WO2011048340A2 - Empilement multiaxial solidarise par des soudures ponctuelles realisees grace a des voiles thermoplastiques intercalaires - Google Patents
Empilement multiaxial solidarise par des soudures ponctuelles realisees grace a des voiles thermoplastiques intercalaires Download PDFInfo
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- WO2011048340A2 WO2011048340A2 PCT/FR2010/052248 FR2010052248W WO2011048340A2 WO 2011048340 A2 WO2011048340 A2 WO 2011048340A2 FR 2010052248 W FR2010052248 W FR 2010052248W WO 2011048340 A2 WO2011048340 A2 WO 2011048340A2
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- stack
- unidirectional
- web
- stack according
- webs
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- 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
- B32B5/00—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
- B32B5/02—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
- B32B5/022—Non-woven fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
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- 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
- B29C70/06—Fibrous reinforcements only
- B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
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- 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
- B29C70/06—Fibrous reinforcements only
- B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
- B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
- B29C70/22—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in at least two directions forming a two dimensional structure
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- 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
- B32B5/00—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
- B32B5/02—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
- B32B5/12—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 characterised by the relative arrangement of fibres or filaments of different layers, e.g. the fibres or filaments being parallel or perpendicular to each other
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- 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
- B32B5/00—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
- B32B5/22—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 the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—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 the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—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 the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/05—Interconnection of layers the layers not being connected over the whole surface, e.g. discontinuous connection or patterned connection
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
- D04H1/498—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres entanglement of layered webs
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/559—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving the fibres being within layered webs
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H13/00—Other non-woven fabrics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2101/00—Use of unspecified macromolecular compounds as moulding material
- B29K2101/12—Thermoplastic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
- B29K2105/08—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts of continuous length, e.g. cords, rovings, mats, fabrics, strands or yarns
- B29K2105/0854—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts of continuous length, e.g. cords, rovings, mats, fabrics, strands or yarns in the form of a non-woven mat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2707/00—Use of elements other than metals for preformed parts, e.g. for inserts
- B29K2707/04—Carbon
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- 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
- B32B2250/00—Layers arrangement
- B32B2250/20—All layers being fibrous or filamentary
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- 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
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
- B32B2260/023—Two or more layers
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- 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
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
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- 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
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0261—Polyamide fibres
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- 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
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/106—Carbon fibres, e.g. graphite fibres
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24058—Structurally defined web or sheet [e.g., overall dimension, etc.] including grain, strips, or filamentary elements in respective layers or components in angular relation
- Y10T428/24124—Fibers
Definitions
- the present invention relates to the technical field of reinforcing materials, suitable for the constitution of composite parts. More specifically, the invention relates to a new multiaxial stack for the production of composite parts, by injection or subsequent infusion of thermosetting resin, and its manufacturing process.
- a direct process is defined by the fact that one or more fibrous reinforcements are implemented in the "dry” state (that is to say without the final matrix), the resin or matrix, being implemented separately , for example by injection into the mold containing the fibrous reinforcements ("RTM” process, of the English “Resin Transfer Molding"), by infusion through the thickness of the fibrous reinforcements ("LRI” process, of the English “Liquid Resin Infusion” or “RFI” process, or by manual coating or impregnation by roller or brush, on each of the unitary layers of fibrous reinforcement, applied successively on the form.
- preforms are made of reinforcement material, mainly carbon fibers, especially of the unidirectional type.
- the resin which is subsequently associated, in particular by injection or infusion, with the unidirectional reinforcement layers during the production of the part may be a thermosetting resin, for example of the epoxy type.
- this resin is, in most cases, very fluid.
- the major disadvantage of this type of resin is their fragility, after polymerization / crosslinking, resulting in low impact resistance of the composite parts made.
- multiaxial stacks are often used comprising unidirectional layers extending in different directions. Most often, these unidirectional sheets are bonded together by sewing or knitting.
- the document EP 1 348 791 describes a combination of unidirectional carbon plies in which the yarns are oriented parallel to each other, the bond between the plies being made by means of thermoplastic binding yarns which are aligned and spaced apart from each other. other.
- one of the objectives of the present invention is to propose a new type of multiaxial stack that can lead to final composite parts that combine good mechanical properties, and a lack of microcracking observed in the case where stitched or knitted stacks are used.
- Another object of the invention is to provide a multiaxial stack that can be produced at an interesting cost.
- Another object of the invention is to provide a multiaxial stack which has good drapability and manipulability.
- the present invention proposes a new stack of fibrous materials comprising at least two layers of unidirectional carbon fibers, each extending in different directions, in which each of the unidirectional sheets is bonded to at least one of its facing an adjacent web of thermoplastic fibers, and wherein at least one web is present between two consecutive unidirectional webs characterized in that the connection between each unidirectional web and each web adjacent thereto is provided by the web, by spot welds leading to a discontinuous overall weld and in that these spot welds also ensure the cohesion of the stack.
- the present invention also relates to a method of manufacturing a stack according to one of the preceding claims, characterized in that it comprises the following steps:
- the unidirectional sheets are made in line, without their own cohesion, before binding to the veil, they are conferred.
- the transverse connection, at each point weld, of all the layers and veils constituting the stack is carried out simultaneously.
- spot welds are made by thermocompression.
- spot welds are made by operating perforations over the entire thickness of the stack, each spot weld being, in particular, made around the perforations.
- Figure 1 is a schematic perspective view partially broken away of a stack according to Example 1.
- Figure 2 is a schematic top view of a stack according to the invention wherein, in the plane of the stack, spot welds are discontinuous lines.
- Figure 3 is a top view of a stack according to the invention in which, in the plane of the stack, spot welds are continuous lines.
- Figure 4A is a schematic top view of a stack according to the invention wherein, in the plane of the stack, spot welds are points in the form of disks.
- Figure 4B is a schematic top view of a stack according to the invention wherein, in the plane of the stack, spot welds are points in the form of rings.
- Figure 5 is another schematic top view of a stack according to the invention wherein, in the plane of the stack, spot welds are discontinuous lines.
- Figs. 6A and 6B are each a perspective view of an exemplary puncturing means.
- Figure 7 is a partial view of a device incorporating a series of in-line perforating means.
- Figures 8 and 9 show the mechanical data obtained for the stack of Example 1, compared to a corresponding stitched stack (comparative example).
- connection between the different unidirectional layers constituting the stack is provided through the thermoplastic nature of the sails. Welds are carried out hot, thanks to the various sails: the interlayers, called internal sails, located between two consecutive unidirectional sheets and those or one located (s) periphery and constituting an outer face of the stack, named (s) veil (s) external (s).
- the interlayers called internal sails
- the various unidirectional sheets (UD) and sails is not provided by a seam or knitting, which has the advantages mentioned above.
- the stack according to the invention consists exclusively of unidirectional sheets of carbon fibers and webs of thermoplastic fibers. It is possible to position two sails, see more, between two consecutive unidirectional sheets. But according to a preferred embodiment of the invention 1, a single web 1 is located between two consecutive unidirectional carbon fiber plies 2, in the stack I. According to an embodiment of the invention which corresponds to that of FIG. Stacking corresponds to a concatenation (web / UD) n , UD designating a unidirectional web and n designating an integer and all the webs present in the stack are of identical weight.
- the stack corresponds to a concatenation (sail / UD) n / sail, UD denoting a unidirectional sheet and n denoting an integer, the external sails having a grammage equal to half-weight of each of the internal veils.
- n is a function of the number of folds present in the stack and will, for example, be in the range from 2 to 32.
- the term "unidirectional sheet of carbon fibers” means a sheet consisting exclusively or almost exclusively of carbon fibers deposited parallel to one another.
- the unidirectional carbon fiber plies can be made in line.
- the threads necessary for the constitution of the web are then unwound from coils and arranged, so as to extend parallel to each other, in a contiguous manner, on a conveyor belt, possibly carrying a veil, him -Even possibly superimposed with one or more unidirectional web / tablecloth sequences.
- each layer of unidirectional carbon fibers has no inherent cohesion, before being bonded to the webs of thermoplastic fibers.
- each unidirectional web is formed by passing a yarn around pegs carried by two parallel endless chains, so that the portions of yarns freely extending between the pegs are parallel. between them.
- Unidirectional webs are formed by guiding the respective yarns in different directions and are bonded together by stitching.
- each unidirectional sheet of carbon fibers has a clean cohesion, before being bonded to the webs of thermoplastic fibers.
- This cohesion can, for example, be obtained by needling, by the presence of thermoplastic bonding yarns which cross, without interlacing, the fibers of the unidirectional sheet and providing a connection by gluing, or by the presence of weft threads forming a fabric unidirectional. It is, for example, possible to use a commercial unidirectional web whose cohesion and manipulability will be, for example, provided by binding yarns, by mechanical bonding by weaving, or by chemical bonding because of the polymeric nature. binding threads.
- the unidirectional web before being secured to the (s) sail (s), will offer, preferably, a total coverage, with a factor opening of 0%.
- Such plies are, for example, marketed by SIGMATEX UK Limited, Runcom Cheshire WA7 1TE, United Kingdom under the references PW-BUD (ex: product no. PC2780600 200GSM / PW-BUD / T700SC 12K 50C / 0600mm), or by the company OXEON AB, Sweden, under TEXERO references.
- thermoplastic type including polyamides, copolyamides, polyesters, copolyesters, block copolymers ester ester / ether, polyacetals, polyolefins, thermoplastic polyurethanes, phenoxy, to facilitate handling, if necessary the tablecloth, before its association with veils of thermoplastic fibers.
- binding yarns will most often extend transversely to the carbon fibers.
- unidirectional web also includes unidirectional fabrics, in which spaced apart weft yarns interleave the carbon fibers which extend parallel to one another and form the warp yarns of the unidirectional fabric.
- the carbon fibers parallel to each other represent at least 95% by weight of the web, which is therefore described as "unidirectional" .
- the unidirectional sheet comprises no weft yarn from interweaving the carbon fibers, so as to avoid any undulation.
- the unidirectional webs used in the context of the invention are neither woven, sewn nor knitted.
- the carbon threads are preferably non-associated with a polymeric binder and thus called dry, that is to say that they are not impregnated, coated or associated with any binder. polymeric before their association with thermoplastic sails.
- Carbon fibers are, however, most often characterized by a standard mass content of sizing which can represent at most 2% of their mass.
- a method for producing unidirectional sheets can also be implemented.
- a method of producing a multiaxial fibrous sheet comprising the steps of superimposing several unidirectional sheets in different directions, and binding the superimposed sheets together, in which, to make at least one of the sheets unidirectionally, at least one cable is spread so as to obtain a sheet of substantially uniform thickness, having a width at least equal to 5 cm and a basis weight at most equal to 300 g / m 2 and the unidirectional layer is given a cohesion allowing to be manipulated prior to its superposition with at least one other unidirectional layer.
- each unidirectional sheet of carbon fibers has a basis weight of 100 to 280 g / m 2 .
- This grammage range makes it easy for design engineers to correctly size composite structures by adapting the stacking sequences of different layers, depending on the different mechanical stress modes of the composite structures.
- a carbon weight of a weaker elementary layer will offer all the more versatility in the choice of different stacks possible constant thickness.
- the carbon fibers are most often in the form of yarns of at least 1000 filaments, and in particular from 3000 to 50,000 filaments, for example 3K, 6K, 12K or 24K filaments.
- the carbon threads have a title of between 60 and 3800 Tex, and preferably between 400 and 900 tex.
- the thicknesses of the unidirectional carbon layer vary between 90 and 270 ⁇ .
- Veil means a nonwoven of continuous or short fibers.
- the constituent fibers of the nonwoven will have average diameters in the range of 0.5 and 70 ⁇ m.
- the fibers will have, for example, a length of between 1 and 100 mm.
- the fibers constituting the web are advantageously made of a thermoplastic material, in particular chosen from polyamides (PA: PA6, PA12, PAA, PA6.6, PA 6.10, PA 6.12, ...), copolyamides (CoPA), polyamides - block ether or ester (PEBAX, PEBA), polyphthalamide (PPA), Polyesters (Polyethylene terephthalate-PET-, Polybutylene terephthalate-PBT -%), Copolyesters (CoPE), thermoplastic polyurethanes (TPU), polyacetals (POM ...), Polyolefins (PP, HDPE, LDPE, LLDPE ....) / Polyethersulfones (PES), polysulfones (PSU %), polyphenylenesulfones (PPSU %), Polyetheretherketones (PEEK), PolyetherKetoneKetone (PEKK), Poly (Phenyl Sulfide) (PPS), or
- the thickness of the sails before their association with the unidirectional sheet is very close to their thickness within the consolidated stack.
- the thickness of the various sails before association can be determined by the NF EN ISO 9073-2 standard by using method A with a test area of 2827 mm 2 (disc of 60 mm diameter) and an applied pressure of 0, 5 kPa.
- each of the webs has, for example, a thickness of 0.5 to 50 microns, preferably 3 to 35 microns. Such a thickness contributes in particular to achieve a high fiber volume ratio when the stack is used to form a composite part, in particular of a large thickness, by the vacuum infusion technique.
- each of the sails has a weight per unit area in the range from 0.2 to 20 g / m 2 .
- the unidirectional layers present are arranged so as to be oriented in two directions different.
- Stacking can be called multiaxial. All unidirectional sheets may have different directions or only some of them, the others may have identical directions. In the case where several sheets will have identical directions, it will not be two consecutive sheets. Otherwise, the unidirectional layers will preferably have identical characteristics.
- Preferred orientations are most often, those making an angle of 0 °, + 45 ° or - 45 ° (also corresponding to + 135 °), and + 90 ° with the main axis of the part to be made.
- the 0 ° corresponds to the axis of the machine to perform the stack, that is to say the axis that corresponds to the direction of advancement of the stack during its design.
- the main axis of the part which is the largest axis of the part is generally confused with the 0 °. It is, for example, possible to produce quasi-isotropic, symmetrical or oriented stacks by choosing the orientation of the folds.
- quasi-isotropic stacking mention may be made of the stack at the angles 45707135790 °, or 90 135 ° 45 °.
- symmetrical stacking mention may be made of 079070 ° or 45 ° / 135745 °.
- the most commonly used fold numbers are 8, 16, 24 and 32 plies, which may, for example, be multiples of the aforementioned 4-ply quasi-isotropic stacks.
- the stack that is to say the set of sails and UD, is not secured by stitching or knitting, but by a weld made thanks to the thermoplastic nature of the sails present within the stack.
- a heating / cooling operation is performed on only certain areas of the surface of the stack.
- This heating can be carried out conventionally by a resistance heating means or by means of ultrasound means.
- the heating causes the melting or at least the softening of the different sails.
- Such a connection using the thermoplastic nature of the sails is advantageous because it makes it possible to avoid all the disadvantages represented by the presence of sewing or knitting threads, such as in particular the problems of waviness, microcracking, the reduction of the mechanical properties at the level of the composite parts subsequently obtained ...
- connection implemented corresponds to a discontinuous welding, as opposed to a continuous welding obtained by a thermocompression carried out on the entire surface of the stack.
- the surface of the set of point welds represents, for example, from 0.1 to 40%, preferably from 0.5 to 15% of the surface of the sheet. unidirectional.
- a discontinuous weld has an advantage in terms of energy and also for the drapability of the stack during the production of subsequent composite parts. Spot welds leading to a discontinuous overall weld are present.
- point is used, in the context of the description, to designate individual welds belonging to a set of welds and therefore includes welds of different shapes.
- the spot welds may especially be in the form of discontinuous lines 10 as shown in FIG. 2 or continuous as illustrated in FIG. that is to say, extending over the entire width of the unidirectional sheet, of points of different shapes, in particular circular shapes as illustrated in FIG. 4A under the reference 20 or of the prism type, rings as illustrated in FIG. 4B under reference number 30.
- These spot welds are distributed over the surface of the stack to ensure its cohesion and ensure a connection between the unidirectional sheets and the webs over the entire thickness of the stack. Such a link may in particular be transverse.
- Suitable heating means thermally or ultrasonically, especially in the form of one or more heating rods in the case of connecting lines or heating punches in the case of connection points, the geometry of the contact points with the stack will be adapted to the shape of the desired point links, may be used.
- Such heating means may be brought to a temperature of 190 to 220 ° C and supported on the stack with a pressure of 10 to 50 kPa, for example from 0.1 to 2s, preferably from 0.5 to 1s.
- these values are purely illustrative and will depend in particular on the number of plies and the thermoplastic material constituting the sails.
- weld points can be made regularly and are preferably distributed over straight lines extending in one or two directions, with in particular a spacing pitch in the range of 4 to 50 mm and a distance between two parallel lines in the range of 10 to 100 mm.
- the welds, from one line parallel to the other, may be aligned as shown in FIG. 4A or offset, in particular by half a step as illustrated in FIG. 4B, which illustrates the case where the weld points have a ring shape.
- Such welding points may, for example, have a larger dimension, measured parallel to the surface of the stack, in the range of 2 to 100 mm.
- the implementation of welding points will be preferred, in the case where the unidirectional sheets will have a clean cohesion before their association with the sails.
- the surface of the set of spot welds represents, for example, from 0.1 to 30%, preferably 0.5 at 5% of the surface of the unidirectional layer.
- the spot welds areas represent a global surface corresponding to 1 to 40%, preferably 5 to 15% of the total area of the unidirectional tablecloth.
- spot welds in the form of lines will preferably be used because they will more easily make it possible to ensure the connection of all the son of the unidirectional layers and to give its cohesion and handling to the stack.
- the spot welds correspond to continuous weld lines parallel to each other.
- the continuous weld lines may, for example, be spaced from each other by 10 to 50 mm.
- the spot welds correspond to discontinuous weld lines.
- Discontinuous welding lines for example, have a length of 10 to 100 mm.
- the discontinuous weld lines may be distributed over parallel lines, being shifted relative to each other from one line to the other, as shown in FIG. 2.
- the discontinuous solder lines may, for example, be spaced from each other by 5 to 50 mm.
- the type of weld lines, continuous or discontinuous they may, for example have a width of 20 to 200 mm. All dimensions given above are of course in the plane of the stack, that is to say in the plane of each of the unidirectional layers.
- the welds may extend along continuous lines across the entire width of the material
- the direction of the lines will then be chosen to extend in a direction parallel with none of the orientations of the unidirectional layers.
- discontinuous lines as illustrated in FIGS. 2 and 5 which are each a top view of a stack I according to the invention on which discontinuous solder lines bearing the reference 10, 2 and the references 40 and 50 in FIG. 5 are made so that each wire of each of the unidirectional layers present in the stack regularly encounters a weld, for example at least one weld every 100 mm. preferably at least one weld every 10 mm.
- welds 40 and 50 with separate heating rods or with a welding means corresponding to a splined bar for performing in a welding operation two weld lines 40 and 50, or more.
- directions for the non-parallel discontinuous weld lines at all directions of the fibers of the unidirectional sheets, or only some of them in the case where several series of discontinuous weld lines are present are preferred.
- these different welding modes using continuous or discontinuous welding lines can also be used when the unidirectional layers have a prior self-cohesion, in this case the orientation of the weld lines is less important and these may be more spaced.
- the perforations present on the stack have, for example, a larger dimension, measured parallel to the surface of the folds, located in the range of 1 to 10 mm.
- the perforations may be made with any suitable perforation means, for example needle, picot or other type. Heating is performed around the perforating means, so as to obtain the desired connection between the folds, which also makes it possible to freeze the perforation. There is then a melting of the veil around the perforation means which after cooling leads to a kind of eyelet around the perforation.
- the heating means is directly integrated with the perforating means so that the perforating means is itself heated.
- the perforation means 100 it is advantageous for the perforation means 100 to have a shoulder 110 as shown in FIG. 6A on which the stack can come into abutment during the perforation, which will make it possible to tighten the folds between them during the connection.
- This shoulder is itself heated and allows to heat the sails, while pressing on the assembly to be welded, and on a larger area surrounding the perforation.
- the spot welds may be related to rings 30, as illustrated schematically in FIG. 4B, which surround each perforation 31.
- FIG. 5B shows another heating / perforation means 200 used in the case where the welds are in the form of discontinuous lines.
- a heating bar 200 for producing discontinuous solder lines is equipped with two needles 210 making it possible to make two perforations by discontinuous line.
- the pressure exerted during the perforation is similar to that described for heating alone and belongs, for example, to the range 20 to 40 kPa, and is in particular exerted for a period of 1.1 to 2 seconds, in particular 0.5 at ls. This pressure is chosen so as to maintain a substantially constant thickness, at any point of the stack.
- thermosetting type a resin or matrix, of thermosetting type, will subsequently be added to the stack, for example by injection into the mold containing it ("RTM” process, of the English Resin Transfer Molding). , or by infusion (through the thickness of the folds: process "LRI”, of the English Liquid Resin Infusion or process "RFI”, of the English Resin Film Infusion).
- RTM injection into the mold containing it
- LRI thickness of the folds
- RFI Liquid Resin Infusion
- RFI the English Resin Film Infusion
- the matrix used is, most often, thermosetting type.
- the injected resin will be, for example, chosen from the following thermosetting polymers: epoxides, unsaturated polyesters, vinyl esters, phenolics, polyimides and bismaleimides.
- the composite part is then obtained after a heat treatment step.
- the composite part is generally obtained by a conventional consolidation cycle of the polymers in question, by performing a heat treatment, recommended by the suppliers of these polymers, and known to those skilled in the art.
- This consolidation step of the desired part is carried out by polymerization / crosslinking according to a cycle defined in temperature and under pressure, followed by cooling.
- the pressure applied during the treatment cycle is low in the case of vacuum infusion and stronger in the case of injection into a RTM mold.
- the composite parts obtained have a fiber volume content of 57 to 63%, preferably 59 to 61%, even when they have a large thickness, especially greater than 10 mm and / or when they are performed according to a method by injection at a pressure below atmospheric pressure, especially less than 1 bar and preferably between 0.1 and 1 bar.
- These volume levels of fibers are compatible with the use of structures for primary parts, that is to say, critical parts in aeronautics that take up the mechanical forces (fuselage, wing ).
- the fiber volume ratio (FVT) of a composite part is calculated from the measurement of the thickness of a composite part by knowing the surface density of the unidirectional carbon layer and the properties of the carbon fiber, from the following equation:
- e plate is the thickness of the plate in mm
- Pfibre carbon is the density of carbon fiber in g / cm 3 .
- the surface mass UD carbon is in g / m 2 .
- the composite parts obtained also have optimal mechanical properties, and in particular the impact resistance (CAI, Compression After Impact), the mechanical properties showing the sensitivity to the holes such as perforated compression (OHC, Open Hole Compression in English), the perforated traction (OHT, Open Hole Traction in English), the matting (Bearing in English), the shear in the plane (IPS, In-Plane Shear in English).
- CAI compressive impact rupture stress
- the opening factors can be measured according to the following method.
- the device consists of a SONY brand camera (model SSC-DC58AP), equipped with a lOx lens, and a Waldmann brand light table, model W LP3 NR, 101381 230V 50HZ 2xl5W.
- the sample to be measured is placed on the light cover, the camera is fixed on a bracket, and positioned at 29cm of the sample, then the sharpness is adjusted.
- the measurement width is determined according to the fibrous material to be analyzed, using the ring (zoom), and a rule: 10cm for open fibrous materials (OF> 2%), 1,17cm for materials fibrous little open (OF ⁇ 2%).
- the brightness is adjusted to obtain a value of OF corresponding to that given on the control plate.
- the Videomet contrast measuring software from Scion Image (Scion Corporation, USA) is used. After image capture, the image is processed as follows: Using a tool, we define a maximum area corresponding to the selected calibration, for example for 10cm-70 holes, and having a number whole pattern. An elementary surface is then selected in the textile sense of the term, that is to say a surface which describes the geometry of the fibrous material by repetition.
- the percentage OF is defined per hundred which is subtracted the black surface divided by the elementary surface is 100- (black surface / elementary surface).
- the brightness adjustment is important because diffusion phenomena can change the apparent size of the holes and therefore the OF. An intermediate brightness will be retained, so that no phenomenon of saturation or diffusion too important is visible.
- Example 1 Multiaxial quasi-isotropic welded by line
- a next stack is made online on a multiaxial manufacturing machine: a unidirectional carbon fiber web oriented at 45 °, a web, a unidirectional sheet of carbon fiber oriented at 135 °, a web.
- the unidirectional sheets of carbon fibers are made in line and their basis weight in carbon fibers is estimated at 268 g / m 2 ⁇ 3% from Hexcel HR fibers whose properties are shown in Table 1.
- Short fiber webs based on polyamides are used.
- the characteristics of the sails used are shown in Table 2.
- the melting point indicated in Table 2 is determined by differential scanning calorimetry (DSC) according to ISO 11357-3.
- the mass per unit area is measured according to ISO 3801.
- the rate of Porosity shown in Table 2 is calculated from the following formula:
- Welding lines 50mm apart are made in the 90 ° orientation with respect to the axis of the machine.
- the welding is performed by a V-shaped heating bar with a radius of curvature at the support of 4mm.
- the heating bar is heated to 200 ° C and a pressure of 30 kPa is applied for 0.8s.
- This bar is actuated so that the contact surface comes to compress the folds evenly, so as to form weld lines as shown in Figure 3.
- the stack as illustrated in Figure 1 below is made online on a multiaxial manufacturing machine: a unidirectional carbon fiber web oriented at 45 °, a web, a unidirectional sheet of carbon fiber oriented at 0 °, a sail, a unidirectional carbon fiber web oriented at 135 °, a web, a unidirectional carbon fiber web oriented at 90 ° and a web.
- the unidirectional sheets of carbon fibers are made in line and their basis weight in carbon fibers is estimated at 194 g / m 2 ⁇ 3% from Hexcel IM fibers, the properties of which are shown in Table 5.
- Table 5 Characteristic Properties of Carbon Fibers
- the sails are identical to those used in Example 1.
- Two series of discontinuous weld lines are made one series in the 90 ° orientation and another in the 135 ° orientation with respect to the axis of the machine, so as to alternate each weld line oriented at 90 ° with a weld line oriented at 135 ° as shown in FIG. 5.
- a splined heating bar for performing in one operation a set of welds 40 and 50 is used. It should be noted that a slight overlap between the discontinuous lines 50 of the same line and between two successive lines 40, is performed to ensure the connection of all the son deposited in the four orientations mentioned above.
- This welding can ideally be combined with perforation, using heating / perforating means as illustrated in Figure 6B.
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- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Laminated Bodies (AREA)
- Nonwoven Fabrics (AREA)
- Reinforced Plastic Materials (AREA)
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Abstract
Description
Claims
Priority Applications (9)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US13/503,032 US9475254B2 (en) | 2009-10-23 | 2010-10-21 | Multiaxial stack rigidly connected by means of weld points applied by means of inserted thermoplastic webs |
CA2774921A CA2774921C (fr) | 2009-10-23 | 2010-10-21 | Empilement multiaxial solidarise par des soudures ponctuelles realisees grace a des voiles thermoplastiques intercalaires |
JP2012534752A JP5868861B2 (ja) | 2009-10-23 | 2010-10-21 | 挿入された熱可塑性ウェブにより適用された接合点により剛性連結された多軸積層体 |
ES10785485.3T ES2616254T3 (es) | 2009-10-23 | 2010-10-21 | Apilamiento multiaxial unido mediante soldaduras puntuales realizadas usando bandas termoplásticas intercaladas |
RU2012121138/12A RU2549955C2 (ru) | 2009-10-23 | 2010-10-21 | Многоосная укладка, скрепленная точечной сваркой, полученной с помощью вставных термопластичных тонких нетканых материалов |
CN201080047746.8A CN102575401B (zh) | 2009-10-23 | 2010-10-21 | 通过插入热塑性网施加的焊点牢固连接的多向层叠体 |
AU2010309642A AU2010309642B2 (en) | 2009-10-23 | 2010-10-21 | Multiaxial stack rigidly connected by means of weld points applied by means of inserted thermoplastic webs |
BR112012007359-1A BR112012007359B1 (pt) | 2009-10-23 | 2010-10-21 | Pilha multiaxial rigidamente ligada por pontos de solda produzidos por meio de tramas termosplásticas intercaladas. |
EP10785485.3A EP2491175B1 (fr) | 2009-10-23 | 2010-10-21 | Empilement multiaxial solidarisé par des soudures ponctuelles réalisées grace à des voiles thermoplastiques intercalaires |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FR0957452A FR2951664B1 (fr) | 2009-10-23 | 2009-10-23 | Empilement multiaxial solidarise par des soudures ponctuelles realisees grace a des voiles thermoplastiques intercalaires |
FR0957452 | 2009-10-23 |
Publications (2)
Publication Number | Publication Date |
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WO2011048340A2 true WO2011048340A2 (fr) | 2011-04-28 |
WO2011048340A3 WO2011048340A3 (fr) | 2011-07-07 |
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PCT/FR2010/052248 WO2011048340A2 (fr) | 2009-10-23 | 2010-10-21 | Empilement multiaxial solidarise par des soudures ponctuelles realisees grace a des voiles thermoplastiques intercalaires |
Country Status (11)
Country | Link |
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US (1) | US9475254B2 (fr) |
EP (1) | EP2491175B1 (fr) |
JP (1) | JP5868861B2 (fr) |
CN (1) | CN102575401B (fr) |
AU (1) | AU2010309642B2 (fr) |
BR (1) | BR112012007359B1 (fr) |
CA (1) | CA2774921C (fr) |
ES (1) | ES2616254T3 (fr) |
FR (1) | FR2951664B1 (fr) |
RU (1) | RU2549955C2 (fr) |
WO (1) | WO2011048340A2 (fr) |
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JP2015536261A (ja) * | 2012-11-19 | 2015-12-21 | ヘクセル ランフォルセマン | 中間材料を貼り付けてそれらの接着を確実にする方法、複合体成分及び中間材料の製造を意図するスタックを形成する方法 |
FR3073774A1 (fr) * | 2017-11-22 | 2019-05-24 | Hexcel Reinforcements | Materiau de renfort comprenant une couche poreuse en un polymere thermoplastique partiellement reticule et procedes associes |
WO2020225019A1 (fr) * | 2019-05-09 | 2020-11-12 | Teijin Carbon Europe Gmbh | Matelas multi-axial comprenant une couche intermédiaire discontinue |
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WO2021214410A1 (fr) | 2020-04-22 | 2021-10-28 | Hexcel Reinforcements | Élément composite intermédiaire, procédé de fabrication et pièce composite |
FR3118723A1 (fr) | 2021-01-14 | 2022-07-15 | Hexcel Reinforcements | Procédés et dispositifs de formage de matériaux composites |
WO2022189744A1 (fr) | 2021-03-11 | 2022-09-15 | Hexcel Reinforcements | Nouveaux matériaux de renfort à base de fils torsadés s et z, adaptés à la constitution de pièces composites, procédés et utilisation |
WO2023067282A1 (fr) | 2021-10-21 | 2023-04-27 | Hexcel Reinforcements | Materiau de renfort comprenant une couche poreuse en un polymere thermoplastique reactif et procedes associes |
FR3128398A1 (fr) | 2021-10-21 | 2023-04-28 | Hexcel Reinforcements | Matériau de renfort comprenant une couche poreuse en un polymère thermoplastique réactif et procédés associés |
FR3128399A1 (fr) | 2021-10-21 | 2023-04-28 | Hexcel Reinforcements | Procédé de fabrication de pièces composites à partir d’un matériau de renfort comprenant une couche poreuse en un polymère thermoplastique réactif et d’une résine thermodurcissable |
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FR2962933B1 (fr) | 2010-07-22 | 2012-09-14 | Hexcel Reinforcements | Nouveau materiau intermediaire de renfort constitue d'un ensemble de fils voiles espaces |
FR3002928B1 (fr) * | 2013-03-08 | 2015-05-01 | Hexcel Reinforcements | Procede et machine d'etalement d'une nappe textile de type tissu et tissus obtenus |
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WO2018099910A1 (fr) | 2016-11-29 | 2018-06-07 | Advanced Materials Design & Manufacturing Limited | Procédé de fabrication de textiles hybrides (en fibres-nanofibres) par l'intermédiaire de liaisons efficaces de fibres à nanofibres comprenant de nouveaux mécanismes de transfert de charge efficaces |
US11904591B2 (en) * | 2018-09-04 | 2024-02-20 | Kai-Hsi Tseng | Composite material for footwear |
US20230391680A1 (en) * | 2022-06-03 | 2023-12-07 | Raytheon Technologies Corporation | Preform tapered hole press for improved cvi-cmc microstructure |
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Also Published As
Publication number | Publication date |
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AU2010309642A1 (en) | 2012-04-26 |
FR2951664B1 (fr) | 2011-12-16 |
EP2491175B1 (fr) | 2016-11-23 |
ES2616254T3 (es) | 2017-06-12 |
RU2549955C2 (ru) | 2015-05-10 |
CA2774921C (fr) | 2017-12-12 |
FR2951664A1 (fr) | 2011-04-29 |
CN102575401B (zh) | 2015-03-04 |
JP5868861B2 (ja) | 2016-02-24 |
AU2010309642B2 (en) | 2013-06-27 |
BR112012007359A2 (pt) | 2016-10-04 |
EP2491175A2 (fr) | 2012-08-29 |
CA2774921A1 (fr) | 2011-04-28 |
CN102575401A (zh) | 2012-07-11 |
WO2011048340A3 (fr) | 2011-07-07 |
US20120202004A1 (en) | 2012-08-09 |
BR112012007359B1 (pt) | 2020-03-10 |
US9475254B2 (en) | 2016-10-25 |
RU2012121138A (ru) | 2013-11-27 |
JP2013508192A (ja) | 2013-03-07 |
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