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
  • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
  • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
  • B29C70/28—Shaping operations therefor
  • B29C70/40—Shaping or impregnating by compression not applied
  • B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
• • 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
  • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
  • B29C70/003—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised by the matrix material, e.g. material composition or physical properties
• • 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
  • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
  • B29C70/02—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising combinations of reinforcements, e.g. non-specified reinforcements, fibrous reinforcing inserts and fillers, e.g. particulate fillers, incorporated in matrix material, forming one or more layers and with or without non-reinforced or non-filled layers
  • B29C70/021—Combinations of fibrous reinforcement and non-fibrous material
  • B29C70/025—Combinations of fibrous reinforcement and non-fibrous material with particular filler
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B19/00—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica
  • B32B19/04—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica next to another layer of the same or of a different material
  • B32B19/045—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica next to another layer of the same or of a different material of synthetic resin
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B19/00—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica
  • B32B19/06—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica next to a fibrous or filamentary layer
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
  • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
  • B32B27/26—Layered products comprising a layer of synthetic resin characterised by the use of special additives using curing agents
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  • B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B5/08—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
  • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
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  • C08G59/3227—Compounds containing acyclic nitrogen atoms
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Definitions

• the present disclosure relates generally to fiber-reinforced polymer (FRP) composites having toughening particles therein and method of making such composites.
• FRP fiber-reinforced polymer
• FIG. 1 shows a scanning electron microscope (SEM) image of ground thermoset particles prepared according one example.
• FIG. 2 shows the cross-sectional view of a cured composite laminate, in which distinct interlaminar regions can be seen.
• Fiber-reinforced polymer (FRP) composites have been used as high-strength, low-weight engineering materials to replace metals in aerospace structures such as primary structures of aircrafts. Important properties of such composite materials are high strength, stiffness and reduced weight.
• a cured composite (e.g. prepreg layup) with improved resistance to delamination is one with improved Compression Strength After Impact (CAI) and fracture toughness (G
• CAI Compression Strength After Impact
• C and GMC fracture toughness
• CAI measures the ability of a composite material to tolerate damage.
• the composite material is subject to an impact of a given energy and then loaded in compression. Damage area and dent depth are measured following the impact and prior to the compression test. During this test, the composite material is constrained to ensure that no buckling instability is taking place and the strength of the composite material is recorded.
• Fracture toughness is a property which describes the ability of a material containing a crack to resist fracture, and is one of the most important properties of a material for aerospace applications. Fracture toughness is a quantitative way of expressing a material's resistance to brittle fracture when a crack is present.
• Fracture toughness may be quantified as strain energy release rate (G c ), which is the energy dissipated during fracture per unit of newly created fracture surface area.
• G c includes G
• the subscript“IC” denotes Mode I crack opening, which is formed under a normal tensile stress perpendicular to the crack, and the subscript“IIC” denotes Mode II crack produced by a shear stress acting parallel to the plane of the crack and perpendicular to the crack front. The initiation and growth of a delamination is often determined by examining Mode I and Mode II fracture toughness.
• CAI performance of fiber-reinforced polymer composites may be improved through two main technologies.
• the first technology involves the use of high-strength reinforcing fibers that have relatively high strain to failure. These fibers appear to absorb a high amount of energy without fracturing thereby redistributing the energy over a larger area of the composite laminate.
• CAI performance of fiber- re info reed polymer composites as well as interlaminar toughness may be improved by incorporating certain toughening particles into the interlaminar regions of a multilayer composite laminate.
• The“interlaminar region” refers to the region between two adjacent structural layers of reinforcement fibers in the composite laminate. The presence of toughening particles in the composite laminate creates a resin rich interlayer which helps to contain the crack propagation in this interlayer region.
• thermoplastic particles such as polyamide (PA) have been incorporated into the interlaminar regions of composite laminates to improve CAI.
• the “interlaminar region” refers to the region between adjacent layers of reinforcing fibres in a multi-layered composite laminate.
• polyamide-based thermoplastic particles can either suffer from low melting points (Tm) especially those polyamides with long aliphatic chains, or be prohibitively hygroscopic such as those polyamides with short aliphatic chains.
• Amorphous thermoplastic particles such as amorphous PA or PI can suffer from poor solvent resistance.
• CTE coefficient of thermal expansion
• thermoset particles as interlaminar toughening particles for increasing the damage tolerance and fracture toughness of fiber- reinforced polymer composites. More specifically, the particles contain chemical functional groups which can react with the thermosettable resin matrix in which they are dispersed to form covalent bonds during curing of the resin matrix.
• the chemically active particles are derived from partially curing a thermosettable resin composition past its gel point so as to achieve“solid-like” properties, followed by grinding to obtain the particle size desired. Due to partial curing, there are unreacted or non-crosslinked functional groups on the particle surface. The particles are sufficiently crosslinked past the gel point of the resin composition to maintain the particle integrity upon curing of the composite laminate in which the particles are embedded and to ensure the formation of a distinct interlaminar region.
• thermosettable resin composition is formulated such that the ratio of thermoset resin(s) and curing agent(s) in the curable resin composition is adjusted so that the composition contains a non-stoichiometric ratio of thermoset resin(s) and curing agent(s), i.e. a deficiency or an excess in the amount of curing agent(s) that is necessary for reacting with 100% of the thermoset resin(s), and consequently, due to this deficiency or excess, there will be unreacted or non-crosslinked functional groups from thermoset resin or curing agent at the end of a full curing cycle. After full curing, the cured resin is then ground to obtain particles with chemically active functional groups on the particle surface.
• a non-stoichiometric ratio of thermoset resin(s) and curing agent(s) i.e. a deficiency or an excess in the amount of curing agent(s) that is necessary for reacting with 100% of the thermoset resin(s), and consequently, due to this deficiency
• the resulting chemically active thermoset particle is composed of crosslinked thermoset resin or thermoset polymer and chemically-active functional groups capable of forming covalent bonds.
• the particles are formed from a thermosettable resin composition containing epoxy resin(s)
• the resulting chemically active thermoset particle is composed of crosslinked polyepoxides and non-crosslinked functional groups.
• the partially cured particles may be formed from the same or substantially the same curable resin composition that is used to form the matrix resin of the fiber-reinforced composite material, e.g. prepreg.
• the term“substantially the same” means more than 50% of the composition is the same.
• some of the matrix resin to be used for forming the composite material may be set aside for partial curing and grinding to form the chemically active particles.
• the partially cured particles are then incorporated into the composite laminate at the interlaminar regions. In this way, the CTE of the particles would be an exact match to that of the surrounding resin matrix, thus eliminating stresses and micro cracking in the cured composite laminates.
• the particles are made of the same or similar material as the matrix resin, interfacial bonding between the particles and the surrounding matrix resin after curing is strong.
• thermoset particles As disclosed herein is a departure from the conventional methods used in the aerospace industry, in which thermoplastic or crosslinked thermoplastic toughening particles with dissimilar chemistries from the surrounding matrix resin are used as interlaminar toughening particles.
• thermoset particles disclosed herein are not swellable during curing as in the case of the crosslinked thermoplastic particles disclosed in US Patent No. 8,846,818 and US Patent No. 9,567,426.
• the swellable crosslinked thermoplastic particles disclosed in the patents are crosslinked, are derived from a composition composed mostly of
• thermoplastic polymers and do not typically have reactive functional groups remaining on the particles’ surfaces.
• the swellable particles are not very reactive with the surrounding epoxy-based matrix of the composite in which the particles are dispersed.
• cure and“curing” as used herein encompass cross-linking of resin precursors or polymers brought about by mixing of based components, heating at elevated temperatures, exposure to ultraviolet light and radiation.
• Fully cured refers to 100% degree of cure.
• Partially cured refers to less than 100% degree of cure.
• the partially cured particles are formed from a curable resin composition, which has been cured to a degree of cure of less than 100%, for example, within the range of 50%- 99% of full cure, including 55%-95%, 50%-86%, 50%-87%, 50%-88%, 50%-89%, 55%-86%, 60%-86%.
• the curable resin composition contains one or more thermoset resins, at least one curing agent, and optional additives such as thermoplastic polymers, elastomeric materials, conductive particulates, inorganic fillers, etc.
• the material At the degree of cure of 50% or higher, the material’s thermomechanical properties are significantly altered and the material possesses “solid-like” properties.
• thermal curing is carried out past the gel point of the resin composition.
• gel point may be defined as the crossover point between the G’ and G” curves derived from rheology analysis during a cure cycle.
• G’ represents the elastic modulus
• G” represents the viscous modulus.
• the degree of cure of a thermoset resin system can be determined by Differential Scanning Calorimetry (DSC).
• DSC Differential Scanning Calorimetry
• a thermoset resin system undergoes an irreversible chemical reaction during curing.
• heat is evolved by the resin, which is monitored by the DSC instrument.
• the heat of cure may be used to determine the percent cure of the resin material. As an example, the following simple calculation can provide this information:
• the particles are formed from a thermosettable resin composition containing epoxy resin(s) and an amine compound as curing agent, the resulting chemically active thermoset particle is composed of crosslinked polyepoxides, non- crosslinked epoxy functional groups and unreacted amine groups.
• the ratio of thermoset resin(s) and curing agent(s) in the curable resin composition is adjusted so that the composition contains either a deficiency or an excess in the amount of curing agent(s) that is necessary for reacting with 100% of the thermoset resin(s), and consequently, due to this deficiency or excess, there will be unreacted or non-crosslinked functional groups from thermoset resin material at the end of a pre determined curing cycle.
• an X amount of a curing agent is needed to achieve 100% degree of cure in a predetermined curing cycle, less than X amount may be used in the resin composition to achieve chemically active particles, e.g., up to 90% X, including 50%-80% X or 60%-70%.
• an X amount of a curing agent is needed to achieve 100% degree of cure in a predetermined curing cycle, more than X amount may be used in the resin composition to achieve chemically active particles, e.g., at least 110% X, including 120%- 150% X or 130%- 140%.
• the simplified Carothers equation is a way to predict the amount of conversion (extent of reaction) needed to reach the gel point for a given epoxy or other thermoset resin with functionality, e.g. 2, 3, 4, etc., when reacted with a curing agent with given functionality, e.g. 2, 3, 4, etc.
• n infinity.
• the cured material Upon full curing of the resin composition, the cured material contains unreacted/ noncrosslinked functional groups, which is the source of chemically-active functional groups capable of forming covalent bonds.
• unreacted/ noncrosslinked functional groups which is the source of chemically-active functional groups capable of forming covalent bonds.
• the resulting cured particles contain unreacted/ noncrosslinked epoxy functional groups.
• the resulting cured particles contain unreacted amine groups.
• the particles are formed from a thermosettable resin composition containing epoxy resin(s) and an amine compound as curing agent and there is a deficiency in the amine compounds, the resulting chemically active thermoset particle is composed of crosslinked polyepoxides and non-crosslinked epoxy functional groups due to the excess amount of epoxy resin(s).
• the chemically active particles may have a mean particle size (d50) of less than about 100 pm, for example, 10-70 pm, 15-50 pm , or 15-30 pm, or 20-25 pm.
• the mean particle sizes as disclosed herein can be measured by a laser diffraction technique, for example, using Malvern Mastersizer 2000 which operates in the 0.002 nanometer - 2000 micron range.
• d50 represents the median of the particle size distribution, or alternatively is the value on the distribution such that 50% of the particles have a particle size of this value or less.
• thermoset resins for forming the particles include, but are not limited to, epoxies, phenolics, phenols, cyanate esters, bismaleimides, benzoxazines, polybenzoxazines, polybenzoxazones, combinations thereof and precursors thereof.
• polyepoxides having a plurality of epoxide functional groups per molecule.
• the polyepoxides may be saturated, unsaturated, cyclic, or acyclic, aliphatic, aromatic, or heterocyclic polyepoxide compounds.
• suitable polyepoxides include the polyglycidyl ethers, which are prepared by reaction of epichlorohydrin or epibromohydrin with a polyphenol in the presence of alkali.
• Suitable polyphenols therefore are, for example, resorcinol, pyrocatechol, hydroquinone, bisphenol A (bis(4-hydroxyphenyl)-2, 2-propane), bisphenol F (bis(4-hydroxyphenyl)methane), fluorine 4,4’-dihydroxy benzophenone, bisphenol Z (4,4’-cyclohexylidenebisphenol) and 1 ,5- hyroxynaphthalene.
• Other suitable polyphenols as the basis for the polyglycidyl ethers are the known condensation products of phenol and formaldehyde or acetaldehyde of the novolac resin-type.
• suitable epoxy resins include diglycidyl ethers of bisphenol A or bisphenol F, e.g. EPONTM 828 (liquid epoxy resin), D.E.R. 331 , D.E.R. 661 (solid epoxy resins) available from Dow Chemical Co.; triglycidyl ethers of aminophenol, e.g. ARALDITE® MY 0510, MY 0500, MY 0600, MY 0610 from Huntsman Corp..
• EPONTM 828 liquid epoxy resin
• D.E.R. 331 D.E.R. 661
• triglycidyl ethers of aminophenol e.g. ARALDITE® MY 0510, MY 0500, MY 0600, MY 0610 from Huntsman Corp.
• Additional examples include phenol-based novolac epoxy resins, commercially available as DEN 428, DEN 431 , DEN 438, DEN 439, and DEN 485 from Dow Chemical Co; cresol-based novolac epoxy resins commercially available as ECN 1235, ECN 1273, and ECN 1299 from Ciba-Geigy Corp.; hydrocarbon novolac epoxy resins commercially available as TACTIX ® 71756, TACTIX ®556, and TACTIX ®756 from Huntsman Corp..
• the curing agents for the curable resin composition may be selected from known curing agents, for example, aromatic or aliphatic amines, or guanidine derivatives.
• An aromatic amine curing agent is preferred, preferably an aromatic amine having at least two amino groups per molecule, and particularly preferable are diaminodiphenyl sulphones, for instance where the amino groups are in the meta- or in the para-positions with respect to the sulphone group.
• DDS 3,3'- and 4,4'-diaminodiphenylsulphone
• methylenedianiline bis(4-amino-3,5-dimethylphenyl)-1 ,4-diisopropylbenzene; bis(4- aminophenyl)-1 , 4-diisopropylbenzene; 4,4’methylenebis-(2,6-diethyl)-aniline (MDEA from Lonza); 4,4’methylenebis-(3-chloro, 2,6-diethyl)-aniline (MCDEA from Lonza);
• Suitable curing agents also include anhydrides, particularly polycarboxylic anhydrides, such as nadic anhydride, methylnadic anhydride, phthalic anhydride,
• the curing agent(s) may be present at a stoichiometry such that there is sufficient amount of reactive groups from the curing agent to react with the reactive groups of the thermoset resin(s), for example, one (1) mole of amine curing agent per mole of epoxy resin.
• the stoichiometry is such that there is insufficient amount of reactive groups from the curing agent to react with the reactive groups of the thermoset resin(s), for example, 0.5 to 0.9 mole of amine curing agent per mole of the epoxy resin.
• the stoichiometry is such that there is an excess amount of reactive groups from the curing agent to react with the reactive groups of the thermoset resin(s), for example, 1.1 to 1.5 mole of amine curing agent per mole of the epoxy resin.
• the optional additives that may be incorporated into the curable resin composition include thermoplastic polymers, elastomers, and combination thereof.
• Thermoplastic polymers may be selected from: polyamides; polyetherimides (PEI); polysulphones, including polyethersulfones (PES), polyetherethersulfones (PEES); polyphenylene oxide (PPO);
• Elastomers may be selected from: rubbers such as amine- terminated butadiene acrylonitrile (ATBN), carboxyl-terminated butadiene acrylonitrile (CTBN), carboxyl-terminated butadiene (CTB); fluorocarbon elastomers, styrene-butadiene polymers.
• the amount of thermoplastic polymer and/or elastomer is less than 40% by weight so the particle retains its thermoset characteristics, for example, 5% - 35% % of thermoplastic polymer, based on the total weight of the resin composition.
• Conductive materials in particulate form may also be added to the curable resin composition to impart through thickness electrical conductivity, also known as Z-conductivity, to the final composite laminate.
• suitable conductive materials include metals in the form of flakes or particles such as silver, gold, nickel, copper, aluminum, and alloys thereof, carbon powder, carbon-based nano-sized materials, such as carbon nano-tubes (single-wall nano tubes or multi-wall nano tubes), carbon nano-fibers.
• the term“nano-sized materials” as used herein, refers to materials having at least one dimension smaller than about 0.1 micrometer ( ⁇ 100 nanometers).
• Carbon nano-tubes are tubular, strand-like structures having external diameters in the range of about 0.4 nm to about 100 nm, for example, the external diameter may be less than about 50 nm or less than about 25 nm, and an aspect ratio from 100: 1 up to 5000: 1.
• the nano-fibers may have diameters ranging from 70 nm to 200 nm and a length in the range of 50-200 microns.
• the amount of conductive materials is less than 10% by weight, for example, 1 % -4%, based on the total weight of the resin composition.
• Flame retardant additives may also be added to the curable resin composition to impart increased flame retardancy to the final composite laminate.
• the Strujtol Polydis product range commercialized by Schill+Seilacher are commercially available flame retardant will be obvious to those skilled in the art.
• the particles are formed from a curable resin composition containing: (a) one or more multifunctional epoxy resin(s); (b) at least one amine curing agent; and (c) a thermoplastic or elastomeric toughening agent.
• the amounts of the components (a)-(c) may be as follows: (a) 100 parts; (b) 5 to 70 parts; (c) 5 to 50 parts.
• the resin composition further includes conductive particles such as carbon nanotubes (CNT), carbon powder, metallic particles, and combinations thereof.
• conductive particles such as carbon nanotubes (CNT), carbon powder, metallic particles, and combinations thereof.
• the amount of conductive particles is up to 10% by weight based on the total weight of the resin composition, for example, 1 %-10%, 2%-5%.
• thermoset particles of the present disclosure may be formed by other processes capable of producing such particles.
• the chemically active particles of the present disclosure may be used as interlaminar particles between layers of reinforcement fibers of a composite laminate, i.e., the particles are located in the interlaminar region of the composite laminate.
• The“interlaminar region” refers to the region between adjacent layers of reinforcing fibres in a multi-layered composite laminate.
• the chemically active particles are dispersed in the interlaminar region formed between adjacent layers of reinforcing fibers at a content of about 2% to about 20% by weight based on the total weight of the matrix resin contained in the composite laminate, including about 5% to about 15%, and about 8% to about 12%.
• a composite laminate containing interlaminar particles may be manufactured using different processes.
• the particles are deposited onto the surface of a prepreg ply prior to laying up multiple prepreg plies together to form a stack or“prepreg layup”.
• the prepreg plies within the layup may be positioned in a selected orientation with respect to one another, e.g. 0°, ⁇ 45°, 90°, etc.
• the particles remain in the interlaminar regions of the laminate.
• the prepreg layup are consolidated and cured under heat and pressure to achieve the required fiber volume fraction with a minimum of voids.
• the particles may be deposited onto the prepreg via any conventional techniques such as sprinkling, electrostatic deposition, scatter coating, spray distribution, and any other technique known by a person skilled in the art.
• the distributed composite particles adhere to the surface of the prepreg due to the tackiness of the matrix resin.
• specific amounts of particles are mixed with a curable resin composition prior to the prepreg manufacturing.
• resin films are manufactured first by coating a particle-containing resin mixture onto a release paper. Then, the resulting resin film is laminated onto a layer of fibres, e.g., unidirectional fibers, under the aid of heat and pressure to impregnate the fibres, thereby forming a prepreg ply with specific fibre areal weight and resin content.
• the particles are filtered out and remain external to the fibre layer due to the fact that the size of the particles is larger than the spacing between the fibres. Subsequently, when two layers of prepregs containing particles are laid up one on top of the other, the particles are positioned in the interlaminar regions of the prepreg layup.
• a curable resin composition without particles is coated onto a release paper to form a resin film, which is then brought into contact with one or both opposing surfaces of an un-impregnated fibre layer.
• the resin impregnates the fibres and leaves a little or no resin on the external surfaces of the fibre layer.
• a second film of curable resin containing the particles is brought into contact with an outer surface of the resin-impregnated fibre layer.
• An additional film of curable resin containing the particles may be brought into contact with the opposite outer surface of the resin-impregnated fibre layer to form a sandwich structure.
• a particle-rich resin layer remains outside of the impregnated fibre layer and does not further impregnate the fibres.
• a plurality of such structures are laminated together to form a composite structure with particles in the interlaminar regions.
• two films of curable resin composition without particles are brought into contact with the two opposing surfaces of an un-impregnated fibre layer.
• the resin impregnates the fibres and leaves little or no resin on the external surfaces of the fibre layer.
• two films of curable resin containing particles are brought into contact with the opposing surfaces of the pre-impregnated fibres layer.
• a plurality of such structures are laminated together to form a composite structure with particles in the interlaminar regions.
• Such approach is preferred as it tends to provide a well-ordered laminate resulted from the particles not disrupting the placement of the fibres.
• the term“prepreg” refers to a layer of fibrous material (in the form unidirectional fibers, nonwoven mat, or fabric ply) that has been impregnated or infused with a curable matrix resin.
• the term“impregnate” as used in this disclosure refers to the introduction of a curable resin to reinforcement fibers so as to partially or fully encapsulate the fibers with the matrix resin.
• the matrix resin of the prepreg may have the same composition as or is similar in composition to that of the chemically active particles.
• the thermoset resins, curing agents and additives disclosed previously in reference to the particles also apply to the prepreg’s matrix resin.
• the fiber reinforcement material may be in the form of a woven or nonwoven fabric ply, or unidirectional tape composed of unidirectional fibers.
• “Unidirectional fibers” refers to a layer of reinforcement fibers, which are aligned in the same direction.
• the prepreg plies within the layup may be positioned in a selected orientation with respect to one another, e.g. 0°, ⁇ 45°, 90°, etc.
• the reinforcement fibers in the composite laminates and prepregs may take the form of chopped fibers, continuous fibers, filaments, tows, bundles, sheets, plies, and combinations thereof.
• Continuous fibers may further adopt any of unidirectional (aligned in one direction), multi-directional (aligned in different directions), non-woven, woven, knitted, stitched, wound, and braided configurations, as well as swirl mat, felt mat, and chopped mat structures.
• Woven fiber structures may comprise a plurality of woven tows, each tow composed of a plurality of filaments, e.g. thousands of filaments.
• the tows may be held in position by cross-tow stitches, weft-insertion knitting stitches, or a small amount of resin binder, such as a thermoplastic resin.
• the fiber materials include, but are not limited to, glass (including Electrical or E- glass), carbon, graphite, aramid, polyamide, high-modulus polyethylene (PE), polyester, poly- p-phenylene-benzoxazole (PBO), boron, quartz, basalt, ceramic, and combinations thereof.
• the reinforcing fibers have a tensile strength of greater than 3500 MPa ((per ASTM D4018 test method).
• Resin U was prepared by mixing the epoxy precursors Araldite® MY0510 and Araldite® PY306 at a temperature ranging between 60°C and 90°C.
• Araldite® MY0510 is a triglycidyl p-aminophenol
• Araldite® PY306 is a diglycidyl ether of bisphenol-F, both from Huntsman Advanced Materials Inc. Sumikaexcel 5003P, a polyethersulphone from
• the resin U so produced was then filmed to a nominal aerial weight of 23.4 gsm (gram per square meter) on a release paper.
• Intermediate modulus carbon fibres were spread in a conventional prepreg machine to form a fiber web of unidirectional fibers with a nominal aerial weight of 190 gsm.
• the formed fiber web was then sandwiched between two films of resin U to obtain a prepreg U with a nominal fiber areal weight (FAW) of 190 gsm, and a nominal resin content of 19.8% by weight.
• FAW nominal fiber areal weight
• Each resin composition in Table 2 was prepared by mixing the epoxy precursors Araldite® MY0510 and Araldite® PY306 at a temperature ranging between 60°C and 90°C.
• Sumikaexcel 5003P polyethersulphone
• Aradur® 9664-1 (4,4’-DDS) and the live thermoset resin particles (LRTP) were then added and mixed at a temperature ranging between 60°C and 90°C.
• Each resin composition P so produced was then filmed to a nominal areal weight of 23.4 gsm onto a release paper.
• the prepreg U formed as described above was sandwiched between two resin films formed from the particle-containing resin composition P to obtain a prepreg P having a nominal fibre areal weight (FAW) of 190 gsm and a total nominal resin content of 33% by weight.
• FAW nominal fibre areal weight
• the different toughening particles that were used are labelled as VP-0X0, PK- OXO, NT-0C0 in Table 2. These three toughening particles were prepared using the resin formulations shown in Table 3.
• the resins VP-OXO, PK-OXO, NT-OXO were prepared by mixing the epoxy precursors Tactix123 and Araldite® PY306 at a temperature ranging between 60°C and 90°C.
• Tactix123 is a diglycidyl ether of bisphenol-A from Huntsman Advanced Materials Inc.
• VP-OXO Resin VP3619 and Aradur® 9664-1 were then added and mixed at a temperature ranging between 70°C and 90°C.
• Struktol VP3619 is nitrile rubber modified epoxy prepolymer based on diglycidyl ether of bisphenol-A from Schill+Seilacher.
• PK-OXO Resin PKHB100, a polyhydroxyether (i.e., phenoxy resin) from InChem, was added to the epoxy mixture and then dissolved at a temperature ranging between 110°C and 130°C. The aromatic amine curing agent Aradur 9664-1 (4,4’-DDS) was then added and mixed at a temperature ranging between 60°C and 90°C.
• NT-0C0 Resin The multi-wall carbon nanotubes were pre-dispersed in a Tactix123/PY306 blend. The aromatic amine curing agent Aradur 9664-1 (4,4’-DDS) was then added and mixed at a temperature ranging between 60°C and 90°C.
• the three different particles (VP-0X0, RK-0C0, NT-0C0) were prepared by partially curing the three resins VP-0X0, RK-0C0, NT-0C0 by heating them at 2°C/min to 180C and cooling them down immediately after reaching 180°C.
• the resulting partially cured resins were granulated prior to be milled with an ACM classifier mill from Hosokawa.
• DSC Differential scanning calorimetry
• FIG. 1 is a scanning electron microscope (SEM) image of the ground particle PK- 0X0 disclosed in Table 4.
• a plurality of prepregs P was laid up to form a composite laminate.
• the laminate was enclosed in a conventional zero-bleed, sealed vacuum bag and cured in an autoclave for 2 hours at 180°C under a pressure of 85 psi (586 kPa or kilopascals) while maintaining the vacuum throughout the cure cycle.
• FIG. 2 shows the cross-sectional of the cured composite laminate, in which distinct interlaminar regions can be seen.

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