WO2010032048A1 - Articles polymères et leur procédé de fabrication - Google Patents

Articles polymères et leur procédé de fabrication Download PDF

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Publication number
WO2010032048A1
WO2010032048A1 PCT/GB2009/051202 GB2009051202W WO2010032048A1 WO 2010032048 A1 WO2010032048 A1 WO 2010032048A1 GB 2009051202 W GB2009051202 W GB 2009051202W WO 2010032048 A1 WO2010032048 A1 WO 2010032048A1
Authority
WO
WIPO (PCT)
Prior art keywords
layers
layer
particles
film
melted
Prior art date
Application number
PCT/GB2009/051202
Other languages
English (en)
Inventor
Professor Ian Macmillan Ward
Dr Richard John Foster Foster
Dr Mark James Bonner
Ian Mark Bingham
Original Assignee
Iti Scotland Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GB0816964A external-priority patent/GB0816964D0/en
Priority claimed from GB0905723A external-priority patent/GB0905723D0/en
Application filed by Iti Scotland Limited filed Critical Iti Scotland Limited
Publication of WO2010032048A1 publication Critical patent/WO2010032048A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/006—Pressing and sintering powders, granules or fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C37/00—Component parts, details, accessories or auxiliary operations, not covered by group B29C33/00 or B29C35/00
    • B29C37/0078—Measures or configurations for obtaining anchoring effects in the contact areas between layers
    • B29C37/0082—Mechanical anchoring
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/58—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres
    • B29C70/64—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres the filler influencing the surface characteristics of the material, e.g. by concentrating near the surface or by incorporating in the surface by force
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    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
    • B29C70/681—Component parts, details or accessories; Auxiliary operations
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    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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    • B32B2377/00—Polyamides

Definitions

  • the present invention relates to polymeric articles made from oriented polymeric strands, and in particular to an improved process for making such articles, sub-articles used to create such articles and processes for making such sub-articles..
  • the moulding temperature is said to be between the melting points of the fibre and the interlayer (matrix).
  • the volume fraction of the fibres is stated to be 0.69 or 0.74.
  • the articles are said to have surprisingly poor properties, possibly because of weak adhesion between fibres and matrix (melted film).
  • W02004/103673 (Ward) describes a process for the production of a polymeric articles comprising the steps of: (a) forming a ply having successive layers, namely (i) a first layer made up of strands of an oriented polymeric material; (ii) a second layer of a polymeric material; (iii) a third layer made up of strands of an oriented polymeric material, wherein the second layer has a lower peak melting temperature than that of the first and third layers; (b) subjecting the ply to conditions of time, temperature and pressure sufficient to melt a proportion of the first layer, to melt the second layer entirely, and to melt a proportion of the third layer; and to compact the ply; and (c) cooling the compacted ply.
  • Cooling in the first and second aspects can include permitting the compacted ply to cool naturally; forced draught cooling; plunge cooling; any other type of accelerated cooling; and retarded cooling.
  • strands is used to denote all oriented elongate elements of polymeric materials useful in the process and may be in the form of fibres or filaments, bands, ribbons or tapes, formed for example by slitting melt formed films, or by extrusion. Whatever their form the strands may be laid in a non-woven web or formed into yarns comprising multiple filaments or fibres, or used in the form of a monofilament yarn.
  • the strands can be made by any suitable process, for example solution or gel or melt forming, preferably by melt forming.
  • the particles have a particle size of up to 100 microns and particularly preferably up to 50 microns and comprise one or more of: a calcium based hydroxyl appetite (Mg3Si4O10(OH)2), talk or clay, carbon black, Aluminium Oxide, Hydroxyapatite, glass, fly ash or cement powder.
  • the process may further including the step of providing an inter-layer polymer film between said first and second layers and having a melting temperature below that of said first and second layers and supplying said particles to the surface of said film.
  • the process may include the step of providing an inter-layer polymer film between said first and second layers and having a melting temperature below that of said first and second layers and supplying and capturing said particles within said film.
  • the method further including the step of supplying said particles within a polymer film and sandwiching said film and particles between said first and second layers.
  • the method includes the step of supplying said particles in said film in a ratio of between 1 :99 and 6:4 and preferably 1 :9 to 2:8 by weight of particles to polymer.
  • the process may use strands of the oriented polymeric material of the first and second layers in the form of polyethylene, polypropylene, polyoxymethylene, polyester, nylon or polyetherketone.
  • a particularly advantageous method includes the step of using a sandwich layer in the form of polypropylene polyethylene, polyoxymethylene, polyester, nylon or polyetherketone.
  • the method may include the step of forming the first, second and sandwich layers of the same type of polymeric material.
  • the method includes the step of using a sandwich layer that has a peak melting temperature at least 4 0 C lower than the peak melting temperature of the first and second layers.
  • Said sandwich layer may have a thickness of up to 1 mm.
  • the compaction pressure is between4.9 MPa and 7MPa and the compaction temperature between 187.3 0 C and 195.2 0 C.
  • the strands may be provided in the form of tapes and preferably at least 1 % but not all of each of the first and second layer is melted (vol/vol of layer). The percentage may be increased to at least 5% but not more than 80% and preferably not more than 40% is melted and preferably the sandwich layer is entirely melted.
  • a polymeric article manufactured by a process as claimed in the attached claims, the polymeric article having oriented regions which are the un-melted portions of the first and second layers and amorphous regions which are composed of the melted and cooled first and second layers together with said particles held therein.
  • the polymeric article has oriented regions which are the un-melted portions of the first and second layers and amorphous regions which are composed of the melted and cooled first and second layers together with a melted sandwich layer therebetween and in which said particles are held therein.
  • a ply having successive layers of unbounded material, namely (i) a first layer made up of strands of an oriented polymeric material; (ii) a second layer made up of strands of an oriented polymeric material; and (iii) a sandwich layer of polymer material between said first and second layers and including embedded particulates and wherein the sandwich layer has a lower peak melting temperature than that of the first or second layers and the particulates have a higher peak melting temperature than that of the first or second layers.
  • polymer article comprising a layer of polymer material and a plurality of grains of granular material embedded partially within one or more exterior surfaces.
  • Such an article may be manufactured according to a process for manufacturing the polymer article comprising the steps of: supplying a sheet of polymer material; heating at least a portion of the surface of said polymer material; introducing granular material to the surface of said polymer material; and pressing said granular material at least partially into the surface of the polymer material.
  • Figure 1 is a diagrammatic representation of a blow film rig
  • Figure 2 is a diagrammatic representation of the compaction process according to the present invention
  • Figure 3 is a graph of peel strength for various samples
  • Figure 4 is a further graph of peel strength for various samples and compares filled and non-filled samples
  • Figure 5 is a graph of peel strength versus compaction temperature for samples incorporating different filler materials within the interlayer film
  • Figure 6 is a graph of peel strength for compacted standard Propex 6060 style geotextile for different levels of surface lubricant ;
  • Figure 7 is a graph of peel strength for woven tapes made from a nucleated polypropylene for different levels of surface lubricant ;
  • Figure 8 is a graph of peel strength at various compaction temperatures for compacted samples of woven popypropylene tapes with and without an interlayer film;
  • Figure 9 is a graph of peel strength at various compaction temperatures for washed Propex 6060 polypropylene geotextile fabric with an interlayer film (pure PP and PP+10% w/w Talk);
  • Figure 10 is a graph of peel strengths of polypropylene geotextile interleaved with the film layers as shown and compacted at 193 0 C and tested at room temperature;
  • Figure 11 illustrates the peel strengths of polypropylene geotextile interleaved with the film layers as shown and compacted at 193 0 C. Tested at 5O 0 C;
  • Figure 12 illustrates the peel strengths of interleaved with polypropylene geotextile the film layers as shown and compacted at 193 0 C. Tested at 9O 0 C;
  • Figure 13 illustrates the peel strengths of interleaved with polypropylene geotextile the film layers as shown and compacted at 193 0 C. Tested at room temperature;
  • Figure 14 illustrates the peel Strength of samples with 20%, 10% Talc films, 10% Vapour Grown Carbon
  • FIG. 14 illustrates the peel strengths of samples with 20%, 10% Talc films and pure PP films and tested at 20, 50, 90 and 12O 0 C. This figure is a simplification of Figure 14;
  • Figure 16 is a performance graph comparing flat weave geometry samples with no interlayer (1-4) with samples with interlayer (5-8);
  • Figure 17 is an expanded view of the interlayer bond line illustrating the function of the granular material at the join line L;
  • Figure 18 is a schematic representation of an apparatus for manufacturing an improved interlayer sub- article used in the production of some of the tested samples.
  • Figure 19 is a cross-sectional view of an interlayer film having particulate material embedded on each main surface.
  • the weaving lubricant on the surface of the Propex® fabric was found to be inhibiting the peel strength of the compacted material. Washing the lubricant from the surface has been shown to improve the peel strength, although the relatively low amount of lubricant of the newer, Propex® 6060 style polypropylene geotextile did not inhibit an improvement in peel strength, as was observed with the older Propex® geotextiles with a large amount of weaving lubricant on the surface.
  • a compaction temperature of 193 0 C was found to be needed to melt enough of the oriented phase in order to provide enough material at the interface to provide a strong bond between the woven layers.
  • the compacted geotextile with the talc filled interlayer film gave a peel strength of around 6N/mm.
  • the peel mechanisms of the two materials was also different. In the standard Curv® the peel region jumped very quickly into an interlayer region of the compacted material (that is between the fabric layers) whilst for the compacted geotextile with the talc filled interlayer film the peel layer always remained between the steel coupon and the compacted product (that is it stayed in the region of the hot melt adhesive).
  • Nanoclay Obtained from Sigma Aldrich (product code 682632).
  • the base polypropylene tapes used throughout this work were based on those used in the commercially available Propex 6060 style geotextile..
  • VGCF Vapour Grown Carbon Fibre
  • the cloth used was a standard 6060 (60 tapes per 10cm in each direction) woven polypropylene geotextile from Propex Fabrics GmbH. Cloths produced from standard PP base resin and a nucleated PP were used. These cloths had different levels of lubrication coated on the surface of the tapes as part of the weaving process. Three different levels of lubrication were considered -high lubrication, low lubrication (-5% of lubrication on high lube cloths) and washed (spin cycle in washing machine at 4O 0 C). The nucleated material was not washed.
  • a bench top twin screw extruder (Thermo Prism Eurolab 16) was used to compound the fillers into the base resin.
  • the base resin and filler were weighed out to an accuracy of ⁇ 5g.
  • the two materials were then placed in their respective feeders.
  • the extruder was set to a uniform temperature profile of 200 0 C down the barrel.
  • the base resin was fed into the first feed port (the one furthest from the exit die) from a single screw feeder.
  • the filler was fed into the last feed port (the one closest to the exit die) from a twin screw feeder designed to handle powders.
  • a vertical force feeder was used to ensure that the filler was integrated into the polymer melt.
  • the extruder was set to 200 rpm and the feeder rates adjusted so that the extruder ran at 80% of its maximum torque output.
  • the output die was circular with a 3mnn diameter.
  • the resulting strand was hauled off through a water bath and then pelletized, producing a pellet 1 to 2mnn in diameter and 1 mm long.
  • the extruder was run until all the base resin pellets had passed through the extruder (the feeders were set so that the filler was fully incorporated into the resin as fast as possible).
  • the initial mixing produced a master batch with pellets of varying concentration (from 0% w/w to about 25 % w/w).
  • the pellets were hand mixed in a bucket and were then fed back into the extruder (using the same temperature and speed) via the first feed port. This produced a well mixed product which was again hauled off and pelletized.
  • Both pure PP and PP with fillers was blown into a film using Bradford University's custom built small-scale blown film line 10 comprising a materials hopper 12, a heater 14 for melting the material, a ram extruder 16 with a heated barrel 18 and an air cooled ring 20 which blows cooling air onto the extruded material at the point of extrusion and annular die 22 which produced tubes 24 of blown material.
  • the above rig 10 had a single screw extruder with two heating zones Z1 , Z2 along the extruder barrel 18, set to 167 and 200 0 C, and two heated die zones D1 and D2, set to 207 and 204 0 C respectively. Other temperatures may be necessary for other materials.
  • the screw speed was set to 38.6rpm.
  • Both the PP and PP/CNF material was extruded through a 30mm annular die, with a gap of 1 mm. Upon extrusion, the material passed through an air cooled ring cooled by compressed air, which controlled the crystallisation of material as it was blown into a bubble by a second air line 26 (not shown) contained within the annular die 22. The blown film was then held as a tube for ⁇ 0.5m to allow cooling to ambient temperature before haul-off and collection.
  • extruder speed and temperatures, die temperatures, air flow to the cooling ring and air pressure used to blow the film into a tube were all varied in order to allow stable film blowing, yet to maintain the thinnest thickness of film possible.
  • a film suitable for use as an interlayer bonding film was created by taking a 20%w/w talc loaded PP resin and casting it into a film using a film casting rig (not shown).
  • the extruder on the caster was set such that the three heating zones were set to 180, 200 and 21O 0 C, with the adapter and die set to 225 0 C.
  • the extruder speed was set at 40RPM and the haul-off speed was varied to hold the extruded film under no net positive tension. Other concentrations of talk were also used in the production of alternative interlayer material.
  • Hot Compaction was performed on the woven cloths with interleaved films either on a small static press (300mm square), or for later compactions, on a large hydraulic press shown schematically as 30 in figure
  • a brass plate 36 was placed on the bottom plate 34. Onto this was placed a sheet of heat proof rubber 38, and a second brass plate 40. This was covered with a sheet of aluminium foil 42 around 0-1 mm thick.
  • the cloth/film sample 50 comprising multiple layers or cloths of woven oriented fibres and the interlayer shown schematically at 52 respectively was then placed into this assembly with another sheet of aluminium foil 56 and another brass plate 58 placed on top of the sample, and finally a second rubber sheet 60 and large brass plate 62 were placed on top of these plates. Either 4 or 8 layers of fabric/cloth 52 were used with the interlayer film 54 inserted between each layer of fabric 52.
  • each fibre melts such as to allow it to bond with its immediately adjacent neighbour whilst the interlayer melts completely so as to allow the embedded material (talk, chalk, calcium based hydroxyl appetite, carbon nanotubes etc) to be dispersed into the melted material at the junction between the layers of cloth, as shown diagrammatically.
  • the embedded particulate material has a higher melting point than the fibres in surrounding the fabric layers. Hence the temperature applied during the bonding process can be sufficient to melt at least part of the fibres but avoid melting the particulate material. This allows the particles to retain their shape and provide a predetermined surface area for the surrounding melted portions of the fibres to bond to.
  • the melting temperature of the interlayer material is selected to be below that of the oriented fibres in the cloth and is preferably selected to have a peak melting temperature at least 4 degrees or more below that of the oriented fibres as determined by Differential Scanning Calorimetry such as to ensure it is fully melted quickly and well before the central core of the oriented fibres themselves melt.
  • thermocouple 70 The compaction temperature (peak temperature reached during the compaction process) was monitored by inserting a thermocouple 70 into the centre of the compacted sample (between central two layers of woven material. Peel Strength:
  • Peel strength samples were cut from the compacted samples. All peel strength samples were 10mm wide and were opened up at the point where the aluminium foil had been placed during compaction and the ends placed into the grips of an RDP-Howden servo-mechanical tensile testing machine (RDP). The samples were peeled apart at 80mm/min, using the RDP, data-logger and laptop to measure the output load as the peel crack progressed. The peel strength of the sample is defined as the average load over the region where the sample is peeling apart after the initial peak (the initiation peak).
  • the peel tests were performed in an oven mounted onto the RDP.
  • the air temperature of the oven was controlled using a separate heater, and monitored using a thermocouple within the oven close to where the sample was mounted.
  • the samples were allowed to acclimatise for approximately 10 minutes, before peeling in the same manner as described above.
  • Tablei above illustrates the Peel strength of various different hot compacted weave styles, with differing numbers of tapes in the warp and weft of the woven cloth.
  • the standard Propex 6060 material used in the samples described herein is cloth E.
  • Cloth D is a flat woven material (similar to the hand woven material in this study) of the same grade of polymer. Results taken from ref [1]. From table 1 , it is clear that the flat woven material has a much greater peel strength than the crimped type weave of the Propex 6060 geotextile used to make Curv ® (cloth E in Table 1 ), however it much more difficult to weave this type of geotextile.
  • the inter-layer coats the whole surface of the woven layer (since the film melts first during the compaction process), and so this overcomes part of this problem caused by using a crimped weave, since the film allows some of the gaps in the weave structure to be filled completely.
  • Figure 3 shows a comparison between the peel strengths for lab spun PP tapes, Propex PP tapes and washed Propex geotextile fabric compacted with pure PP and PP/CNF films.
  • This figure shows clearly that the three samples with PP films have a similar peel strength, yet the three samples with PP/CNF films show different peel strengths.
  • the peel strengths for PP and PP/CNF films in lab spun PP tapes (left) and Propex PP tapes (centre), both hand woven into a flat weave, are compared to the washed Propex fabric (right).
  • CNF films were used as a direct comparison to Figure 3, discussed later herein. From this figure it will be appreciated that the lab spun tapes of PP significantly outperformed the standard Propex PP Tape and the washed 6060 fabric.
  • the flat, hand woven material shows greater peel strength than that of the standard washed Propex material since, although the whole surface is coated, Figure 4 indicates that it is the interface region between the matrix and tapes phases that controls the peel strength.
  • the flat woven material has a much greater interface region since the whole area of each woven layer can form an interface, whereas the gaps in the crimped weave mean that the interface does not run total along the surface.
  • Figure 4 illustrates the Peel Strength for Various compacted samples with and without VGCF Filler and from which it can be seen that the filled tapes with unfilled film provided the highest peel strength whilst the filled tapes and filled film was close behind.
  • Figure 5 shows the results for hot compacted samples with interleaved films, using the commercial Propex geotextile cloth. These results, excepting a single anomalous result, showed a spread of results in the 7-1 ON/1 Omm range, but no increase with a filled interleaved film layer in the hot compacted product, in direct contrast to the results shown by Carbon Nanofibres in flat woven lab spun polypropylene tapes.
  • a weaving package in particular a lubricant on the surface, is added to the Propex tapes during the commercial weaving process. It was believed that this lubricant acted as a inhibitor to improved bonding during the compaction process, and possibly reduced the amount of fibrillation (leading to energy absorbed) when the woven layers (or woven layer and film layer) were peeled apart. The removal of this lubricant by means of a washing step would, therefore, have beneficial results.
  • Figure 7 shows the peel strength for (nucleated geotextile cloths) and illustrates the peel strengths of hot compacted nucleated polypropylene geotextile cloth with different levels of surface lubricant. Samples were produced with no interleaved film, pure PP (non-nucleated), PP+10%w/w VGCF and PP+10%w/w
  • the key parameter with hot compacted products is the compaction temperature, since this controls the amount of material melted in the tape phase.
  • Re-examining the first results of the 6060 with interleaved films (pure PP) shows the dependence of peel strength with compaction temperature, as illustrated in Figure 8.
  • Figure 9 illustrates the peel Strength measurements for washed Propex geotextile fabric with interleaved films (pure PP and PP+10%w/w talc) plotted against compaction temperature and from which it will be appreciated that the addition of 10% Talc to the interleaved film has a significant advantage in that it raises the peel strength of the samples by in excess of 25%. This increase in peel strength occurs at compaction temperatures that allow for the retention of the structure of the oriented tape (i.e. the compaction can be performed at lower temperatures). This is obviously a significant advantage since we can obtain high peel strengths and retain acceptable mechanical properties.
  • Peel strength at elevated temperatures The peel strength of each of the large plaques produced on the hydraulic press, i.e. the standard Propex material interleaved respectively with 20% Talc film, 10% Talc film, 10% VGCF and pure PP films, and compacted at 193 0 C, were measured at room temperature (2O 0 C), 5O 0 C, 9O 0 C and 12O 0 C. These results are shown in Figures 10-15.
  • Eight layer laminate composed of woven lab spun PP/10%w/w CNF tapes, with interleaved PP/10%w/w CNF films, and compacted at 187.6°C.
  • a crack was initiated in the samples by a thin strip of aluminium foil, and 10mm wide strips were cut from the sample and peeled as previously described. The surfaces of the above samples were then observed in an SEM.
  • Sample 1 showed a smooth surface, with very little sign of damage, corresponding to the low (0.28N/10mm) peel strength measured for this sample.
  • the only features visible on the surface are a number of darker lateral 'lines' across the image corresponding to either the boundaries between tapes, or where a split has occurred in the tape in the direction of molecular orientation.
  • a number of darker 'lines' perpendicular to the lateral lines are also visible, corresponding to the boundaries between tapes (remembering that the surface is a layer of woven PP tapes).
  • no obvious sign of fibrillation can be seen on the surface.
  • Sample 2 showed the similar boundaries between tapes, seen in sample 1 , however also visible are signs of fibrillation from the surface, indicating more damage has occurred, corresponding to the increased measured peel load (4.6N/10mm).
  • the fibrillation generally ran in the direction of the peel (top to bottom of the image), along the direction of orientation in the tapes.
  • Sample 3 showed a dramatic increase in the amount of damage across the surface, reflecting again the increase measured peel load (11.3N/10mm). Intense fibrillation is observed across the entire peel surface, predominantly in the peel direction. Samples 4, 5 and 6 showed similar surface damage on all three samples, reflecting the similar measured peel loads (19, 17 and 19N/10mm). All three showed signs of fibrillation across the surface, but the surfaces are dominated by fracture of the tapes. Large holes in the surface are visible where the tapes have been pulled out from the woven layer by the peeling motion during the test.
  • Figure 16 illustrates the performance advantage well known from earlier work relating simply to the use of interlayer films without any particle or nano-particle additions and is included here simply to establish the starting point for the present invention.
  • figure 17 provides an exploded view of the interlayer portion and particularly illustrates the position of the particulate material.
  • the particulate material may be any material having a higher melting point than the surrounding oriented polymeric material layers so that during the bonding process, the temperature applied can be sufficient to melt at least part of the fibres in the polymeric material, but avoid melting the particulate material. This allows the particles to retain their shape during the bonding process and provides a predetermined surface area for the surrounding oriented polymeric material layers to bond to.
  • Examples of such particulates may include talc, clay, carbon black, Aluminium Oxide, Hydroxyapatite, glass, fly ash, cement powder or carbon nano-tubes. It is thought that there are two strengthening mechanisms which the particles participate in.
  • the particles increase the total surface area exposed to bonding at the interlayer boundary and, secondly, the particles themselves present a physical barrier to the propagation of any split along the join line, shown schematically at 100.
  • the increase in the surface area of contact or bonding can be further enhanced by employing irregular shaped particles (as shown) and it is thought that the irregular nature of the particles provides a further degree of mechanical interaction between the melted polymer material and the particles themselves.
  • it is possible to increase still further the relative surface area of contact by reducing the size of the particles, there being an advantageous ratio between total surface area and volume. In view of this, it is considered appropriate to use a range of particle sizes and to experiment therewith in order to establish the most appropriate size for a given bond strength.
  • the ratio of particle to interlayer polymer may also be varied and, consequently, the percentage values provided herein are provided by way of example only and may be expanded upon as and where appropriate. Still further, it has been found that the thickness of the interlayer polymer material into which the particulate or granular material is embedded does not have a significant affect on the bond strength. It is therefore reasonable to suggest that it is the existence of the particulate or granular material itself which provides the improved bonding. Consequently, it may be appropriate to reduce the thickness of the polymer material to the minimum necessary to hold the particulate in place during the bonding process. Should this approach be adopted the interlayer polymer effectively becomes a simple carrier material which ensures the correct and even distribution of particulate or granular material.
  • the particulate or granular material may be deposited between the layers to be compacted in any one of a number of ways, including spraying, shaking or spreading onto a lower layer prior to the bonding step. Additionally, the particulate or granular material may be spread onto a first lower layer prior to the deposition of an interlayer of lower melt temperature polymer which is itself then coated with particulate or granular material before a further, upper, layer of fabric is deposited thereover. Subsequent compaction will drive the particulate into both the interlayer and the upper and lower layers adjacent thereto.
  • the peel strength of the hot compacted products has been directly related to the amount of surface area in direct contact from each layer, which allows an interface between layers to be created during compaction.
  • a compaction temperature of approximately 193 0 C is required with a 20% w/w Talc film. At room temperature the measured peel strength was 19.6 ⁇ 0.8 NhOmm.
  • the base polypropylene (PP) used throughout this work is BP 100GA02, which is the standard Curv ® base resin.
  • Talc powder was obtained from Sigma Aldrich and had a particle size described as 325 mesh. This means that 90% of the particles will pass through a sieve with 325 holes per linear inch. This equates to a particle size of less than 44 microns. Discussions with the technical specialist from Sigma indicate that the actual particle size is likely to be between 10 and 20 microns.
  • the cloth used was a standard 6060 (60 tapes per 10cm in each direction) woven polypropylene geotextile from Propex Fabrics GmbH and was composed of the same base PP resin (BP 100GA02).
  • a bench top twin screw extruder (Thermo Prism Eurolab 16) was used to compound the fillers into the base resin.
  • the base resin and filler were weighed out to an accuracy of ⁇ 5g.
  • the two materials were then placed in their respective feeders.
  • the extruder was set to a uniform temperature profile of 200 0 C down the barrel.
  • the base resin was fed into the first feed port (the one furthest from the exit die) from a single screw feeder.
  • the filler was fed into the last feed port (the one closest to the exit die) from a twin screw feeder designed to handle powders.
  • a vertical force feeder was used to ensure that the filler was integrated into the polymer melt.
  • the extruder was set to 200RPM and the feeder rates adjusted so that the extruder ran at 80% of its maximum torque output.
  • the output die was circular with a 3mm diameter.
  • the resulting strand was hauled off through a water bath and then pelletized, producing a pellet 1 to 2mm in diameter and 1 mm long.
  • the extruder was run until all the base resin pellets had passed through the extruder (the feeders were set so that the filler was fully incorporated into the resin as fast as possible).
  • the initial mixing produced a master batch with pellets at a concentration of 20% w/w Talc.
  • the pellets were hand mixed in a bucket and were then fed back into the extruder (using the same temperature and speed) via the first feed port. This produced a well mixed product which was again hauled off and pelletized. Throughout this report filler percentages are quoted as weight percentages (% w/w)
  • Film layers were cast using the cast film line at the University of Bradford.
  • the extruder was set at 185 C, haul-off speed of 5.3m/min and the chill rollers were set to 5 0 C.
  • the cast-line was started with pure PP before the Talc-filled material was fed in.
  • the thickness of the films was measured as shown in Table 3. Table 3. Thickness of pure and Talc-filled PP films produced on cast film line at Bradford University.
  • Hot compaction was performed on the woven cloths of fabric with interleaved films either on a small static press at Leeds University (300mm square), or on a large hydraulic press at Bradford University with ⁇ 600m square platens. Samples produced on the smaller press were 100mm x 100mm, and the samples on the larger press were 300mm x 320mm. Samples were compacted at a pressure of 4.9MPa (700psi) or in the case of a small number of samples, at a pressure of 7MPa (1 OOOpsi).
  • the filler was sprinkled as evenly as possible across the surface.
  • the amount to be sprinkled across the surface was calculated on the basis of 20% w/w for a pure PP film of thickness of 201m (i.e. Propex Fabrics standard PP film). This corresponded to a concentration on the surface of approximately 5g/m 2 . This approximate concentration was then used for all samples where the nanofiller was sprinkled onto the surface of the fabric or film.
  • a small strip of thin aluminium foil ⁇ 2-3cm wide
  • the compaction temperature (peak temperature reached during the compaction process) was monitored by inserting a thermocouple into the centre of the compacted sample (between central two layers of woven material.
  • Peel strength samples were cut from the compacted samples. All peel strength samples were 10mm wide. The samples were opened up at the point where the aluminium foil had been placed during compaction and the ends placed into the grips of an RDP-Howden servo-mechanical tensile testing machine (RDP). The samples were peeled apart at 80mm/min, using the RDP, data-logger and laptop to measure the output load as the peel crack progressed. The peel strength of the sample is defined as the average load over the region where the sample is peeling apart after the initial peak (the initiation peak).
  • the thinner Nordania PP/Talc film did not result in improved peel strength. There are two possible explanations for this. The thinner film did not provide enough extra matrix material to enhance the peel strength and wet the Talc particles completely. More likely is that the PP/Talc film from Nordania was not well mixed, and there were differing concentrations of Talc in the film. It is possible that in this compaction, a Talc rich region of film was used, and so the particle surfaces were again, not completely wetted.
  • the filler particles must be completely wetted in order to achieve good interlayer bonding. If the particles are not wetted, then the particles actually inhibit bonding between the layers, since the melted matrix material from each of the woven layers cannot reach the opposite layer. This means that the filler particles cannot be sprinkled directly onto the fabric surface.
  • the particles are either embedded into a film layer or sprinkled onto a thick film layer in between the fabric layers.
  • film thickness may be important, and also that it is important to obtain an even dispersion of filler throughout the film.
  • an improved process of manufacture and an improved final product may be achieved by employing an interlayer of lower melting temperature material having a selected particulate material either sprinkled onto the surface thereof during the manufacturing process and immediately prior to compaction or embedded in the surface or surfaces.
  • a suitable apparatus 100 for creating such a product is shown in figure 18 which provides an optional heating station 102, a hopper 106 for containing and distributing granular material 108 across the upper surface 104a of a film of material 104 to be used as an interlayer (54 of fig 2) between the woven layers 32, 34 of figure 2.
  • a pair of compaction rollers are provided at 110 and between which the film 104 and granular material passes in a manner such as to push the granular material 108 at least partially into the surface of the film itself such as to embed them therein but present them conveniently at the interface with the woven material 32, 34 to which the interlayer is to be bonded.
  • This positioning of the granular material presents it at the very junction of the materials at which de-lamination is known to occur during the peel tests. It is thought that the improved peel strength is due to the physical barrier the granular material presents to the propagation of a de-lamination and also to the increase in the contact area between the woven material and the granules and the granules and the interlayer.
  • the interlayer is selected to melt at a temperature below that of the woven material and that there should be sufficient interlayer material to ensure the granules are fully wetted or coated in order to ensure optimum bonding. It is also known that the granular material should have a melting temperature above that of the interlayer material and optionally above that of the woven material such as to ensure it remains intact during the heating and bonding process. Still further it is suggested that the granular material is preferably of a type that has a melting temperature considerably above that of both the interlayer material and the woven material such as to ensure it remains in its solid phase during heating and bonding. Examples of such materials would include glass particles, sand and the like.
  • VCF Vapour Grown carbon Fibers

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention porte sur un article polymère formé à partir de brins polymères orientés (52) faits à l'aide d'un procédé de compactage à chaud et dans lequel des couches desdits brins sont disposées l'une au-dessus de l'autre et la liaison entre elles est améliorée par l'inclusion d'une pluralité de particules (108) étalées à travers les surfaces opposées avant liaison. Les particules ont un point de fusion supérieur à celui des brins polymères orientés. Les particules peuvent être incorporées dans une couche polymère (54) avant introduction entre lesdites surfaces.
PCT/GB2009/051202 2008-09-16 2009-09-16 Articles polymères et leur procédé de fabrication WO2010032048A1 (fr)

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GB0816964A GB0816964D0 (en) 2008-09-16 2008-09-16 Process for fabricating polymeric articles
GB0816964.1 2008-09-16
GB0905723A GB0905723D0 (en) 2009-04-02 2009-04-02 Process for fabricating polymeric articles
GB0905723.3 2009-04-02

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Cited By (2)

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JP2013046986A (ja) * 2011-07-26 2013-03-07 Hitachi Chemical Co Ltd 波長変換型太陽電池封止材の製造方法及び太陽電池モジュール
EP3064346A1 (fr) * 2015-03-02 2016-09-07 Gerflor Dalle ou lame electro-conductrice pour la réalisation d'un revêtement de sol

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Publication number Priority date Publication date Assignee Title
EP4223123A1 (fr) * 2022-02-02 2023-08-09 Kraton Polymers Nederland B.V. Substrats antimicrobiens

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FR2124350A1 (fr) * 1971-02-02 1972-09-22 Zito Co
GB2030891A (en) * 1978-08-23 1980-04-16 Atomic Energy Authority Uk Embedding particles in thermoplastic materials
WO1998015397A2 (fr) * 1996-10-04 1998-04-16 University Of Leeds Innovations Limited Polymeres olefiniques
DE19752586A1 (de) * 1997-11-27 1999-06-02 Wickmann Werke Gmbh Verfahren zum Anbringen und/oder Befestigen mindestens einer metallischen Fläche
WO2004103673A2 (fr) * 2003-05-22 2004-12-02 Btg International Limited Prodede pour fabriquer des articles polymeres

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EP0419594B1 (fr) * 1989-02-02 1997-03-26 Chemfab Corporation Procede de fabrication de composites stratifies contenant du ptfe et leurs produits
EP1479498A1 (fr) * 2003-05-22 2004-11-24 Btg International Limited Procédé de fabrication d'articles en matière plastique

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Publication number Priority date Publication date Assignee Title
GB991909A (en) * 1960-05-14 1965-05-12 Ruhrchemie Ag Improvements in or relating to the provision of adhesively bondable surfaces on bodies of thermoplastic synthetic resins
FR2124350A1 (fr) * 1971-02-02 1972-09-22 Zito Co
GB2030891A (en) * 1978-08-23 1980-04-16 Atomic Energy Authority Uk Embedding particles in thermoplastic materials
WO1998015397A2 (fr) * 1996-10-04 1998-04-16 University Of Leeds Innovations Limited Polymeres olefiniques
DE19752586A1 (de) * 1997-11-27 1999-06-02 Wickmann Werke Gmbh Verfahren zum Anbringen und/oder Befestigen mindestens einer metallischen Fläche
WO2004103673A2 (fr) * 2003-05-22 2004-12-02 Btg International Limited Prodede pour fabriquer des articles polymeres

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013046986A (ja) * 2011-07-26 2013-03-07 Hitachi Chemical Co Ltd 波長変換型太陽電池封止材の製造方法及び太陽電池モジュール
EP3064346A1 (fr) * 2015-03-02 2016-09-07 Gerflor Dalle ou lame electro-conductrice pour la réalisation d'un revêtement de sol
FR3033283A1 (fr) * 2015-03-02 2016-09-09 Gerflor Dalle ou lame electro-conductrice pour la realisation d'un revetement de sol
US10129968B2 (en) 2015-03-02 2018-11-13 Gerflor Electro-conducting tile or floorboard floor covering

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