The hot compaction behaviour of woven oriented polypropylene fibres and tapes. I. Mechanical properties

The aim of this work was to establish the important parameters that control the hot compaction behaviour of woven oriented polypropylene. Five commercial woven cloths, based on four different polypropylene polymers, were selected so that the perceived important variables could be studied. These include the mechanical properties of the original oriented tapes or fibres, the geometry of the oriented reinforcement (fibres or tapes), the mechanical properties of the base polymer (which are crucially dependant on the molecular weight and morphology), and the weave style. The five cloths were chosen so as to explore the boundaries of these various parameters, i.e. low and high molecular weight: circular or rectangular reinforcement (fibres or tapes): low or high tape initial orientation: coarse or fine weave.A vital aspect of this study was the realisation that hot compacted polypropylene could be envisaged as a composite, comprising an oriented ‘reinforcement’ bound together by a matrix phase, formed by melting and recrystallisation of the original oriented material. We have established the crucial importance of the properties of the melted and recrystallised matrix phase, especially the level of ductility, in controlling the properties of the hot compacted composite.     

The development of morphology during hot compaction of Tensylon high-modulus polyethylene tapes and woven cloths

The development of morphology in tapes and woven cloths of oriented melt-spun Tensylon polyethylene has been studied both before and after hot compaction over a range of temperatures below and above the optimum. For both the unidirectional fibres and the woven cloths, the optimum temperature was found to be where approximately 30% of the original structure was lost which, for Tensylon tapes, was ∼2 K below the point of major crystalline melting, giving a processing window roughly twice as wide as for other previously studied polyethylene materials. Transverse sections show a two-component morphology after etching of cratered ribbons emerging from a flat, relatively featureless landscape. This morphology disappears at the highest temperature studied when the longitudinal morphology consists of oriented walls from which transcrystalline units have grown during cooling. Morphological comparison with other polyethylenes and their compactions places Tensylon behaviour alongside Dyneema, Spectra and Tekmilon rather than the melt-spun Certran.     

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.     

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 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.     

Structural description of self-reinforced polypropylene composites

Self-reinforced polypropylene composites (SR-PP) possess an exceptional property spectrum and are predestined for use in a multitude of structural or semi-structural applications. However, the underlying macromolecular orientation can only be transferred into the layered composites consolidated out of highly stretched fibres and tapes of semi-finished textile products. Specific preservation of the self-reinforcement throughout processing and beyond is necessary and creates special challenges for processing technology. Depending on the processing temperatures and pressures selected, the highly oriented fibres and tapes are influenced by their own degree of self-reinforcement, which, in turn, affects the microstructure and remaining composite properties. In this publication, three different semi-finished textile products are introduced as basic materials. Exemplary selected test samples, which display a low degree of compaction on the one hand and a high degree of compaction on the other, were subject to wet chemical etching to enable confocal laser scanning microscopic images to be created. These images were then used to compare the microstructures of the semi-finished textile products that were used.     

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 poly(ethylene terephthalate) multifilaments

Here we describe the development of a process, and the resulting mechanical properties, for hot‐compacted sheets of woven poly(ethylene terephthalate) (PET) multifilaments. Investigation of the various processing parameters showed that a key aspect was the time spent at the compaction temperature, termed the dwell time. Molecular weight measurements, using intrinsic viscosity, showed that hydrolytic degradation occurred rapidly at the temperatures required for successful compaction, leading to embrittlement of the resulting materials with increasing dwell time. A dwell time of 2 min was found to be optimum because this gave the required percentage of melted material to bind the structure together, while giving only a small decrease in molecular weight. A combination of techniques, including mechanical tests, differential scanning calorimetry, and scanning electron microscopy, was used to examine the mechanical properties and morphology of the optimum compacted sheets. These tests reinforced the view from previous studies on hot‐compacted polypropylene, of hot‐compacted sheets as self‐reinforced composites, whose behavior is a combination of the properties of the two components, that is, the original oriented multifilaments and the melted and recrystallized matrix. Other key findings from the research included a confirmation of the importance of obtaining high ductility in the melted and recrystallized phases, promoted by using a high molecular weight or by suppressing crystallinity during processing, and the proportionately high‐impact performance of hot‐compacted sheets, compared with that of other materials. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 2223–2233, 2004     

Developments in oriented polymers, 1970–2004

Abstract

The discovery of methods to make highly oriented polymers has given tremendous stimulus to both basic polymer science and industrial developments in the period 1970 to the present. High modulus, high strength fibres for aramids and polyethylene, are based on very different methodologies but the ultimate result is similar in producing fully extended polymer chains. For polymers in solid sections, the enhancement of properties is less dramatic but still very worthwhile. In this case, three methods are described: hydrostatic extrusion, die-drawing and hot compaction of oriented fibres and tapes. Hot compaction is a new technique with many possibilities for which a wide range of applications has already been identified.     

Influence of Different Woven Geometry in Poly(propylene) Woven Composites

Summary: The difference between the melting temperatures of poly(propylene) (PP) fibre and random poly(propylene‐co‐ethylene) (PPE) was exploited in order to establish processing conditions for an all PP composite. Under these conditions the matrix must be a liquid in order to ensure good wetting and impregnation at the fibres, though the temperature must not be too high to avoid melting the fibres. The high chemical compatibility of the two components allowed creation of strong physico‐chemical interactions, which favour strong interfacial adhesion. The static and dynamic mechanical properties and morphology of poly(propylene) woven fabric reinforced random PPE composites have been investigated with reference to the woven geometry that influenced the properties of the woven composites. Among the various cloth architectures that were used in the PP‐PPE composites, the satin weave imparted overall excellent mechanical properties due to the weave parameters, such as high float length and fibre count, low interlace point and crimp angle, etc. Morphology of the composite has been investigated by macro photography and scanning electron microscopy. Images from scanning electron microscopy provided confirmation of the above results by displaying the consolidation and good fibre‐matrix wetting of the composites.

Loss modulus of poly(propylene) woven‐matrix composites with different types of woven geometry.     

Solid‐state compaction and drawing of nascent reactor powders of ultra‐high‐molecular‐weight polyethylene

The continuous production of ultra‐high‐molecular‐weight polyethylene (UHMWPE) filaments was studied by the direct roll forming of nascent reactor powders followed by subsequent multistage orientation drawing below their melting points. The UHMWPE reactor powders used in this study were prepared by the polymerization of ethylene in the presence of soluble magnesium complexes, and they exhibited high yield even at low reaction temperatures. The unique, microporous powder morphology contributed to the successful compaction of the UHMWPE powders into coherent tapes below their melting temperatures. The small‐angle X‐ray scattering study of the compacted tapes revealed that folded‐chain crystals with a relatively long‐range order were formed during the compaction and were transformed into extended‐chain crystals as the draw ratio increased. Our results also reveal that the drawability and tensile and thermal properties of the filaments depended sensitively on both the polymerization and solid‐state processing conditions. The fiber drawn to a total draw ratio of 90 in the study had a tensile strength of 2.5 GPa and a tensile modulus of 130 GPa. Finally, the solid‐state drawn UHMWPE filaments were treated with O₂ plasma, and the enhancement of the interfacial shear strength by the surface treatment is presented. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 718–730, 2005     

On morphologies developed during two‐dimensional compaction of woven polypropylene tapes

The microstructure of compacted woven polypropylene cloths prepared at their optimum compaction temperature of 184°C has been examined. Details of transverse and longitudinal cross‐sections have been revealed by permanganic etching and observed with scanning electron microscopy. The original cloth was found to contain perpendicular cracks and biconical defects reported previously in other systems. After compaction, the cloth bonded together to form a thick solid sheet, with a melting point raised for the residual material but reduced for the recrystallized component. The higher melting regions form a continuous three‐dimensional network with linear traces in a longitudinal section, in agreement with recent observations of fiber structure. Recrystallization occurs both within and externally from tapes: where parallel tapes meet, transcrystalline layers emanate from tape surfaces, with a distinct line where the two growth fronts meet. In some more extensive recrystallized regions row structures are formed, probably indicating local flow during compaction. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 787–793, 2000     

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.     

Interfacial properties of highly oriented coextruded polypropylene tapes for the creation of recyclable all‐polypropylene composites

The creation of highly oriented, coextruded polypropylene (PP) tapes allows the production of novel, wholly thermoplastic, recyclable “all‐polypropylene” (all‐PP) composites, which possess both a large temperature processing window (>30°C) and a high volume fraction of reinforcement phase (highly oriented PP tapes: >90%). This large processing window is achieved by using coextruded, highly drawn PP tapes. To achieve coherent all‐PP composites the interfacial characteristics following consolidation must be understood. This article investigates the interfacial characteristics of these coextruded tapes by using microcomposite models to create interfaces between tapes of varying draw ratios, drawing temperatures, skin/core ratios, and skin layer thicknesses. The tape drawing parameters are seen to control the interfacial properties in subsequent microcomposite models. The failure mode of these specimens, and hence bond strength, varies with consolidation temperature, and a model is proposed describing and explaining this behavior. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 118–129, 2007     

Resonant frequency study of tensile and shear elasticity moduli of carbon fibre reinforced composites (CFRC)

The dynamic elastic properties are important characteristics of composite materials. They control the vibrational behaviour of composite structures and are also an ideal tool for monitoring of the development of CFRCs’ mechanical properties during their processing (heat treatment, densification). The present studies have been performed to explore relations between the dynamic tensile and shear moduli and some structural features (viz., fibre fraction, fibre type, porosity, weave pattern of woven reinforcement) of various unidirectional or bi-directional fibre reinforced carbon/carbon composites, made out of PAN- or pitch-based fibres as reinforcements and phenolic resin or coal tar pitch as matrix precursors. The dynamic tensile and in-plane shear moduli were determined from resonant frequencies of a beam with free ends. The longitudinal dynamic Young’s modulus of unidirectional CFRC composites – besides its dependence on the original fibre modulus and fibre volume contents – also reflects changes induced in matrix and fibres by heat treatment. The in-plane shear modulus does not depend on the fibre type but there exists its distinct tendency to increase with increasing fibre fraction. For bi-directionally reinforced composites, the longitudinal tensile modulus is more sensitive to the fabric weave pattern than to the fibre type. Tensile modulus of diagonally cut specimens and in-plane shear modulus of longitudinally cut ones are mutually correlated and, therefore, simultaneously controlled by densification steps and graphitisation heat treatment.     

A small-angle X-ray scattering study of powder compaction

This work demonstrated a novel and potentially important application of two-dimensional small-angle X-ray scattering (2D-SAXS) to investigate powder compaction. SAXS from powder compacts of three materials commonly used for pharmaceutical tabletting exhibited azimuthal variations, with stronger intensity in the direction of the applied compaction force, relative to the transverse direction. This implied that compaction of a (macroscopic) powder could also produce changes on the molecular (nanometre) scale, which can be probed by 2D-SAXS. Two possible explanations for this effect were suggested. A combination of anisometric (i.e. elongated or flattened) granules with anisotropic morphologies could result in azimuthal variation in X-ray scattering due to granule orientation. It is expected that this mechanism would require relatively low packing density, so may operate during die filling. Granule re-orientation appeared less likely at higher packing densities and compaction pressures, however. Under these conditions, the changes in the 2D-SAXS patterns would be consistent with the powder granules becoming relatively flattened in the compression direction, with corresponding changes in their nano-scale morphology. The magnitude of this effect was found to vary between the materials used and increased with compaction pressure. This suggested that 2D-SAXS studies could provide useful information on force-transmission within a compressed powder. Further analysis of the data also suggested differences in the compaction mechanisms (i.e. granule re-orientation, deformation or fragmentation) between the materials studied.     

Influence of Different Woven Geometry and Ply Effect in Woven Thermoplastic Composite Behaviour-Part 2

Abstract

Works on woven composite both thermoset and thermoplastic are numerous, however in most instances they involve the use of preimpregnated fabric. It is apparent that woven thermoplastic system has significant potential due to the combined properties such as better damage tolerence, recyclability, easy processing, storage, etc. Here work on woven thermoplastic composites based on Continuous Fiber Impregnated towpreg (COFIT) tape rather than conventional approach is reported. The influences of different woven geometry and ply effect were investigated. Correlations between different woven geometry and weave characteristics were also noted. In general, the woven composite properties are influenced by many process variables such as type of towpreg, woven geometry, number of plies etc.     

Texturing unsaturated granular media submitted to compaction and kneading processes

The aim of this study is to characterise the mass and volume of wet unsaturated granular media for an equilibrium state obtained after a compaction or kneading process. For two mixing processes for powder and water, under constant operating conditions, the dry density is correlated to water content by a characteristic relation. As observed in the dynamic compaction of soils, this phenomenon exists also for the kneading and static compaction of different raw materials. An analytical expression is suggested for modelling the relation between these two parameters.     

Multi‐jet nozzle electrospinning on textile substrates: observations on process and nanofibre mat deposition

Electrospinning is a simple and versatile process for producing small‐diameter fibres (nanofibres). However, in spite of the many potential applications of electrospun nanofibres, further process developments are still necessary to achieve a decisive productivity breakthrough for electrospinning plants. Increasing knowledge of multi‐jet electrospinning is crucial for developing industrial devices for large‐scale nanofibre production. This paper reports on the effect of a non‐conducting textile substrate placed between a jet‐emitting source (nine‐nozzle arrangement) and collector. Shielding the electric field changes the electrospinning conditions, nanofibre morphology, stability of jets and fibre deposition on the collecting surface. Various perturbation phenomena of the electrically driven jets were recorded and are described. The intensity of the perturbations increases as the weight of the non‐woven substrate increases resulting in defects in the nanofibrous mat (i.e. beaded nanofibres), production of tick fibres or failure to produce fibrous materials (e.g. films, droplets). The paper also reports an objective image‐processing procedure to enhance the evaluation of the collector after nanofibre deposition. Copyright © 2010 Society of Chemical Industry     

Compaction of textile reinforcements for composites manufacturing. II: Compaction and relaxation of dry and H2O-saturated woven reinforcements

Previous analysis of published experimental results on compaction and relaxation of textile reinforcements allowed the effects of some processing parameters on the mechanical behavior of the reinforcements to be identified. However, a limited number of relaxation results are available; also, the effect of some parameters on compaction received limited attention, and the behavior observed with fluid-saturated reinforcements has not been investigated. In this paper, the results of a structured experimental program of compaction and relaxation performed on three woven reinforcements are reported. In half the trials, a relaxation period was imposed on the samples. In the other half, samples saturated with distilled H₂O were compacted. The selection of the processing parameters was found to be as important as the selection of the reinforcement itself for the definition of a manufacturing operation. The processing parameters governing the compaction and relaxation were seen not to be the same, and the fiber reorganization that occurs during the compaction phase was found to have a different effect on successive compaction cycles than the reorganization occurring during the relaxation.