.e. Sun Certified Programmer for the Java 2 Platform 1.4 (SCJP), Microsoft Certified Professional Developer, Web Developer (MCPD), Microsoft Certified Technology Specialist, .NET Framework 2.0 Web (MCTS). 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