Hot compaction of polyethylene naphthalate

In this article, we describe the production of single polymer composites from polyethylene naphthalate (PEN) multifilaments by using the hot compaction process. In this process, developed at Leeds University, highly oriented tapes or fibers are processed at a critical temperature such that a small fraction of the surface of each oriented element is melted, which on cooling recrystallizes to form the matrix of the composite. This process is, therefore, a way to produce novel high‐volume fraction polymer/polymer composites where the two phases are chemically the same material. A variety of experimental techniques, including mechanical tests and differential scanning calorimetry, were used to examine the mechanical properties and morphology of the compacted PEN sheets. Bidirectional (0/90) samples were made at a range of compaction temperatures chosen to span the melting range of the PEN multifilaments (268–276°C). Measurement of the mechanical properties of these samples, specifically the in‐plane modulus and strength, allowed the optimum compaction temperature to be ascertained (～ 271°C), and hence, the optimum mechanical properties. The optimum compacted PEN sheets were found to have an initial modulus close to 10 GPa and a strength of just over 200 MPa. The glass transition temperature of the optimum compacted sheets was measured to be 150°C, nearly 40°C higher than compacted poly(ethylene terephthalate) (PET) sheets. In previous work on polypropylene and PET hot compacted materials, it proved instructive to envisage these materials as a composite where the original oriented multifilaments are regarded as the reinforcing phase, and the melted and recrystallized material are regarded as the matrix phase. Dynamic mechanical bending tests (DMTA) were used here to confirm this for PEN. DMTA tests were carried out on the original fibers and on a sample of completely melted material to determine the fiber and matrix properties, respectively. The composite properties were then predicted by using a simple rule of mixtures and this was found to be in excellent agreement with the magnitude and measured temperature dependence of the hot compacted PEN material. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 796–802, 2004     

Hot compaction of woven nylon 6,6 multifilaments

We describe a study of the hot compaction of woven nylon 6,6 multifilaments produced by a patented procedure, developed at the University of Leeds, for creating novel single‐polymer composites. In this process, an assembly of oriented elements, often in the form of a woven cloth, is held under pressure and taken to a critical temperature so that a small fraction of the surface of each oriented element is melted, which on cooling recrystallizes to form the matrix of the single‐polymer composite. This process is therefore a way of producing novel high‐volume‐fraction polymer/polymer composites in which the two phases are chemically the same material. Nylon is an obvious candidate material for this process because oriented nylon multifilaments are available on a commercial scale. The aim of this study was first to establish the conditions of temperature and pressure for the successful hot compaction of oriented nylon 6,6 fibers and second to assess the mechanical properties of the manufactured hot‐compacted nylon sheets. A crucial aspect of this work, not previously examined in hot‐compaction studies of other oriented polymers, was the sensitivity of the properties to absorbed water, with a significant change in the properties measured immediately after hot‐compaction processing and 2 weeks later when 2% water had been absorbed by the compacted nylon sheets. As expected, the water uptake had a greater effect on those properties that depended on local chain interactions (e.g., the modulus and yield strength) and less effect on those properties that depended on the large‐scale properties of the molecular network (e.g., strength). The only negative aspect of the properties of the hot‐compacted nylon sheets was the elevated‐temperature performance of the wet sample, with the modulus falling to a very low value at a temperature of 80°C. However, apart from the elevated‐temperature performance, the majority of the measured properties of the hot‐compacted nylon sheets were comparable to those of hot‐compacted polypropylene and poly(ethylene terephthalate). © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 991–997, 2006     

The incorporation of carbon nanofibres to enhance the properties of self reinforced, single polymer composites

This paper describes the incorporation of carbon nanofibres (CNF) into polypropylene (PP) single polymer composites, materials where both the reinforcing phase and the matrix phase are PP. The CNF/PP composites were produced from an assembly of highly oriented tapes. The process of making the composites involves heating the tapes to a critical temperature such that a small fraction of the surface of each tape is melted; on cooling this recrystallises to form the matrix of the composite. The production of the composites required optimisation of three stages; incorporation of CNF into PP tapes, orientation of CNF/PP tapes by tensile drawing and hot compaction of the tapes. Results are presented to describe the research and findings in each of these key stages.Preliminary studies showed that the introduction of small amounts of carbon nanofibres (CNF) significantly improved the properties of isotropic PP. For example, 5% volume addition of CNF gave a 60% increase in the room temperature Young's modulus and a reduction of 35% in the thermal expansion coefficient. Moreover, the percentage enhancement of properties was greater at high temperatures where the stiffness of the PP is much reduced. These results can be very well understood in terms of conventional composite modelling.In unidirectional CNF/PP hot compacted composites the major improvements in mechanical behaviour are in the direction transverse to the orientation direction, where the CNF can make a proportionately greater contribution to the properties, and as shown by dynamic mechanical behaviour, this is most marked at high temperatures. Composite modelling based on uniform strain with appropriate allowance for the CNF aspect ratio predicts the behaviour extremely well. A very interesting result is that the peel strength of composites produced by hot compaction of woven CNF/PP shows a four-fold increase over woven PP composites and this is increased by another factor of two by the addition of a maleic anhydride compatibiliser. A further interesting result, of some practical significance, is that although the incorporation of CNF into PP causes voiding and some loss of molecular orientation during drawing, the hot compaction process closes and seals the voids, so that the original PP density is recovered.     

A dynamic mechanical study on unidirectional carbon fiber-reinforced polypropylene composites

Fiber-reinforced polymer composites show high specific strength and stiffness. The alignment of reinforcing fibers results in anisotropy of the material. This anisotropic behavior has been studied through dynamic mechanical analysis of unidirectional carbon fiber-reinforced polypropylene (CFRPP) composites measured in both parallel and transverse directions to fiber arrangement. Several parameters such as storage modulus (E′), loss modulus (E″), loss factor or damping factor (tan δ), and complex viscosity (MU^*) have been determined over a wide range of frequencies and at a fixed temperature. Relaxation and retardation spectra have been constructed for these composites. Modulus enhancement occurs due to stiffness imparted by the fiber and efficient stress transfer at the interface. Relaxation of the polymer matrix ceases with increase in the volume fraction of the fibers. α′-relaxation is observed for the composite having a 13% volume fraction of fibers and is ascribed to relaxation in the crystalline phase where the additional crystallinity arises out of the transcrystalline growth at the fiber–matrix interface. There exists a good correlation between theroretical curves with the experimental ones. Relaxation and retardation spectra and the dynamic parameters determined for these composites show a good correlation with the volume fraction of fibers as well as the direction of the applied load. © 1994 John Wiley & Sons, Inc.     

Performance enhancement of nylon/kevlar fiber composites through viscoelastically generated pre‐stress

Kevlar‐29 fibers have high strength and stiffness but nylon 6,6 fibers have greater ductility. Thus by commingling these fibers prior to molding in a resin, the resulting hybrid composite may be mechanically superior to the corresponding single fiber‐type composites. The contribution made by viscoelastically generated pre‐stress, via the commingled nylon fibers, should add further performance enhancement. This paper reports on an initial study into the Charpy impact toughness and flexural stiffness of hybrid (commingled) nylon/Kevlar fiber viscoelastically pre‐stressed composites at low fiber volume fractions. The main findings show that (i) hybrid composites (with no pre‐stress) absorb more impact energy than Kevlar fiber‐only composites; (ii) pre‐stress further increases impact energy absorption in the hybrid case by up to 33%; (iii) pre‐stress increases flexural modulus by ∼40% in the hybrid composites. These findings are discussed in relation to practical composite applications. POLYM. COMPOS., 35:931–938, 2014. © 2013 Society of Plastics Engineers     

Optically transparent self-reinforced poly(ethylene terephthalate) composites: molecular orientation and mechanical properties

Self-reinforced composites have been fabricated by compaction of oriented polyethylene terephthalate (PET) fibers under pressure at temperatures near, but below, their melting point. The originally white fiber bundles, which were about 40% crystalline, show increased crystallinity (55%) but optical translucency after processing. Differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) were used to study the crystallization and orientation of the fibers, revealing that the degree of crystallinity was somewhat insensitive to compaction conditions while the melting point increased substantially with increasing compaction temperature. Crystalline orientation, gauged using the Hermans orientation parameter from WAXD data, indicated that no significant loss in orientation of the crystalline fraction occurs due to compaction. Mechanical characterization revealed a stepwise decrease in flexural modulus (9.4-8.1 GPa) and concomitant increase in transverse modulus and strength on increasing the compaction temperature from 255 to 259 °C. This transition in behavior was accompanied by a loss of optical transparency and a change in the distribution of amorphous fraction from fine intrafibrillar domains to coarse interfibrillar domains as seen with electron microscopy. We argue then that the mechanical properties of PET compactions are influenced more by orientation of the amorphous phase than that of the crystalline phase. The impact properties of compacted materials, characterized using an unnotched Charpy test method, showed remarkable impact resistance after compaction, with impact toughness decreasing as compaction temperature was increased.     

Strength of short-fiber reinforced composites

The structural utility of short, glass fiber-reinforced epoxy composities is experimentally investigated for fiber volume fractions from 0.15 to 0.5. The strength and stiffness of systems with randomly oriented fibers are compared with those of similar composites with aligned fibers. The ultimate strength of both types of material increses in a reasonably linear fashion with volume fraction up to 0.5. For all volume fractions in this range, strength of the random composites is slightly higher than the longitudinal and much higher than the transverse strength of equivalent compsites with aligned fibers. The modulus of the random system is approximately two-thirds the longitudinal and twice the transverse modulus of the unidirectional material. The structural utility of the flow molded material is greatest in uniaxial, stiffness critical situations. The greater strength and planar isotropy of the random composites make them preferable in all strength limited or multiaxial applications.     

Effect of short polyethylene terephthalate fibers on properties of ethylene-propylene diene rubber composites

The alteration in some properties of electron beam (EB) cured ethylene-propylene diene rubber (EPDM) reinforced by polyethylene terephthalate (PET) fiber was investigated in this study. Bonding system Resorcinol/Hexamethylenetetramine/Silica (RHS) was used to enhance the fiber/EPDM adhesion and to maintain optimum composite strength properties. Mechanical properties of composites namely; tensile strength, hardness and modulus at 100 % elongation have been enhanced by adding PET fibers and increasing irradiation dose. Moreover, the effect of fiber loading and irradiation dose on the soluble fraction behavior of the composite in benzene was also investigated. The soluble fraction of the composites decreased with increasing the fiber loading and irradiation dose. The extent of fiber alignment and strength of fiber-rubber interface adhesion were analyzed from the anisotropic swelling measurements. In addition, thermal stability of the composites was increased. Besides, the mechanical properties like tensile strength and stiffness were improved by thermal ageing. Scanning electron microscopy (SEM) for the fractured surfaces and Wide- angle X- ray diffraction (WAXD) of the investigated samples confirmed that the adhesion occurred between fibers and EPDM.     

Morphology and mechanical properties of unidirectional sisal– epoxy composites

Plant fibers are of increasing interest for use in composite materials. They are renewable resources and waste management is easier than with glass fibers. In the present study, longitudinal stiffness and strength as well as morphology of unidirectional sisal–epoxy composites manufactured by resin transfer molding (RTM) were studied. Horseshoe‐shaped sisal fiber bundles (technical fibers) were nonuniformly distributed in the matrix. In contrast to many wood composites, lumen was not filled by polymer matrix. Technical sisal fibers showed higher effective modulus when included in the composite material than in the technical fiber test (40 GPa as compared with 24 GPa). In contrast, the effective technical fiber strength in the composites was estimated to be around 400 MPa in comparison with a measured technical fiber tensile strength of 550 MPa. Reasons for these phenomena are discussed. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 2358–2365, 2002     

Biopolyamide hybrid composites for high performance applications

This study focuses on the performance characteristics of wood/short carbon fiber hybrid biopolyamide11 (PA11) composites. The composites were produced by melt‐compounding of the fibers with the polyamide via extrusion and injection molding. The results showed that mechanical properties, such as tensile and flexural strength and modulus of the wood fiber composites were significantly higher than the PA11 and hybridization with carbon fiber further enhanced the performance properties, as well as the thermal resistance of the composites. Compared to wood fiber composites (30% wood fiber), hybridization with carbon fiber (10% wood fiber and 20% carbon fiber) increased the tensile and flexural modulus by 168% and 142%, respectively. Izod impact strength of the hybrid composites exhibited a good improvement compared to wood fiber composites. Thermal properties and resistance to water absorption of the composites were improved by hybridization with carbon fiber. In overall, the study indicated that the developed hybrid composites are promising candidates for high performance applications, where high stiffness and thermal resistance are required. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43595.     

Influence of fiber volume fraction and aspect ratio in resol–sisal composites

Vegetable fibers are being used as reinforcements in polymeric matrices with a wide variety of applications. Among these fibers, sisal is of particular interest due to the high impact strength and moderate tensile and flexural properties of its derivated composites. Because of its low cost and affinity, a phenol–formaldehyde resin, resol, has been selected as the matrix to obtain resol–sisal composites. The influence of fiber length and volume fraction on flexural properties has been studied. An optimum for the fiber length as well as for the fiber volume fraction was found. The improvement of the properties occurred up to a length of about 23 mm. The use of longer fibers lead to reduced properties because they tended to curl and bend during processing. Besides, actual composite densities were lower than theoretical ones mainly due to the presence of voids. This undesirable porosity produced a reduction in flexural properties at high fiber contents. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 2714–2722, 2003     

A microindentation study of polyethylene composites produced by hot compaction

Microindentation measurements are reported on a range of single polymer polyethylene (PE) composites, which are produced by hot compaction of high modulus PE fibers. It is possible to measure two hardness values, parallel and perpendicular to the fiber direction respectively, from which the microindentation anisotropy is defined. The hardness values relate to the instantaneous elastic recovery of the fibers, and the results show that the microindentation measurement is deforming a material volume below the surface of the sheets comparable to the dimensions of the fibers. It appears that the microindentation anisotropy approaches a limiting value with increasing fiber orientation, i.e., as the Young's modulus of the fibers increases. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1659–1663, 2006     

Solid freeform fabrication of epoxidized soybean oil/epoxy composites with di‐, tri‐, and polyethylene amine curing agents

Soybean oil/epoxy‐based composites are prepared by solid freeform fabrication (SFF) methods. SFF methods built materials by the repetitive addition of thin layers. The mixture of epoxidized soybean oil and epoxy resin is modified with di‐, tri‐, or polyethylene amine gelling agent to solidify the materials until curing occurs. The high strength and stiffness composites are formed through fiber reinforcement. E‐glass, carbon, and mineral fibers are used in the formulations. The type of fiber affects the properties of the composites. It was found that a combination of two types of fibers could be used to achieve higher strength and stiffness parts than can be obtained from a single fiber type. In addition, the effects of curing temperature, curing time, and fiber concentration on mechanical properties of composites are studied and reported. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 356–363, 2004     

The incorporation of carbon nanofibres to enhance the interlayer adhesion of hot compacted single-polymer polypropylene composites

The current work is a major extension of two very different studies carried out previously to investigate factors that affect the peel strength of single-polymer composites produced by the Leeds hot compaction process. First, it was found that the peel strength was significantly increased by introducing interleaved films, of the same polymer, between the layers of woven oriented tapes that make up the composite. Secondly, it was shown that incorporation of carbon nanofibres (CNF) into the oriented tapes prior to hot compaction could also increase peel strength.In the present study we have investigated the amalgamation of these two approaches, in particular to see if there are synergistic advantages in the combination. Samples were produced with and without interleaved films, and with and without carbon nanofibres, located either in the oriented polypropylene tapes, in the interleaved film or in both. Maximum peel strength was achieved with the combination of the interleaved film and the incorporated nanofibres, but importantly this could be achieved with the CNF located only in the film. This has significant processing and performance advantages as the incorporation of CNF into the oriented tapes tends to limit the drawability of the polypropylene due to internal voiding around the particles.Scanning electron micrographs of the hot compacted composites show a strong correlation between the observed damage on the peel surfaces and the measured peel loads. It is shown that the peel load is dependent on the fraction of melted matrix at the interface and hence the interleaved films give additional matrix material at this point. It is also shown that the incorporation of CNF promotes fibrillation, and so increases the amount of energy absorbed during peeling.     

The extrusion and performance of plasticized poly(vinyl chloride) hose reinforced with short cellulose fibers

Short fibers of natural cellulose treated to provide dispersability and strong interfacial bonding are ideal reinforcements for plasticized vinyl compounds. The development of substantial strength and stiffness in unidirectional composites indicates the reinforcing potential of these high aspect-ratio fibers in soft compositions. Special extrusion dies developed to control fiber directionality in rubber extrudates are equally applicable to vinyl hose. The unusual expanding geometry of these tools aligns the fibers toward the circumferential direction to provide optimum reinforcement against contained pressure loading. Thus, reinforced poly(vinyl chloride) air and water hoses can be produced in a single extrusion step, since all of the necessary reinforcement is contained in the compound.     

A study of the thermomechanical properties of carbon fiber-polypropylene composites

Short fiber composites were produced using polypropylene as matrix and polyacrylonitrile (PAN)-based fibers or vapor grown carbon fibers (VGCF) as reinforcement. The strength, stiffness, and coefficient of thermal expansion (CTE) of the composites were measured. The VGCF-composites showed strength and CTE that are competitive with those of “conventional” PAN-fiber composites, but the stiffness was marginally lower. Micromechanical modeling of the PAN composite properties gives results consistent with the measurements. The models can be used to infer the apparent VGCF-properties from their composites.     

PP/碳纤维纸夹芯“三明治”复合材料性能

以碳纤维纸(CFP)作为芯材,聚丙烯(PP)作为皮材,用平板硫化机热压制成PP–CFP–PP"三明治"式复合材料,并测试了复合材料的各项力学性能。结果表明,加入CFP后复合材料的力学性能总体上有所改善,针对不同PP基体、CFP对复合材料力学性能的改善方式有所不同,对基材本身强度/刚度小的复合材料增强/增刚效果明显,而对于基材本身强度/刚度大的复合材料,加入CFP后其断裂伸长率、无缺口冲击强度提高明显,同时复合材料的缺口冲击强度有所降低。     

Resol–vegetable fibers composites

Vegetable fibers like cotton, sisal, and sugar cane bagasse have been used as reinforcement in a polymeric matrix. Because of its low cost and affinity with lignocellulosic fibers, a phenol‐formaldehyde resin —resol— was selected as the matrix. Composites were prepared by compression molding. The influence of fiber volume fraction‐V_f‐in flexural properties and density of composites has been studied. Cotton and sugar cane bagasse composites present a V_f value at which flexural strength and modulus are maxima. However, sisal composites show a continuous rise in flexural strength and modulus as fiber volume fraction increases, up to 76%, which is the highest concentration studied. Composites made with raw cotton show the highest values of strength and stiffness. The actual density of composites is always lower than theoretical density, due to the presence of voids. Scanning Electron Microscopy reveals a good adhesion between fiber and matrix in the composites. In addition, the flexural properties were analyzed with an efficiency criterion, which relates strength and stiffness with density, and the values obtained were compared with those corresponding to typical structural materials. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 1832–1840, 2000     

The use of an interleaved film for optimising the properties of hot compacted polyethylene single polymer composites

It is shown that the incorporation of interleaved films has major advantages for the production of polyethylene single polymer composites by the process of selective melting (termed hot compaction). The key issue is to choose a compaction temperature which melts the minimum amount of the original oriented elements whilst achieving acceptable bonding within the compacted structure. Utilising an interleaved film, excellent interlayer peel strengths can be achieved at lower compaction temperatures giving greater retention of the oriented fraction of the original fibres or tapes and a wider processing window. For example, using a very high modulus, ultra-high molecular weight, polyethylene tape, together with an interleaved film, resulted in an in-plane modulus of 25 GPa, an in-plane strength of 500 MPa, and an interlayer strength of >10 N/10 mm. These are amongst the highest values reported for a single polymer composite. Other important factors have been investigated including fabric weave style and whether it is better to use fibres or tapes as the oriented reinforcement.     

Bio‐composites for structural applications: Poly‐l‐lactide reinforced with long sisal fiber bundles

Fully bio‐based and biodegradable composites were compression molded from unidirectionally aligned sisal fiber bundles and a polylactide polymer matrix (PLLA). Caustic soda treatment was employed to modify the strength of sisal fibers and to improve fiber to matrix adhesion. Mechanical properties of PLLA/sisal fiber composites improved with caustic soda treatment: the mean flexural strength and modulus increased from 279 MPa and 19.4 GPa respectively to 286 MPa and 22 GPa at a fiber volume fraction of V_f = 0.6. The glass transition temperature decreased with increasing fiber content in composites reinforced with untreated sisal fibers due to interfacial friction. The damping at the caustic soda‐treated fibers‐PLLA interface was reduced due to the presence of transcrystalline morphology at the fiber to matrix interface. It was demonstrated that high strength, high modulus sisal‐PLLA composites can be produced with effective stress transfer at well‐bonded fiber to matrix interfaces. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40999.