WO2012174623A1 - Matière de support, mélange à mouler en feuille et procédé permettant de réaliser une matière à mouler - Google Patents

Matière de support, mélange à mouler en feuille et procédé permettant de réaliser une matière à mouler Download PDF

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Publication number
WO2012174623A1
WO2012174623A1 PCT/BR2012/000197 BR2012000197W WO2012174623A1 WO 2012174623 A1 WO2012174623 A1 WO 2012174623A1 BR 2012000197 W BR2012000197 W BR 2012000197W WO 2012174623 A1 WO2012174623 A1 WO 2012174623A1
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WO
WIPO (PCT)
Prior art keywords
moulding
substrate
support
resin
compound
Prior art date
Application number
PCT/BR2012/000197
Other languages
English (en)
Inventor
Chris Harrington
Denis Granger
Edmundo Ortiz
Original Assignee
Hexcel Composites Limited
Hexcel Composites Sasu
Hexcel Brasil Serviços Ltda
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
Application filed by Hexcel Composites Limited, Hexcel Composites Sasu, Hexcel Brasil Serviços Ltda filed Critical Hexcel Composites Limited
Priority to DE112012002551.2T priority Critical patent/DE112012002551T5/de
Priority to GB1400165.5A priority patent/GB2507672A/en
Publication of WO2012174623A1 publication Critical patent/WO2012174623A1/fr

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Classifications

    • 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
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • 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
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • 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
    • B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
    • B29C43/30—Making multilayered or multicoloured articles
    • B29C43/305—Making multilayered 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
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • 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
    • B29C70/08—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers
    • B29C70/086—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers and with one or more layers of pure plastics material, e.g. foam layers
    • 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
    • B29C70/08—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers
    • B29C70/088—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers and with one or more layers of non-plastics material or non-specified material, e.g. supports
    • 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
    • B29C70/46—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs
    • 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
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/14—Layered products comprising a layer of metal 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
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C09J163/04—Epoxynovolacs
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/26—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer which influences the bonding during the lamination process, e.g. release layers or pressure equalising layers
    • B32B2037/268—Release layers
    • 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
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0076—Curing, vulcanising, cross-linking
    • 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
    • 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
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • 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
    • B32B2305/00—Condition, form or state of the layers or laminate
    • B32B2305/07—Parts immersed or impregnated in a matrix
    • 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
    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/30—Iron, e.g. steel

Definitions

  • the present invention relates to a moulding material, particularly but not exclusively to a support material for use with a formable material, a use of a support material, a sheet moulding compound and a moulding process.
  • Composite moulding materials generally comprise a reinforcement material which is commonly a fibrous material and a resin material. Traditionally, these moulding materials are laid up in one or more layers in a mould to form a composite structure moulding which is subsequently cured to form a product or an article.
  • the resin material may be a thermoset- ting plastic, also known as a thermoset or a thermoplastic.
  • a thermoset is a polymer material that irreversibly cures.
  • the traditional lay up is time consuming and labour intensive.
  • the conditions need to be controlled to ensure that properties of the moulding can be controlled.
  • the material can usually cure at ambient temperatures ranging typically from -200C to 300C, but the time for the material to proceed to full cure at these temperatures is long, typically ranging from an hour to several days or even weeks or months. This is undesirable for the commercial manufacture of composite moulded products. Therefore, the cure reactions are enhanced to decrease the moulding time by increasing the energy of the material through heating (generally above 40 °C), or irradiation such as electron beam processing.
  • the curing reaction for thermoset materials is an exotherm reaction.
  • the energy input is typically staged into two or more stages. If the energy input is in the form of heating to increase the temperature of the moulding, then typically in the first stage of processing, the temperature is increased over time to a desired first level and held constant for a time period (known as the dwell stage or dwell period). Following on from the first dwell period, the temperature is further increased to a second level and held constant over time (second dwell stage). The temperature increase and subsequent dwell may be further repeated depending on the properties of the moulding.
  • mouldings In addition, the processing of mouldings is generally complicated and requires a lot of expertise and equipment to control the energy input or temperature of the moulding during curing. Often, in addition to heating and temperature control equipment, the moulding is also pressurized to ensure adequate wetting out of the reinforcement material by the resin mate- rial.
  • the present invention aims to obviate or at least mitigate the above described problems and/or to provide improvements generally.
  • a support material to reinforce a formable material comprising a moulding material, said moulding material comprising a fibrous reinforcement material and a reinforcement resin material.
  • the resin material may at least partially or fully impregnate the fibrous reinforcement material to form a semi-prepreg or prepreg respectively.
  • the resin material may be conjoined to the surface of the fibrous material.
  • the support material preferably further comprises an adhesive or adhesive layer.
  • the adhesive layer is adapted to adhere the moulding material to the formable material.
  • the adhesive material improves the bond between the support or moulding material and the substrate material. This is particularly important for metal substrate materials such as steel or aluminium. These materials may comprise an oxidized surface or a surface comprising contaminants such as a lubricant which renders the direct bonding of the moulding material to the surface of the substrate material more difficult.
  • the adhesive material preferably electrically insulates the substrate material from the moulding material. This is particularly important for metal substrate materials in combination with carbon fiber reinforcement mate- rial as the adhesive layer prevents galvanic coupling which could otherwise result in corrosion of the substrate.
  • the adhesive layer extends beyond the support material to prevent the edges of the support material from being in contact with the substrate. This is particularly relevant around apertures in the support material which correspond with aper- tures in the substrate.
  • the support material may comprise a release material for releasing the support material from a mould surface.
  • the formable material comprises a substrate material, the sub- strate material being cold mouldable and/or thermoformable.
  • the substrate material may be a thermoplastic or a metal.
  • a moulding process comprising a) providing a substrate material; b) providing a support material comprising a moulding material comprising a resin material and a fibrous reinforcement material; locating said substrate ma- terial and said support material in relation to a mould; and forming the substrate and curing said support material to bond the moulding material to the substrate.
  • the mould may comprise a first portion and a second portion, the first portion being heated. The heated first por- tion is in contact with the substrate material. This is particularly advantageous for a metal substrate material as this provides good heat conductivity to heat up and cure the support material in the forming and curing step of the process.
  • moulding materials improve the mechanical properties of the support materials.
  • Preferred support materials or substrate materials are thermoformable materials such as thermoplastics, or cold formable materials such as metal.
  • the substrate material and the moulding material are provided in the form of a sheet moulding compound comprising a substrate material having conjoined thereto the support material.
  • the support material may comprise an adhesive ma- terial.
  • the sheet moulding compound may further comprise an adhesive for bonding the moulding material to the substrate material.
  • moulding materials comprise a reinforcement material and a resin material.
  • the moulding material is cured to form a moulded article.
  • the curing proc- ess transforms the resin from a plastic substance by a cross-linking process.
  • Energy and/or catalysts are added that cause the molecular chains to react at chemically active sites linking into a rigid, 3-D structure.
  • the crosslinking process forms a molecule with a larger molecular weight, resulting in a material with a higher melting point.
  • the molecular weight increases to a point so that the melting point is higher than the surrounding ambient temperature, and the material forms into a solid material. Uncontrolled reheating of the material results in reaching the decomposition temperature before the melting point is obtained. Therefore, a thermoset material cannot be melted and reshaped after it is cured.
  • the moulding material may be in the form of a support material for reinforcing a formable substrate material.
  • the support material may comprise a moulding material, said moulding material comprising a fibrous reinforcement material and a reinforcement resin material.
  • the resin material may be conjoined to the surface of the fibrous reinforcement material.
  • the moulding material further comprises an adhesive for adhering the moulding material to the formable or substrate material.
  • the adhesive improves the bond between the moulding material and the substrate material.
  • the moulding material comprises at least one reinforcement layer comprising said fibrous reinforcement and said reinforcement resin and an adhesive layer.
  • the substrate material may be cold mouldable and/or thermoformable.
  • a cold mouldable substrate material is a material which may be moulded, shaped or formed without increasing the temperature of the substrate material prior to moulding, shaping or forming.
  • a thermoformable substrate material is a material which may be moulded, shaped or formed by increasing the temperature of the substrate.
  • the substrate material may be a thermoplastic (which is thermomouldable) or a metal (which is cold mouldable).
  • the moulding material may comprise a resin material conjoined to the surface of the reinforcement material.
  • the resin material may at least partially impregnate the reinforcement material.
  • the substrate material and the moulding material are provided in the form of a sheet moulding compound comprising a substrate material having conjoined thereto a moulding material comprising a resin material conjoined to the surface of the fibrous reinforcement material; followed by locating the sheet moulding compound in a mould; and forming the substrate and curing the resin material.
  • the sheet moulding compound preferably further comprises an adhesive for bonding the moulding material to the substrate material.
  • the moulding material may further comprise a release material for releasing the moulding material from a mould surface.
  • Suitable release materials may comprise polyolefin film materials.
  • the polyolefin film material may comprise multiple layers of varying polyolefin polymers ranging from C2 (polyethylene) through to C6, and/or copolymers thereof.
  • Other suitable release material may comprise fluorinated thermoplastic films (such as polytetrafluoroethylene (PTFE), fluorinated ethylene propylene (FEP), ethylene tetrafiuoroethylene (ETFE), polyvinyl fluoride (PVF), chlorinated thermoplastic films such as polyvinylchloride (PVC), low surface energy thermoplastic films (such as polymethylpentene PMP), thermoplastic films chemically modi- fied to have low surface energy (such as siloxane treated polyethylene terephthalate (PET), thin metal foils (such as Aluminium), pre-cured thermoset fibre reinforced laminates, films of low melting temperature waxes (such as paraffin wax) or synthetic waxes (such as substituted amide waxes) or salts of
  • a preferred release film material is Hostaphan PET film material as supplied by Mitsubishi Plastics Inc.
  • the release film may be removable from the thermoformed part or the film may remain on the cured part.
  • Suitable adhesive materials may be applied in film form, as a paste, or sprayed and could be selected from the group consisting of thermoset resins such as epoxy, cyanate ester, and phenolic resins or from groups consisting of thermoplastic bonding adhesives such as polyurethane, polyvinylacetate (PVA) and PVC.
  • thermoset resins such as epoxy, cyanate ester, and phenolic resins
  • thermoplastic bonding adhesives such as polyurethane, polyvinylacetate (PVA) and PVC.
  • Suitable epoxy resins include diglycidyl ethers of bisphenol A, diglycidyl ethers of bisphenol F, epoxy novolac resins and N-glycidyl ethers, glycidyl esters, aliphatic and cycloaliphatic glycidyl ethers, glycidyl ethers of amino- phenols, glycidyl ethers of any substituted phenols and blends thereof. Also included are modified blends of the aforementioned thermosetting polymers.
  • These polymers are typically modified by rubber or thermoplastic addition such as carboxy terminated butyl rubber (CTBN/RAM) combinations where the olefinic nature of the modifier enhances enables the ability of the adhesive to absorb oil from a substrate surface and form a better bond.
  • CBN/RAM carboxy terminated butyl rubber
  • These polymers are often further modified by a surfactant or adhesion promoting chemical.
  • Any suitable catalyst may be used. The catalyst will be selected to correspond to the resin used.
  • One suitable catalyst for use with an epoxy resin is a dicyandiamide curing agent. The catalyst may be accelerated. Where a dicyandiamide catalyst is used, a substituted urea may be used as an accelerator.
  • Suitable accelerators include Diuron, Monuron, Fenuron, Chlortolu- ron, bis-urea of toluenediisocyanate and other substituted homologues.
  • the epoxy curing agent may be selected from Dapsone (DDS), Diamino-diphenyl methane (DDM), BF3-amine complex, substituted imidazoles, accelerated anhydrides, metaphenylene diamine, diamino- diphenylether, aromatic polyetheramines, aliphatic amine adducts, aliphatic amine salts, aromatic amine adducts and aromatic amine salts.
  • the adhesive comprises an epoxy resin, a dicyandiamide (DICY) curative, a substituted urea accelerator and an ethylene vinyl acetate.
  • DICY dicyandiamide
  • the adhesive layer preferably comprises a woven fabric or scrim.
  • the scrim controls the bond line thickness between the moulding material and the substrate material. This ensures that the adhesive cannot leech away from the surface of the substrate when the sheet moulding compound or blank is subjected to pressure during moulding.
  • the scrim may be provided on the moulding material before the application of the adhesive layer.
  • Suitable reinforcement resin materials may be selected from the group consisting of thermoset resins such as epoxy, cyanate ester and phenolic resins.
  • Suitable epoxy resins include diglycidyl ethers of bisphenol A, diglycidyl ethers of bisphenol F, epoxy novolac res- ins and N-glycidyl ethers, glycidyl esters, aliphatic and cycloaliphatic glycidyl ethers, glycidyl ethers of aminophenols, glycidyl ethers of any substituted phenols and blends thereof. Also included are modified blends of the aforementioned thermosetting polymers. These polymers are typically modified by rubber or thermoplastic addition. Any suitable catalyst may be used.
  • the catalyst will be selected to correspond to the resin used.
  • One suitable catalyst for use with an epoxy resin is a dicyandiamide curing agent.
  • the catalyst may be accelerated.
  • a dicyandiamide catalyst is used, a substituted urea may be used as an accelerator.
  • Suitable accelerators include Diuron, Monuron, Fenuron, Chlortoluron, bis-urea of toluenediisocyanate and other substituted homologues.
  • the epoxy curing agent may be selected from Dapsone (DDS), Diamino-diphenyl methane (DDM), BF3-amine complex, substituted imidazoles, accelerated anhydrides, metaphenylene diamine, diaminodiphenylether, aromatic polyetheramines, aliphatic amine adducts, aliphatic amine salts, aromatic amine adducts and aromatic amine salts.
  • the resins may further contain a dicyandiamide (DICY) curative, a substituted urea accelerator. They may also contain an ethylene vinyl acetate.
  • the resin materials may comprise a toughening agent.
  • Suitable toughening agents can be selected from liquid rubber (such as acrylate rubbers, or carboxyl-terminated acryloni- trile rubber), solid rubber (such as solid nitrite rubber, or core-shell rubbers) in the nano or macro size range, thermoplastics (such as poly (EtherSulphone), poly (Imide)), block copolymers (such as styrenebutadiene-methacrylate triblocks), High modulus particles (such as Silica) in the nano or macro size range or blends thereof.
  • liquid rubber such as acrylate rubbers, or carboxyl-terminated acryloni- trile rubber
  • solid rubber such as solid nitrite rubber, or core-shell rubbers
  • thermoplastics such as poly (EtherSulphone), poly (Imide)
  • block copolymers such as styrenebutadiene-methacrylate triblocks
  • High modulus particles such as
  • the fibrous reinforcement material may comprise any fibrous material such as natural fibres (eg flax, hemp, straw, hay, seagrass, basalt), glass fibre, aramid, PAN or carbon fibre.
  • the fibrous reinforcement material may also comprise multiple layers of fibrous material.
  • the fibrous reinforcement layers comprises oriented fibres.
  • the fibrous material layer may comprise a weight ranging from 55 to 10000 gsm (g/m2), preferably from 100 to 8000 gsm and more preferably from 150 to 4000 gsm.
  • the thickness of the fibrous layer may range from 0.05 mm to 10 mm, preferably from 0.1 mm to 8 mm.
  • the fibrous material may be unidirectional, woven, chopped, biaxial or triaxial.
  • the fibre length may vary from 1 mm to several meters, preferably from 5 mm to 100 mm, more preferably from 10 mm to 100mm or less.
  • the moulding material may comprise unidirectional fibrous reinforcement in multiple layers as set out in the below Table 1.
  • the moulding material may comprise an insulating layer to prevent galvanic cou- pling between the substrate material and the fibrous reinforcement material. This is particularly advantageous for metal substrates and carbon fibre reinforcement to prevent corrosion of the metal.
  • the adhesive layer may also comprise an insulating layer to prevent galvanic coupling between the substrate material and the fibrous reinforcement material.
  • the insulating layer in the adhesive layer may be formed by the adhesive or by another material.
  • the insu- lating layer material in the adhesive may differ from the insulating layer material of the moulding material.
  • Insulating layer may comprise a suitable insulating layer material having a conductivity of 1 S.m-1 or less, preferably 0.1 S.m-1 or less, and more preferably of 0.01 S.m-1 or less, or combinations of the aforesaid ranges.
  • suitable insulating materials may comprise glass fibre, flax, hemp, rubber, thermoplastics such as polyamide, EVA.
  • the insulating material may be inthe form of a veil, scrim of fabric.
  • Curing of the compound or blank may take place in a single stage or in multiple stages such as two, three or more stages. Curing may take place following compression moulding or during compression moulding. If curing occurs in multiple stages, one or more stages may coincide with compression moulding.
  • typical initial cure cycles for the support or moulding materia- lor sheet moulding compound include an increase in temperature from ambient to temperatures up to 30 to 200 degrees C, preferably 30 to 160 degrees C, and may be followed by a dwell stage at a fixed temperature ranging from 30 to 200 degrees C, preferably 50 to 160 degrees C, more preferably 80 to 150 degrees C for a period of time ranging from 1 s to 10 hours, preferably 10s to 1 hour, 1 mins to 1 hour, 1 mins to 45 mins or 1 mins to 30 mins or 1 to 30 mins and/or combinations of the aforesaid periods.
  • the temperature is further increased to temperatures up to 60 to 200 degrees C, preferably 60 to 160 degrees C, followed by a cure stage at a fixed temperature ranging from 60 to 200 degrees C, preferably 60 to 160 degrees C, more preferably 80 to 160 degrees C for a period of time ranging from 1 s to 10 hours, preferably 10s to 1 hour, 1 mins to 1 hour, 1 mins to 45 mins or 1 mins to 30 mins or 1 to 30 mins and/or combinations of the aforesaid periods.
  • Typical post cure cycles for the moulding material include an increase in temperature from ambient to temperatures up to 30 to 200 degrees C, preferably 30 to 160 degrees C, and may be followed by a dwell stage at a fixed temperature ranging from 30 to 200 degrees C, preferably 50 to 160 degrees C, more preferably 80 to 150 degrees C for a period of time ranging from 1 s to 10 hours, preferably 10s to 1 hour, 1 mins to 1 hour, 1 mins to 45 mins or 1 mins to 30 mins or 1 to 30 mins and/or combinations of the aforesaid periods.
  • the temperature is further increased to temperatures up to 60 to 200 degrees C, preferably 60 to 160 degrees C, followed by a cure stage at a fixed temperature ranging from 60 to 200 degrees C, preferably 60 to 160 degrees C, more preferably 80 to 160 degrees C for a period of time ranging from 1 s to 10 hours, preferably 10s to 1 hour, 1 mins to 1 hour, 1 mins to 45 mins or 1 mins to 30 mins or 1 to 30 mins and/or combinations of the aforesaid periods.
  • the article is moulded in a single step at a temperature ranging from 60 to 200 degrees C, preferably 80 to 160 degrees C over a period of from 20s to 8 minutes, preferably from 40s to 3 minutes, more preferably from 60s to 120s and/or combinations of the aforesaid periods.
  • the article may be cured or part cured.
  • the part cured article may proceed through to cure during other subsequent production steps such as assembly or coating.
  • the sheet moulding compound comprises a substrate material in the form of a cold rolled steel which may be used with no surface preparation to remove contaminants or residues of oil.
  • the support material which is located on the surface of the substrate material comprises an adhesive layer and a moulding material.
  • the adhesive layer may comprise AV 4600 (Huntsman) a paste adhesive
  • the moulding material comprises resin impregnated fibrous reinforcement layers in the form of 8 layers of Unidirectional AS4 C carbon fibres (Hexcel) arranged so that a balanced quasi-isotropic arrangement of fibre directions is achieved.
  • the resin is a thermosetting epoxy formulation as supplied by Hexcel.
  • the release layer is 50im thick Kynar PVDF film (Arkema) which is located on the surface of the moulding material.
  • This sheet moulding compound is processed by being placed at ambient temperature into a moulding press or mould comprising two portions in the form of upper and lower platens, both heated at a temperature of greater than 120°C. Following placing of the sheet moulding compound, the press is closed so that both platens are in contact with the sheet moulding compound and they are held closed for at least 30 minutes, preferably at least 1 minute or 2 minutes. After this time the press is opened and the moulded article is removed and then cooled to ambient temperature. The moulded article can then be stored at ambient temperature. The article may also be subsequently heated to a temperature of at least 160°C for at least 20 minutes in a secondary process during which the moulding material proceeds to full cure.
  • tape material of a predetermined length may be fed and located above the substrate surface.
  • the tape can be pre-cut into a tape section or can be fed from a tape supply and cut into a tape section (or course) of the desired length.
  • the tape section is moved toward the substrate surface. Once near or on the substrate surface, the entire tape section can be tacked to the underlying material in one operation.
  • the tacking can comprise, for example, the fusing of the tape section to the underlying material at isolated locations using a spot welder.
  • the present invention can be used to create a laminate comprising multiple plies of tape material.
  • Each ply contains one or more sections of tape (also called courses) placed parallel to each other, 8 and each ply is fused to one or more underlying plies.
  • the shape of each ply and the orientation, or angle, of the fibers in the ply relative to fibers in other plies in the laminate are chosen such that the final produced part will have the desired structural characteristics. Also the lay up of the tape in conformation to the desired shape reduces scrap or the requirement for trimming or cutting of the laid up moulding material.
  • the first step of the method used to fabricate a tailored blank is to feed tape material of a specified length from a spool into a tape section positioning system that suspends the tape above the tooling surface upon which the tape will be placed.
  • the second step which could occur concurrently with step one, involves positioning the tape section relative to the tool such that when the tape section is lowered onto the tool, it is in the correct position and orientation for the part.
  • the guide lowers the tape section and the section is either tacked to underlying material or secured to the tooling surface. Any material that di- rectly touches the tooling surface can be secured to the tool using techniques (e.g., vacuum) that may differ from the methods used to tack tape layers to each other.
  • the tape section locating system and tacking system return to their starting positions and a new section of material is fed into the guide and the process is ready to be repeated until the blank is com- plete.
  • alternate embodiments of this invention could involve placing tape sections that have been pre-cut rather than cutting the tape after it has been fed into the guide rails. Staging pre-cut tape before the guide rails could speed up the operation of the machine since the cut operation would be removed from the critical path in the order of machine operation.
  • the tape sections could be pre-cut in line with the feed and placement, or the tape sections could be pre-cut off-line and staged as a kit to be fed into the guide rails.
  • the method used to tack plies together and the degree to which they are tacked is another parameter that could vary in different embodiments.
  • Methods for tacking the courses to underlying plies could include contact heating, ultrasonic welding, induction welding, laser heating, hot gasses, or other methods of adhering plies to each other.
  • the method could be used with an articulating head or a moving substrate surface, or a combination of the two positioning approaches.
  • an embodiment described herein uses a fixed ma- terial placement head that is positioned over a flat substrate surface that can move in the x and y directions as well as rotate, the relative motion between the placement head and the substrate surface could also be achieved by moving the placement head or a combination of the two.
  • an apparatus for manufacturing compos- ite preform support materials from composite tape comprising: a tape supply unit from which tape material is dispensed; a tape feed unit that receives tape from the tape supply unit; a cutter unit that cuts tape fed from the tape feed unit; a tape section guide that receives a tape section fed from the tape feed unit and cut by the cutter unit; a substrate surface; and a tape tacking device that tacks the tape section to other like tape sections, wherein the tape sec- tion guide suspends the tape section across the substrate surface, wherein at least one of the tape section guide and the substrate surface moves to position the tape section to a desired location and angle relative to the substrate surface, wherein the tape section guide moves the tape section toward the substrate surface, and wherein the tape tacking device presses on the tape section and tacks the tape section to another like tape section.
  • the composite tape may comprise a moulding material comprising a resin material and a fibrous reinforcement material.
  • the tape supply unit may comprise one or more creel boxes that contain spools of tape material that are actively uncoiled in such a way that tape tension between the tape feed unit and the tape spools is minimized.
  • the apparatus may further comprise a pinch roller that feeds tape from a spool into a slack coil of tape within a creel box, wherein the pinch roller maintains the slack loop size to within a determined range using feedback by one or more slack loop position sensors.
  • the tape feed unit may comprise a pinch roller and feed guides that maintain tape alignment.
  • the cutter unit may be adapted to cut at a plurality of angles relative to the longitudinal axis of the tape.
  • the tape section guide may maintain a substantially constant distance between the tape section guide and the cutter unit before and after the cutter unit changes an angle of cut.
  • the tape section guide may comprise two or more substan- tially parallel grooved rails connected to a carriage and positioned relative to each other such that when the tape is fed into the grooved rails, opposing longitudinal edges of the tape are held in grooves of the grooved rails, with a middle longitudinal portion of the tape unsup- ported.
  • the carriage may move a tape section positioned in the tape section guide from a first position at which the tape is fed and cut, to a second position near the substrate surface.
  • the substrate surface may rotate and translate in two perpendicular horizontal axes to position the tape section at the desired location and angle relative the substrate surface.
  • the tape tacking device may comprise an array of one or more ultrasonic tack welding heads that press against the tape section and affix the tape section to a previously laid tape section.
  • the tape section guide may comprise two opposing spaced apart rails each holding a longitudinal edge of the tape, and wherein the two spaced apart rails move in opposite directions substantially parallel to the longitudinal axis of the tape to maintain the substantially constant distance between the tape section guide and the cutter unit.
  • the tape section guide may support a first longitudinal side portion of the tape section and a second longitudinal side portion of the tape section opposite to the first longitudinal side portion, leaving a remaining longitudinal middle portion of the tape section unsupported.
  • the tape section guide may squeeze the tape section in a direction transverse to a longitudinal direction of the tape section such that the tape section is held in a cupped configuration before the tape tacking device presses on the tape section.
  • an apparatus for manufacturing composite preforms from composite tape comprising: a cutter unit that receives and cuts composite tape, wherein the cutter unit adjusts an angle of cut between cuts; and a tape section guide that receives composite tape conveyed through the cutter unit, wherein the tape section guide maintains substantially the same distance between the cutter unit and the tape section guide before and after the cutter unit adjusts the angle of cut.
  • the tape section guide may comprise two opposing spaced apart rails each holding a longitudinal edge of the composite tape, and wherein the two spaced apart rails move in opposite directions substantially parallel to the longitudinal axis of the composite tape to maintain the substantially same distance between the cutter unit and the tape section guide.
  • the sheet moulding compound or blank is particularly suited to moulding parts or in- serts of vehicles.
  • the blank may be suited to molding sill parts or inserts, pillar parts or inserts and/or firewall parts or inserts.
  • the support material may be cured or part cured. If the support material is part cured, the material may proceed to final curing during one or more additional steps of the production process of the vehicle such as during coating of the vehicle.
  • Figure 1 presents a diagrammatic view of a sheet moulding compound according to an embodiment of the invention
  • Figure 2 presents a diagrammatic view of an apparatus for providing a support material on a formable substrate according to a further embodiment of the invention
  • Figure 3 presents a diagrammatic view of another apparatus for moulding parts from blanks according to another embodiment of the invention, and;
  • Figure 4 presents a diagrammatic flow diagram of the process for manufacturing blanks for moulding parts.
  • the sheet moulding compound 110 comprises a substrate material 112 in the form of a steel layer.
  • the compound 110 further comprises an adhesive layer 1 14 and a moulding material formed by a fibrous reinforcement layer 16 and a reinforcement resin layer 20 which is conjoined to the surface of the fibrous reinforcement layer 116.
  • the adhesive layer 114 ensures adequate bonding of the moulding material to the substrate material 112.
  • the moulding material further comprises a release layer 118 which ensures that the moulding compound can be released promptly from the mould following forming and curing.
  • the sheet moulding compound 110 is located in a mould.
  • the mould contains two portions, one portion is heated.
  • the heated mould portion is in contact with the substrate.
  • the unheated mould portion is in contact with the release layer.
  • pressure is applied to the compound to form the substrate material whilst the temperature is also increased to the cure temperature of the moulding material.
  • a preferred temperature is 120°C. This allows the resin 120 to flow into the fibrous material 1 16 to impregnate this material 116. Following impregnation, the resin proceeds to full cure.
  • the moulded article can be promptly released from the mould as the release layer prevents the moulding from adhering to the mould.
  • Figure 2 is shown an apparatus for providing a support material on a substrate.
  • the apparatus comprises a material dispensing system 1 , tape transport rails 2, a placement head 3, a vacuum table 4 that serves as the blank tooling surface, a 3-axis motion table 5, and a structural beam 6.
  • the placement head 3 and tape transport rails 2 are affixed to the structural beam and positioned over the motion table 5 and vacuum table 4. Additional sup- port systems are depicted and include an operator interface computer 7, an electronics control cabinets 8, a vacuum pump 9, and perimeter safety guarding 10.
  • the material dispensing system 1 also called a creel rack, contains one or more creel boxes (not shown) that contain tape unspooler mechanisms (not shown).
  • a roll of tape is loaded onto a spindle and secured in place.
  • Spool guards (not shown) are put in place to stop the tape from unraveling.
  • FIG 3 an example of a process for making moulded parts is shown.
  • the process comprises the following steps: a) providing a substrate material; b) providing a support material comprising a moulding material comprising a resin material and a fibrous reinforcement material (44,46); locating said substrate material and said moulding material in relation to a mould (50); and forming the substrate and curing said moulding material to bond the moulding material to the substrate (50).
  • a robot arm (48) collects the substrate in the form of a shaped metal sheet and places this a mould (50). Meanwhile, multiaxial moulding material is supplied from a roll of prepreg (46) which is subsequently cut to the required shape to conform to the shape of the moulded article (44). The robot arm (48) then places the cut moulding material onto the substrate.
  • An adhesive layer may also form part of the prepreg or the adhesive layer may be applied separately in relation to the moulding material and the substrate (not shown).
  • the part is moulded in the moulding station (50). The process is controlled by the control unit (42).
  • a flow diagram is presented of a process of forming a sheet moulding compound or blank.
  • a support material is formed as a kit from layers of a multiaxial prepreg (200) which are laid up to form a laminate stack (202).
  • the stack is subse- quently cut (204) to the desired shape.
  • An adhesive (206) is applied to the stack and the stack is applied to a metal substrate material (208) to form the sheet molding compound or blank.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Thermal Sciences (AREA)
  • Reinforced Plastic Materials (AREA)
  • Laminated Bodies (AREA)
  • Moulding By Coating Moulds (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

L'invention concerne un procédé permettant de former une matière à mouler, le procédé de moulage consistant: a) à utiliser une matière de substrat; b) à utiliser une matière de support comprenant une matière à mouler contenant une résine collée à la surface d'une matière de renfort fibreuse, ou une matière à mouler contenant une résine imprégnant au moins en partie une matière de renfort fibreuse; c) à placer ladite matière de substrat et ladite matière à mouler dans un moule; d) à former le substrat puis à cuire la matière à mouler afin de coller la matière à mouler au substrat, le collage étant obtenu grâce à l'étape au cours de laquelle une couche adhésive est appliquée entre la matière de support et la matière de substrat, laquelle couche adhésive s'étend au-delà de la matière à mouler. La matière de substrat et la matière de support sont utilisées sous la forme d'un mélange à mouler en feuille comprenant une résine collée à la surface de la matière de renfort fibreuse. Le procédé consiste également a) à placer le mélange à mouler en feuille dans un moule; b) à former le substrat et à cuire la résine. Le procédé peut également consister à utiliser une matière de support pour renforcer un matériau apte au formage.
PCT/BR2012/000197 2011-06-20 2012-06-25 Matière de support, mélange à mouler en feuille et procédé permettant de réaliser une matière à mouler WO2012174623A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE112012002551.2T DE112012002551T5 (de) 2011-06-20 2012-06-25 Trägermaterial, SMC-Formmasse und Verfahren zur Herstellung eines Formungsmaterials
GB1400165.5A GB2507672A (en) 2011-06-20 2012-06-25 Support material, sheet moulding compound and process for makig a moulding material

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GBGB1110441.1A GB201110441D0 (en) 2011-06-20 2011-06-20 Molding material
GB1110441.1 2011-06-20
GB1206994.4 2012-04-20
GBGB1206994.4A GB201206994D0 (en) 2011-06-20 2012-04-20 Moulding material

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WO2012174623A1 true WO2012174623A1 (fr) 2012-12-27

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GB (3) GB201110441D0 (fr)
WO (1) WO2012174623A1 (fr)

Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN107123755A (zh) * 2016-02-25 2017-09-01 藤森工业株式会社 电池外包装用层叠体、电池外包装体及电池
US10814571B2 (en) 2016-04-14 2020-10-27 Becker Orthopedic Appliance Company Curable, conformable composite precursors, conformable core structures, resulting products and methods
RU2736621C2 (ru) * 2016-06-22 2020-11-19 Хексел Композитс Лимитед Ультразвуковая сварка усиленных волокном секций термоотверждаемой смолы
US10874539B2 (en) 2017-05-05 2020-12-29 Becker Orthopedic Appliance Company Configurable orthosis and method of definitive orthotic design, fabrication and validation

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GB910821A (en) * 1957-11-21 1962-11-21 Bristol Aeroplane Plastics Ltd Improvements in the manufacture of panels of fibre-reinforced resin
US3993827A (en) * 1973-04-06 1976-11-23 Pennwalt Corporation Plastic laminate construction
US4339490A (en) * 1979-09-12 1982-07-13 Mitsubishi Rayon Company, Limited Fiber reinforced plastic sheet molding compound
US4803232A (en) * 1987-07-30 1989-02-07 Lord Corporation Rubber-modified epoxy adhesive compositions
JPH03227210A (ja) * 1990-02-01 1991-10-08 Ikeda Bussan Co Ltd 内装材の製造方法
EP0640467A1 (fr) * 1993-08-11 1995-03-01 General Electric Company Procédé pour le moulage d'un objet multicouches impregné à l'état fondu ayant une surface en métal
US20030219578A1 (en) * 2000-10-03 2003-11-27 Jones Daniel Thomas Sheet moulding compound (SMC) with ventilating structure for entrapped gases
US20100166998A1 (en) * 2007-03-29 2010-07-01 Gurit (Uk) Ltd. Fibre-reinforced composite moulding and manufacture thereof

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JP3227210B2 (ja) * 1992-07-03 2001-11-12 株式会社クラレ （メタ）アクリル酸の重合抑制方法

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Publication number Priority date Publication date Assignee Title
GB910821A (en) * 1957-11-21 1962-11-21 Bristol Aeroplane Plastics Ltd Improvements in the manufacture of panels of fibre-reinforced resin
US3993827A (en) * 1973-04-06 1976-11-23 Pennwalt Corporation Plastic laminate construction
US4339490A (en) * 1979-09-12 1982-07-13 Mitsubishi Rayon Company, Limited Fiber reinforced plastic sheet molding compound
US4803232A (en) * 1987-07-30 1989-02-07 Lord Corporation Rubber-modified epoxy adhesive compositions
JPH03227210A (ja) * 1990-02-01 1991-10-08 Ikeda Bussan Co Ltd 内装材の製造方法
EP0640467A1 (fr) * 1993-08-11 1995-03-01 General Electric Company Procédé pour le moulage d'un objet multicouches impregné à l'état fondu ayant une surface en métal
US20030219578A1 (en) * 2000-10-03 2003-11-27 Jones Daniel Thomas Sheet moulding compound (SMC) with ventilating structure for entrapped gases
US20100166998A1 (en) * 2007-03-29 2010-07-01 Gurit (Uk) Ltd. Fibre-reinforced composite moulding and manufacture thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107123755A (zh) * 2016-02-25 2017-09-01 藤森工业株式会社 电池外包装用层叠体、电池外包装体及电池
US10814571B2 (en) 2016-04-14 2020-10-27 Becker Orthopedic Appliance Company Curable, conformable composite precursors, conformable core structures, resulting products and methods
RU2736621C2 (ru) * 2016-06-22 2020-11-19 Хексел Композитс Лимитед Ультразвуковая сварка усиленных волокном секций термоотверждаемой смолы
US10874539B2 (en) 2017-05-05 2020-12-29 Becker Orthopedic Appliance Company Configurable orthosis and method of definitive orthotic design, fabrication and validation
US11786391B2 (en) 2017-05-05 2023-10-17 Becker Orthopedic Appliance Company Configurable orthosis and method of definitive orthotic design, fabrication and validation

Also Published As

Publication number Publication date
GB201206994D0 (en) 2012-06-06
GB201400165D0 (en) 2014-02-19
GB201110441D0 (en) 2011-08-03
DE112012002551T5 (de) 2014-02-27
GB2507672A (en) 2014-05-07

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