WO2024038387A1 - Matériau composite - Google Patents

Matériau composite Download PDF

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Publication number
WO2024038387A1
WO2024038387A1 PCT/IB2023/058222 IB2023058222W WO2024038387A1 WO 2024038387 A1 WO2024038387 A1 WO 2024038387A1 IB 2023058222 W IB2023058222 W IB 2023058222W WO 2024038387 A1 WO2024038387 A1 WO 2024038387A1
Authority
WO
WIPO (PCT)
Prior art keywords
resin
composite material
fibres
reinforcement
binder
Prior art date
Application number
PCT/IB2023/058222
Other languages
English (en)
Inventor
Antonio NIERI
Luca NUCARA
Masateru GOTO
Nicola DEL DEBBIO
Giuseppe PAGANO
Marzia SERRONI
Original Assignee
Delta - Tech S.P.A.
Delta Preg S.P.A. Con Unico Socio
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 Delta - Tech S.P.A., Delta Preg S.P.A. Con Unico Socio filed Critical Delta - Tech S.P.A.
Publication of WO2024038387A1 publication Critical patent/WO2024038387A1/fr

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Classifications

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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B1/00—Layered products having a general shape other than plane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysiloxanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
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    • B32B5/06—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 a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
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    • 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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    • 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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    • B32B7/04—Interconnection of layers
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    • B32B7/04—Interconnection of layers
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    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • B32B2250/00—Layers arrangement
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    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
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Definitions

  • the present invention relates to a composite material , a method of manufacturing an article and a kit comprising such a composite material .
  • thermosetting resin matrix that are more or less reinforced with fibres
  • This intermediate material once laminated on the surface of the mould, is then subj ected to the moulding process which is carried out with the application of a compaction pressure of the di f ferent layers and of an appropriate polymerisation temperature of the matrix ( ces ) .
  • the moulding time given a speci fic thermal profile , is adj usted on the basis of the chemical-physical characteristics of the thermosetting matrix ( ces ) .
  • thermosetting matrix-based composite materials More in detail and purely by way of example , some moulding techniques for thermosetting matrix-based composite materials are reported .
  • This moulding technique compared to the previous one , although more expensive , allows to obtain better quality moulded components both with regards to aspects relative to the structural strength of the laminate and with regards to aspects concerning the superficial qual ity of the article , a fundamental element for the subsequent painting step .
  • the mould is formed by two components , the mould and the counter-mould .
  • the mould is kept open so that there is space between the two hal f-moulds to introduce therein the reinforcement and matrix layerings .
  • the mould is closed by operating the relative press , so as to guarantee an appropriate closure force between the two hal f-moulds and consequently an adequate compaction between the various layers of the laminate .
  • the mould is then suitably heated so as to allow the polymerisation reaction of the matrix to progress .
  • the activities described above require operators to carry out a long manual lamination process with an obvious impact on the overall production cost .
  • the articles obtained can present imperfections , especially when they have to reproduce particularly complex shapes .
  • the typical defectivenesses of the laminates can be divided into superficial defects , and therefore already visible sometimes even to the naked eye , and defects present inside the laminate that can be found with appropriate destructive and nondestructive techniques .
  • Porosity pitting
  • reference is made to small cavities having dimension smaller than a millimetre (general of the order of a tenth of a millimetre ) , which are present on the surface of the component .
  • these pores are attributable to the failure to evacuate the air at the interface between the mould and the first layer of the laminate before the gelation of the matrix during the moulding process .
  • This porosity represents a defect that must be adequately removed during the surface treatment step preparatory to painting . In case of excessive porosity, appropriate additional treatments are unfortunately necessary before being able to proceed with painting with the consequent increase in costs .
  • Irregular superficial distribution of the resin may contribute to generating visible irregularities on the surface of the component, such as, for example, a local increase or decrease in the superficial thickness of the matrix to protect the underlying reinforcement fibres. This may be due for example to the lack of adherence of the first pre-preg layer to the surface of the mould ( typical of the concave areas of the mould) before the gelation of the matrix . In this case , a local thickening of the resin layer to protect the fibres (bridging) can be noted .
  • a second example concerns the presence of wrinkles of the reinforcement layers that can be generated when laminating the various layers .
  • Aim of the present invention is that of providing a composite material , a method of manufacturing an article and a kit that allow to overcome , at least partially, the drawbacks of the prior art and are , at the same time , easy and economical to implement .
  • a composite material a method of manufacturing an article and a kit comprising such a composite material as claimed in the following independent claim and, preferably, in any one of the claims directly or indirectly dependent on the independent claim .
  • Figure 1 schematically shows a section of a composite material in accordance with the present invention
  • Figure 2 schematically shows a section of a material with overlapping layers constituted by the material of Figure 1 and a layer of reinforcement material .
  • Figure 3 schematically shows the shape of the DSC curve in the area of the glass transition temperature
  • Figure 4 schematically shows a template necessary for the preparation of the specimens used for the mechanical tests (the measurements reported are indicated in millimetres ) ;
  • Figure 5 is a photograph of the template placed on a composite material 1 during the preparation of the specimens used for the mechanical tests ;
  • Figure 6 schematically shows a trimming tool (the measurements reported are indicated in millimetres ) ;
  • Figure 7 shows the trimming steps of a reinforcement 4 of a specimen of the composite material 1 used for the mechanical tests ;
  • Figure 8 shows the trimming steps of a surface film of the specimen used for the mechanical tests ;
  • Figure 9 is a photograph of the specimen of the composite material 1 used for the mechanical tests ;
  • Figure 10 schematically shows the geometry of a mould used to test the present invention (the measurements reported are indicated in millimetres ) ;
  • Figure 11 shows the lamination steps of Test N1 ( configuration A - example 5 reported below) ;
  • Figure 12 shows the lamination steps of Test N2
  • Figure 13 shows the lamination steps of Test N3
  • Figure 14 schematically shows a typical configuration of mould for autoclave complete with moulding material (prepreg) and vacuum bag with the various auxiliaries and vacuum line ;
  • Figure 15 shows results of tests carried out with a reference material and described within Example 5 reported below
  • Figure 16 shows results of tests carried out with a reference material and described within Example 5 reported below;
  • Figure 17 shows results of tests carried out with an embodiment of a material in accordance with the present invention and described within Example 5 reported below;
  • Figure 18 is a photograph of a mould used to test the present invention (Example 6 ) ;
  • Figure 19 contains photographs of three moulded components ;
  • Figure 20 contains three optical microscope images of the sections performed on the points CSA1 , CSB1 and CSC1 reported in Figure 19 ;
  • Figure 21 schematically shows a section of an alternative embodiment of the composite material of Figure 1 .
  • a composite material 1 ( Figure 1 ) to manufacture articles though moulding .
  • the composite material 1 has a surface film 2 , which comprises a first ( thermosetting) resin formulation having an areal weight up to about 700 g/m 2 ; a reinforcement 4 , which consists of an at least partially dry first fibrous material having, taking into account the sole fibrous component , an areal weight up to about 900 g/m 2 ; and at least one binder 3 , which binds the surface film 2 to the reinforcement 4 .
  • the areal weight of the first ( thermosetting) resin formulation of the surface film 2 is measured according to standard ASTM D 3529/D 3529M - 97 ( reapproved 2008 ) .
  • the areal weight of the first fibrous material is measured according to standard BS EN12127 : 1998 .
  • thermosetting resin formulation means a thermosetting resin (properly so called) and optionally further components in addition to the thermosetting resin (properly so called) .
  • further components are ( in addition to the crosslinkers ) : accelerators , tougheners , additives to modi fy the rheology/resistance/wettability, organic and/or inorganic fillers etc . ( and combinations thereof ) .
  • thermosetting resin means both a resin provided with a crosslinker and a resin capable of crosslinking i f subj ected to heat .
  • the resin is composed of a combination of more types of resins .
  • the resin is composed of only one type of resin .
  • crosslinkers examples include aliphatic amines , cycloaliphatic polyamines , aromatic amines , aromatic polyamines , polyamides , polyamidoamines , imidazolines , polyaminoimidazolines, ketimines, enamines, imidazoles, cyanamide, dicyandiamide, ureas, hydrazines, hydrazides, carboxylic acids, carboxylic acid anhydrides, phenolic resins, polysulfides, polymercaptans, boron complexes, quaternary phosphonium salts, ternary sulfonium salts.
  • aromatic amines particularly useful in the context of the present text are: aromatic amines, imidazoles, cyanamide, dicyandiamide, ureas, hydrazides, carboxylic acid anhydrides, phenolic resins, boron complexes (and combinations thereof) .
  • the at least partially dry material has at least one part without resin (in particular, the binder 3; more in particular, the binder 3 and an adhesive binder - described in more detail below) .
  • the first fibrous material has fibres that , being dry, are able to move independently of each other, compatibly with the intertwine and/or stitching constraints ; more in particular, such fibres are on the opposite side with respect to the side of the surface film 2 .
  • the fibres capable of moving independently of each other are substantially dry .
  • the dry fibre content ( or alternatively the degree of impregnation) of the reinforcement 4 may conveniently be expressed in terms of water pick-up (WPU) measurable through the procedure reported in the literature ( Simmons M . et al , WO2013186389 ) .
  • WPU water pick-up
  • the water pick-up value increases as the percentage of dry fibres present within a given reinforcement increases . It is also possible to identify two limit situations potentially applicable to any type of reinforcement : ( a ) completely dry reinforcement (not at all impregnated) , therefore with 100% of dry fibres , for which the maximum water pick-up value is expected, and (b ) completely impregnated reinforcement , therefore with 0% of dry fibres , in which the water pick-up value typically tends to zero .
  • the reinforcement 4 has a dry fibre content, expressed as %DF-R4 (based on the formula of Equation 1 - reported below) , greater than about 20%, in particular greater than about 25%, more in particular greater than about 30%.
  • the reinforcement 4 has a dry fibre content, expressed as %DF-R4, up to about 99.8% (in particular, up to about 99.7%; more in particular, up to about 99.5%) .
  • the composite material 1 offers a particularly strong drapability as described in Examples 5 and 6 reported below.
  • the efficacy and the functionality of the composite material 1 are correlated to the percentage of dry fibres of the reinforcement 4 (%DF- R4 ) •
  • thermosetting resin formulation constituted by a dry reinforcement made of carbon fibre and a dry reinforcement made of glass fibre and by the respective prepregs with a thermosetting resin formulation:
  • Such a reinforcement is a composite biaxial fabric as described below: carbon fibre T700SC 12K 50C, fibre weight areal weight — 250 g/m 2 , arranged at -45°/ + 45°.
  • the carbon fibre is stitched/knitted with a polyester thread (stitch yarn) at 0° and areal weight of 8 g/m 2 , with a chain/pillar knitting type; the fabric is stabilised with the following stabilisation thread at 0°: 136 tex E Glass, areal weight of 7 g/m 2 .
  • Overall reinforcement areal weight (all-up mass) 265 g/m 2 (in the present text by g/m 2 are intended grams per square metre) and overall reinforcement width, 1270 mm.
  • This reinforcement is a fabric with VR48 style, intertwine of weave Twill 2x2, composed as described below: glass fibre in warp (type and tex) 3 x EC9 68 1x0, glass fibre in weft EC9 204 1x0 or ECU 204 1x0; the GI6224/1 primer is applied to the glass fibre.
  • the fabric has a number of 7.0 threads per cm in the warp direction and a number of 7.0 threads per cm in the weft direction.
  • the minimum tensile strength in the warp is 310 N/cm, the minimum tensile strength in the weft is 250 N/cm.
  • Overall reinforcement areal weight (all-up mass) 290 g/m 2 , reinforcement thickness of 0.23 mm and overall reinforcement width of 1270 mm.
  • - GG250X (T700) -DT150-40 ME (H 127 cm) (code M-PRO19235) is a biaxial fabric impregnated with a thermosetting resin system and has the following characteristics: carbon fibre T700SC 12K 50C, fibre weight areal weight 250 g/m 2 , arranged at -45°/+45°.
  • the carbon fibre is stitched/knitted with a polyester thread (stitch yarn) at 0° and areal weight of 8 g/m 2 , with a chain knitting type; the fabric is stabilised with the following stabilisation thread at 0°: 136 tex E Glass, areal weight of 7 g/m 2 .
  • Overall reinforcement area weight (all-up mass) 265 g/m 2 and overall reinforcement width 1270 mm.
  • the reinforcement thus described is impregnated with the resin system DT150; the material has a nominal resin content of 40% by weight and a theoretical moulded sheet thickness of 0.27 mm.
  • the resin DT150 (product manufactured by Delta-Tech SpA) has the following characteristics: maximum achievable DMA tg of 140 °C; processing through curing in vacuum bag in autoclave and compression moulding; 30 days of preservability at 21 °C; average tackiness; chemical nature Thermosetting Epoxy Resin; polymerisation temperature interval from 120 to 150 °C; density of the pure polymerised resin 1.24 g/cm 3 ; average dynamic viscosity, 500-1000 Poise at 60 °C.
  • ME H 127 cm
  • code MW290T0440 is a glass fibre fabric with weaving style twill 2x2, impregnated with a thermosetting resin system and has the following characteristics: glass fibre in warp (type and tex) 3 x EC9 68 1x0, glass fibre in weft EC9 204 1x0 or ECU 204 1x0.
  • the fabric has a number of 7.0 threads per cm in the warp direction and a number of 7.0 threads per cm in the weft direction.
  • Overall reinforcement areal weight (all-up mass) 290 g/m 2 and overall reinforcement width, 1270 mm.
  • the reinforcement thus described is impregnated with the resin system DT150; the material has a nominal resin content of 40% by weight and a theoretical moulded sheet thickness of 0.27 mm.
  • the characteristics of the resin system DT150 are similar to those described for the previous material .
  • Table 1 reports the experimental water pickup values recorded on each material.
  • the percentage of dry fibres of the reinforcement 4 in the composite material 1 can be assessed on the basis of the following mathematical formula (Eq . 1 ) : where WPUR4 is the water pick-up measured on the reinforcement 4 of the composite material 1 ( example values are indicated in the last column of Table 1 for the last two materials ) and WPUDry-R4 is the water pick-up measured on the completely dry reinforcement 4 ( example values are indicated in the last column of Table 1 for the first two materials ) . It should be noted that the determination of the WPUR4 value requires the separation of the reinforcement 4 from the surface film 2 and, as far as possible , from the layer of binder 3 interposed between the surface film 2 and the reinforcement 4 .
  • this separation can be made by applying a peeling force on a flap of the surface film 2 and a flap of the reinforcement 4 or, alternatively, according to a procedure suitably identi fied based on the possible variants of the composite material 1 .
  • the surface film 2 comprises a support 8 of a second fibrous material in particular having an areal weight smaller than about 200 g/m 2 ( in particular, smaller than about 100 g/m 2 ; more in particular, smaller than about 40 g/m 2 ) .
  • the surface film 2 further comprises a first superficial layer 7 , which defines an outer surface of the composite material 1 and comprises ( in particular, mainly consists of ; more in particular, it is substantially constituted by; more in particular, it consists of ) the first ( thermosetting) resin formulation .
  • the support 8 is arranged between the superficial layer 7 and the binder 3 .
  • the first superficial layer 7 is mainly constituted by (in particular, consists of) the first (thermosetting) resin formulation.
  • the first thermosetting resin formulation (in particular, the surface film 2) comprises (in particular, inorganic) fillers dispersed (inorganic fillers dispersed) (in particular, in the superficial layer 7) .
  • fillers in particular inorganic fillers, in the first thermosetting resin formulation (in particular, in the surface film 2; more in particular, in the first superficial layer 7) allows to improve the obtaining of homogeneous and regular surfaces on the finished component once moulded.
  • the surface film 2 (in particular, the first thermosetting resin formulation) is without fillers (in particular, inorganic fillers) .
  • the fillers are constituted by (a combination of) inorganic fillers of a different chemical nature, such as for example carbonates, silicates, sulfates, metal oxides, etc. (and a combination thereof) .
  • the fillers are between 5% (in particular, 15%) and 60% by weight, relative to the weight of the first (thermosetting) resin formulation of the surface film 2 (in particular, of the first superficial layer 7) .
  • the fillers have a particle size below 200 microns (in particular, at least 1 micron; more in particular, at least 5 microns) .
  • the dimensions (particle size) are obtained through successive sievings with sieves with holes having decreasing dimensions (diameters) .
  • the diameter of the holes of the first sieve that does not allow the passage of the particles indicates the dimensions (i.e. diameter) of the particles.
  • the measurements by means of subsequent sievings are carried out as long as the dimensions (i.e. diameters) of the particles and of the holes of the sieves allow it (in particular, up to a minimum of 0.05 mm) .
  • the dimensions of the particles are measured as average diameter D(v,0.5) measured through a laser granulometer - in particular, using a laser granulometer Mastersizer Microplus Ver. 2.19 (Malvern Instruments® Ltd) .
  • the first superficial layer 7 has a thickness that is at least 20% (in particular, up to 99.6%; more in particular, up to 98%) of the overall thickness of the surface film 2 (for the measurement of these parameters see further below in relation to the determination of the position of the support 8) .
  • the first superficial layer 7 has a thickness of at least 0.01 mm (in particular, up to 0.8 mm) .
  • the support 8 is arranged in the area of a surface of the surface film 2 opposite the first superficial layer 7 and facing said binder 3; in particular, the support 8 is (at least partially) arranged in contact with the binder 3.
  • the support 8 is arranged inside the (embedded in the) first (thermosetting) resin formulation.
  • the surface film 2 comprises a second layer 9 of the first resin formulation such that the support 8 is arranged between the first superficial layer 7 and the second layer 9 ( Figure 21) .
  • the placement of the support 8 inside the surface film 2 can be defined through the coordinate system Tf S along the relative thickness.
  • Tf S 0 the interface surface of the surface film 2 bordering the layer of binder 3.
  • Tf S 100 the outer surface of the surface film 2 , i . e . the surface opposite the binder 3 , and intended to come into direct contact with the mould .
  • the support 8 its median plane P m f .
  • the support 8 of the composite material 1 is arranged with the relative median plane P m f in the dimension T S f ranging from 0 to 50 .
  • the placement of the support 8 is evaluated through an analysis of the section of the composite material 1 performed with the aid of an appropriate microscope .
  • a freezer suitable for reaching this temperature or, alternatively, to the use of liquid nitrogen .
  • the thickness of the first superficial layer 7 can be determined .
  • the first thermosetting resin formulation comprises a first thermosetting resin chosen from the group consisting of : epoxy resin, cyanate ester resin, vinyl ester resin, acrylic resin, phenolic resin, melamine resin, urethane resin, siloxane resin, alkyd resin, benzoxazine resin, maleimide resin, furan resin, polyester (and a combination thereof) .
  • the first thermosetting resin formulation comprises (more precisely, the first resin is) an epoxy resin.
  • the first resin comprises (in particular, is) an epoxy resin.
  • the first resin formulation comprises at least 40% (in particular, at least 50%; more in particular, at least 60%; even more in particular, at least 90%) by weight, relative to the weight of the first resin formulation, of the first resin.
  • the first resin formulation comprises up to 95% (in particular, 85%; more in particular, up to 40%) by weight, relative to the weight of the first resin formulation, of the first resin.
  • the first resin formulation consists of the first resin.
  • the first thermosetting resin formulation (in particular, the first resin) has in its inside a crosslinker.
  • the crosslinker is chosen from the group consisting of: aliphatic amines, cycloaliphatic polyamines, aromatic amines, aromatic polyamines, polyamides, polyamidoamines, imidazolines, polyaminoimidazolines, ketimines, enamines, imidazoles, cyanamide, dicyandiamide, ureas, hydrazines, hydrazides, carboxylic acids, carboxylic acid anhydrides, phenolic resins, polysulfides, polymercaptans, boron complexes, quaternary phosphonium salts, ternary sulfonium salts (and a combination thereof) .
  • aromatic amines particularly useful in the current context are: aromatic amines, imidazoles, cyanamide, dicyandiamide, ureas, hydrazides, carboxylic acid anhydrides, phenolic resins, boron complexes.
  • the first (thermosetting) resin formulation has an areal weight of at least about 30 g/m 2 (in particular, at least about 120 g/m 2 ) . More precisely but not necessarily, the first (thermosetting) resin formulation has an areal weight up to about 600 g/m 2 (in particular, up to about 400 g/m 2 )
  • the first thermosetting resin formulation (in particular, the first resin) has a contained viscosity variation following heating and a medium-low tackiness.
  • the second fibrous material has an areal weight of at least about 3 g/m 2 (in particular, at least about 10 g/m 2 ) .
  • the second fibrous material comprises (in particular, mainly comprises; more in particular, is made of) carbon fibres, glass fibres, basalt fibres, natural fibres (e.g., flax) , synthetic fibres (e.g., polyester and/or aramid fibres) .
  • the second fibrous material comprises (in particular, mainly comprises; more in particular, is made of) synthetic fibres (e.g. polyester fibres) .
  • the areal weight of the first (thermosetting) resin formulation is at least about 0.7 times (in particular, at least about 1 time; more in particular, at least about 2 times; even more in particular, at least about 5 times; in particular, up to about 100 times; more in particular, up to about 30 times) the areal weight of the second fibrous material.
  • the first fibrous material has, taking into account the sole fibrous component, an areal weight smaller than about 500 g/m 2 (in particular, smaller than about 300 g/m 2 ) .
  • the first fibrous material has an areal weight of at least about 30 g/m 2 and comprises (in particular, mainly comprises; more in particular, is made of) carbon fibres, glass fibres, basalt fibres, natural fibres such as flax, synthetic fibres such as polyester and/or aramid fibres.
  • the first fibrous material is (a fabric and is) chosen from the group consisting of: woven fabrics, unidirectional fabrics, multiaxial fabrics (optionally stabilised through stitching threads) and nonwoven fabrics (in particular, with fibres stabilised through binder) .
  • the first fibrous material is a unidirectional fabric or a multiaxial (in particular, biaxial) fabric.
  • the first fibrous material is a multiaxial (in particular, biaxial) fabric.
  • fabric is meant both a material containing woven and nonwoven fibres.
  • the binder 3 comprises (in particular, is) an adhesive binder and is arranged between the surface film 2 and the reinforcement 4.
  • the areal weight of this adhesive material is measured according to standard ASTM F2217/F2217M - 13 (reapproved 2018) .
  • the binder 3 comprises (in particular, is) an adhesive binder, having a glass transition temperature (Tg) smaller than about 20 °C.
  • the adhesive binder has these characteristics it can be sufficiently adhesive (tacky) to be able (even in a small amount) to perform its function of connection between the surface film 2 and the reinforcement 4.
  • the glass transition temperature is smaller than about 15 °C (more in particular, smaller than about 0 °C) .
  • the glass transition temperature is greater than about -80 °C.
  • the adhesive binder has an areal weight smaller than the areal weight of the reinforcement 4 (in particular, smaller than half the areal weight of the reinforcement 4) .
  • the adhesive binder has an areal weight greater than 2 % ( in particular, greater than 4 % ; more in particular, greater than 6% ) of the areal weight of the reinforcement 4 .
  • the adhesive binder has an areal weight smaller than about 300 g/m 2 ( in particular, smaller than about 150 g/m 2 ; more in particular, smaller than about 60 g/m 2 ; even more in particular, smaller than about 30 g/m 2 ) .
  • the adhesive binder has an areal weight greater than about 5 g/m 2 .
  • the adhesive binder comprises ( in particular, is ) a second ( in particular, thermosetting) resin formulation, which, in turn, comprises ( in particular, is ) a second ( in particular, thermosetting) resin chosen from the group consisting of : epoxy resin, cyanate ester resin, vinyl ester resin, acrylic resin, phenolic resin, melamine resin, urethane resin, siloxane resin, alkyd resin, benzoxazine resin, maleimide resin, furan resin, polyester ( and a combination thereof ) .
  • the second resin in particular, the adhesive binder
  • thermosetting adhesive binder (the second resin) comprises a crosslinker .
  • the adhesive binder in particular, the second resin formulation; more in particular, the second resin
  • the second resin formulation is not crosslinked (in particular, the second resin formulation - more in particular, the second resin - is not crosslinked) .
  • the adhesive binder in particular, the second resin formulation; more in particular, the second resin
  • the second resin is without
  • the adhesive binder succeeds in performing its function of connection between the surface film 2 and the reinforcement 4 for a long period of time (in practice, ageing more slowly) .
  • the adhesive binder can harden by exploiting the crosslinker of the first resin formulation (that of the surface film 2) and/or that present in the rear layer 5 (described in more detail below) .
  • the binder 3 (in addition to the aforementioned adhesive binder) also comprises a fibrous material (in particular, a fibrous layer) immersed in the adhesive binder.
  • this third fibrous material comprises (in particular, mainly comprises; more in particular, is made of) carbon fibres, glass fibres, mineral fibres (e.g. basalt fibres) , natural fibres (e.g. flax) , synthetic fibres (e.g. polyester and/or aramid fibres) , metal fibres and combinations (mixtures) thereof.
  • this fibrous material (of the binder 3) comprises (in particular, mainly comprises; more in particular, is made of) synthetic fibres (e.g. polyester fibres) .
  • the binder 3 (in particular, the adhesive binder) has a connection force (between the surface film 2 and the reinforcement 4) of at least about 0.6 N (in particular, at least about 1.0 N) measured on a sample of about 25 mm X 200 mm.
  • the binder 3 (in particular, the adhesive binder) has a connection force up to about 200 N (in particular, up to about 150 N) measured on a sample of about 25 mm X 200 mm.
  • the binder 3 (in particular, the adhesive binder) has a connection stress (between the surface film 2 and the reinforcement 4) of at least about 0.1 kPa (in particular, at least about 0.2 kPa) .
  • the binder 3 (in particular, the adhesive binder) has a connection stress smaller than about 40 kPa (in particular, smaller than about 30 kPa) .
  • the binder 3 is arranged between the surface film 2 and the reinforcement 4 so as to form a continuous layer and be homogeneously distributed .
  • the binder 3 is distributed heterogeneously ( so that there are , between the surface film 2 and the reinforcement 4 zones without binder 3 ) according to a defined design (for example forming dots , circles , lines etc . ) or a disordered shape ( random distribution) .
  • a method of manufacturing an article comprises a first lamination step, during which the composite material 1 as described above is arranged on a mould ( in particular, such that the surface fi lm 2 is in contact with the mould) , in particular such that the composite material 1 substantially acquires the shape of the mould; a second lamination step, which i s subsequent to the first lamination step and during which a rear layer 5 ( Figure 2 ) is arranged on said composite material 1 in contact with the latter so as to obtain a material with overlapping layers 6 ( see Figure 2 ) substantially having the shape of the mould; and a moulding step, which is subsequent to the second lamination step and during which the material with overlapping layers 6 arranged on the mould i s compressed (pressed - in particular, subj ected to pressure greater than the atmospheric pressure ) and heated .
  • the rear layer 5 and the composite material 1 are compressed (pressed) towards each other .
  • the material with overlapping layers 6 arranged on the mould is suitably compacted and heated in order to obtain the polymerisation of the thermosetting matrix .
  • the rear layer 5 comprises a third fibrous material (which is understood as such and therefore dry without resin components ) and a quantity of a third resin formulation .
  • the third resin formulation is thermosetting and comprises ( in particular, is ) a third ( in particular, thermosetting) resin chosen from the group consisting of : epoxy resin, cyanate ester resin, vinyl ester resin, acrylic resin, phenol ic resin, melamine resin, urethane resin, siloxane resin, alkyd resin, benzoxazine resin, maleimide resin, furan resin, polyester ( and a combination thereof ) ; more in particular, the third thermosetting resin comprises a crosslinker .
  • a third ( in particular, thermosetting) resin chosen from the group consisting of : epoxy resin, cyanate ester resin, vinyl ester resin, acrylic resin, phenol ic resin, melamine resin, urethane resin, siloxane resin, alkyd resin, benzoxazine resin, maleimide resin, furan resin, polyester ( and a combination thereof ) ; more in particular, the third thermosetting resin comprises a crosslinker .
  • the fibre content of the material 6 with overlapping layers expressed as Fibre Volume Fraction ( FVF) ranges from the minimum value of about 20% ( in particular, the minimum value of about 35% ) to the maximum value of about 75% ( in particular, the maximum value of about 65% ) .
  • FVF Fibre Volume Fraction
  • the layer of binder 3 must be considered in the overall calculation, taking into account the relative areal weight as matrix in case it is adhesive binder without fibrous material ( Rleg ) , as combination of resin formulation (R leg ) and of fibre (F leg ) in case it is adhesive binder containing a fibrous material .
  • the reinforcement 4 i.e. first fibrous material, must be counted as fibre (F rinf,4 ) .
  • the rear layer 5 must be counted considering both its fibrous component (F sp ) and its resin component (R sp ) .
  • the distribution of the resin component and of the relative fibrous component has no influence on the calculation of the Fibre Volume Fraction.
  • the FVF can then be evaluated based on the following formula :
  • F leg is the areal grammage of the fibrous material of the binder 3 (where present)
  • D fleg is the density of the fibre of the fibrous material of the binder 3 (where present)
  • F einf ,4 is the areal grammage of the fibre of the reinforcement 4
  • D rinf,4 is the density of the material of the fibrous reinforcement 4
  • F sp is the areal grammage of the fibre of the rear layer 5
  • D fsp is the density of the fibre of the rear layer 5
  • R leg is the areal grammage of the adhesive binder 3
  • D rleg is the density of the resin formulation of the adhesive binder 3
  • R sp is the areal grammage o f the resin formulation present in the rear layer 5
  • D rsp is the density of the resin formulation of the rear layer 5 .
  • the term F leg /D fleg is to be considered null .
  • the FVF can then be evaluated based on the following formula :
  • both the terms F leg /D fleg and R leg /D rleg must be considered in the calculation of the FVF (Eq . 2 ) .
  • the rear layer 5 combined with the composite material 1 , of fers an appropriate ratio between the areal weight of the fibre and the areal weight of the matrix such as to place the overall FVF of the entire laminate within the limits indicated above .
  • the rear layer 5 should contain an adequate excess of the third resin formulation so as to rebalance the FVF (overall of the laminate) of the material with overlapping layers 6.
  • the fibrous component of the rear layer 5, third fibrous material has an areal weight of at least about 100 g/m 2 (in particular, at least about 350 g/m 2 ; in particular, up to about 2000 g/m 2 ; more in particular, up to about 1500 g/m 2 ) .
  • the rear layer 5 comprises a quantity of the third resin formulation such as to satisfy the overall FVF of the laminate based on the equation 2 (or equation 3) .
  • the areal weight of the fibrous component of the rear layer 5 is measured according to standard ASTM D 3529/D 3529M - 97 (reapproved 2008) .
  • the third fibrous material is chosen from the group consisting of: woven fabrics, unidirectional fabrics, multiaxial fabrics (in particular, biaxial fabrics; optionally stabilised through stitching threads) , nonwoven fabrics (and a combination thereof) . More in particular, the third fibrous material is chosen in the group consisting of: woven fabrics and multiaxial (in particular, biaxial) fabrics. Even more in particular, the third fibrous material is a woven fabric.
  • the third thermosetting resin comprises a crosslinker.
  • the third fibrous material comprises (in particular, mainly comprises; more in particular, is made of) carbon fibre, glass fibre, basalt fibre, natural fibres such as flax, synthetic fibres such as polyester or aramid fibres.
  • the material with overlapping layers 6 is subjected to a compression (pressure) of at least about 1 Kgforce/cm 2 (in particular, up to about 150 Kgf O rce/cm 2 ; more in particular up to about 50 Kgforce/cm 2 ) .
  • the material with overlapping layers 6 arranged on the mould is moulded with vacuum bag (inside which the material with overlapping layers 6 and the mould are arranged) and furnace, by applying a depression inside the bag such that the absolute pressure inside the bag is smaller than 0.5 bar (in particular, greater than 0.001 bar) .
  • the material with overlapping layers 6 is inserted inside a furnace whose temperature is at least 50 °C (in particular, up to 200 °C) .
  • the material is moulded in autoclave at an absolute pressure of at least 2 bar (in particular, up to 10 bar) .
  • the moulding step is carried out in the press, by applying a compaction pressure of the layers generally greater than 2 Kgforce/cm 2 .
  • kits to implement the above-described method comprises the composite material 1 and the rear layer 5 as described above .
  • F1-F4 indicate the formulations of four di f ferent binders ( among them alternatives ) that have been prepared and can be used in accordance with the present invention and more precisely :
  • Fl is an epoxy binder without crosslinker ;
  • F2 is an epoxy binder with crosslinker ;
  • F3 is a binder containing rubber (with crosslinker ) ;
  • F4 is a cyanate-ester binder .
  • Araldite® GY2600 (produced and marketed by Huntsman®) is an unmodified, average viscosity, bisphenol A diglycidyl ether (DGEBA) epoxy resin resulting from the reaction of bisphenol A and epichlorohydrin.
  • DGEBA diglycidyl ether
  • the main characteristic of this resin is its low content of hydrolysable chlorine. It offers high mechanical performance and confers a good chemical resistance.
  • Epoxy equivalent weight EEW (ISO 3001) : 184 - 190 g/eq;
  • Araldite® GT 7071 (produced and marketed by Huntsman®) is a low melting point bisphenol A diglycidyl ether (DGEBA) solid epoxy resin with low to medium molecular weight (type 1) . It is used to produce high-performance coating materials, thanks to its exceptional adhesion to a variety of substrates (e.g. metals, cement, wood, etc.) and chemical resistance. It offers greater flexibility and high impact resistance.
  • DGEBA diglycidyl ether
  • HyPox® RA95 (produced and marketed by Huntsman®) is a high viscosity mixture constituted by a butadiene-acrylonitrile elastomer dissolved in bisphenol A epoxy resin. Based on a solid CTBN elastomer, HyPox RA95 combines the functionalities of the epoxy resins with toughness and impact resistance. Compared to the conventional epoxy systems, its use improves resistance to impact, peeling and cutting.
  • Primaset® PT-30 (produced and marketed by Arxada®) is a multifunctional cyanate-ester resin capable of providing a highly crosslinked structure with high thermal stability. If properly polymerised, the resulting Tg may exceed 300 °C. This high performance thermosetting resin is characterised by excellent dielectric and mechanical properties and allows an epoxy-like processing
  • Dyhard® 10 OS (produced and marketed by AlzChem®) is a micronized dicyandiamide (DICY) -based crosslinker.
  • the singlecomponent systems containing DICY are capable of crosslinking if exposed to 145-160 °C for 30-60 min. After adequate polymerisation, the DICY-based epoxy systems lead to a very dense polymeric structure, which offers a high thermal and chemical resistance.
  • Dyhard® UR500 (produced and marketed by AlzChem®) is a micronized bifunctional accelerator based on substituted urea. It is usually used as an accelerator of DICY, allowing a reduction of the polymerisation temperature of the epoxy formulation up to 80 °C. The resulting crosslinked matrix shows a dense polymeric network, characterised by good mechanical performance. Despite its high reactivity, Dyhard UR500 can also be applied as a single crosslinker and latencies of up to 2 months are possible. In addition, thanks to its low enthalpy development during the hardening process, it is particularly suitable for thick laminates reinforced with carbon fibre.
  • Manganese (II) acetylacetonate (produced and marketed by Merck®) is a metal complex that can be adopted as a catalyst for the cyanate-ester resins to promote the cyclotrimerization reaction .
  • the binder with formulation Fl has high tackiness, viscosity at 50 °C 20 Pa -s and density at 25 °C 1.17 g/cm 3 and was obtained with the following methodology.
  • a quantity of Araldite GY 2600 (60 g) preheated to 50 °C and Araldite GT 7071 (40 g) was introduced in a 250 ml glass beaker, mixed with a spatula and heated in a furnace at 120 °C for 1 hour. The mixture was stirred with a spatula every 15 minutes to ensure complete dissolution of the solid component, obtaining a colourless and clear mixture.
  • the binder with formulation F2 was obtained with the following methodology .
  • the binder with formulation F3 was obtained with the following methodology .
  • a quantity of HyPox RA95 ( 80 g) preheated to 70 ° C and Araldite GT 7071 ( 20 g) was introduced in a 250 ml glass beaker, mixed with a spatula and heated in the furnace at 120 ° C for 1 hour .
  • the mixture was stirred with a spatula every 15 minutes to ensure complete dissolution of the solid component .
  • the resulting mixture was cooled to 70 ° C and a quantity of Dyhard 100S ( 8 g) and Dyhard UR500 ( 2 g) was added .
  • the final formulation was then vigorously stirred with a spatula to obtain a homogeneous white mixture .
  • the binder with formulation F4 was obtained with the following methodology .
  • a quantity of Primaset PT-30 ( 100 g) preheated to 50 ° C and Manganese ( 11 ) Acetylacetonate ( 1 g) was introduced in a 250 ml glass beaker .
  • the resulting mixture was then vigorously stirred with a spatula to obtain a brownish mixture .
  • Example 2
  • This example describes the methodology for measuring the glass transition temperature (Tg) and determining the Tg for the binders described in Example 1.
  • Tg values of fresh pure resins were determined by performing DSC measurements from -40 °C to 50 °C under a constant nitrogen flow (50 ml/min) .
  • the analyses were performed on a Mettler-Toledo DSC 1 provided with an autosampler using 40 pl aluminium crucibles with a perforated lid. A quantity of 6-10 mg of fresh resin was used for the analysis.
  • the DSC method applied for the analyses is reported as follows.
  • Step 1 isothermal at -40 degrees Celsius for 1 minute, under N2 50 ml/min
  • Step 2 scan from -40 °C to 50 °C, 10 °C/min, under N2 50 ml/min .
  • the Tg determination was carried out using only the curve of step 2.
  • the scanning temperature interval from -40 to +50 °C was chosen as the glass transition temperature should fall in this region.
  • the glass transition values were determined according to ASTM D3418-15, wherein the Tg is equal to the average value between T1 and T2 as shown in Figure 3.
  • the scanning start temperature may be suitably set below -40 °C to improve the readability and the reliability of the Tg calculation.
  • the scanning start temperature may be suitably set below -40 °C to improve the readability and the reliability of the Tg calculation.
  • the value of the glass transition temperature is expected to be around -60 °C
  • a scanning start temperature of -90 °C can be conveniently used for DSC measurement.
  • Equipment with scanning temperatures starting from -150 °C is used to measure glass transition temperatures below -60 °C.
  • This example describes the manufacture of the composite material 1. The following is used as starting material.
  • a surface film FS011-200-20-1260 G (code MF020001200) , which is a commercial product manufactured and marketed by Delta-Preg SpA (Loc. Bonifica del Tronto km 16, 64016 Sant'Egidio alia Vibrata (TE) ) , is a film composed of a resin system and of a support and has the following characteristics: resin FS011, resin areal weight 200 g/m 2 , polyester fibre support, support areal weight 20 g/m 2 , theoretical sheet thickness 0.15 mm.
  • the resin FS011 (product manufactured by Delta-Tech SpA) has the following characteristics and properties: maximum achievable DMA Tg of 160 °C; processing through curing in vacuum bag in autoclave, vacuum bag in furnace and compression moulding; 30 days of preservability at 20 °C; chemical nature Thermosetting Epoxy Resin; polymerisation temperature interval from 80 to 135 °C; density of the pure polymerised resin 1.48 g/cm 3 ; very high dynamic viscosity; average tackiness.
  • the binder Fl after preheating to a temperature of 55 °C, was spread through continuous filming process (with rotating rollers at a temperature of 55 °C) on a support (in particular silicone paper) , obtaining a continuous layer of the binder Fl with an areal grammage of 50 g/m 2 .
  • This intermediate material is identi fied by the code M-LAB-22035 and corresponds to the description BINDER1- 050/GG250X ( T700S ) (H 127 cm) .
  • the composite material thus obtained was laminated at room temperature together with the surface film FS 011-200-20- 1260 G so as to put in direct contact the surface of the reinforcement CBX250R-CAT C020250R00A200002 wetted by the binder Fl with the polyester support of the surface film FS 011-200-20- 1260 G .
  • the resulting composite material 1 was then wound in the form of a roll .
  • a relevant aspect of the production process of the composite material 1 concerns the coupling of the dry reinforcement CBX250R-CAT with the layer of binder Fl .
  • the binder does not wet all the fibre of the reinforcement , so that the rear layer remains at least partially dry . It is likewise important that a dryness level of the reinforcement CBX250R-CAT is also preserved following the coupling of the intermediate material with the surface film .
  • the composite material 1 as described in Example 3 , has a suf ficient adhesive stability such that it can be used and handled for lamination operations .
  • the presence of the binder thanks to its tacky character, guarantees an adequate adhesion between the reinforcement CBX250R-CAT C020250R00A200002 and the surface film FS011-200-20-1260 G, which would otherwise tend to separate, complicating manual lamination operations.
  • the present example describes the procedure for the quantification of the adhesion force (connection force) exerted by the binder of formulation Fl between the surface film and the reinforcement CBX250R-CAT - C020250R00A200002, evaluated through dynamometric measurements under sliding conditions of the two layers.
  • the measurements were performed on 5 specimens for each material (in other words, 5 specimens for material M-LAB22046 and 5 specimens for material M-LAB22036) by using an MTS Insight dynamometer, provided with a 100 N load cell and configured to perform tensile measurements .
  • the applied measurement speed was 2 mm/min . All the measurements were carried out at a temperature of 2011 ° C .
  • the specimens of composite material 1 necessary for the measurements were obtained using the template schematically represented in Figure 4 ( and photographed in Figure 5 ) .
  • This tool handcrafted by a mechanical workshop, is constituted by a metal frame 8 mm thick, having external dimensions 300x75 mm, internal dimensions 250x25 mm and two slits of approximately 15 mm in length and 8 mm in depth placed along each internal corner .
  • the preparation of the specimens was carried out at a temperature of 2011 ° C .
  • Each specimen was obtained on the basis of the procedure reported below :
  • the specimen In the case of use of woven fabrics , stitched unidirectional fabrics , multiaxial fabrics of various kind as reinforcement 4 , the specimen must be aligned to the direction with the highest fibre content , in order to minimi ze the deformation of the specimen itsel f during the dynamometric test before the relative breakage . In other cases , the orientation of the template must coincide with the direction of greater tensile elastic modulus (ASTM D3039-3039M- 08 ) .
  • each specimen was suitably trimmed for the creation of the gripping areas , necessary for the coupling of the specimen to the clamps of the dynamometer .
  • these operations were carried out by using the trimming tool schematically shown in Figure 6 .
  • This tool handcrafted by a mechanical workshop, is constituted by a thin bent metal sheet about 1 mm thick, on the front side of which and near the lower edge there is a slit .
  • Always on the same side at a height of 25 mm from the lower edge , there is also a demarcation line , used to check the length of the flap of material to be trimmed .
  • the trimming procedure applied is reported below : - Once the polyethylene layer (protective layer covering the reinforcement 4 ) has been removed from the reinforcement 4 , place the specimen on a cutting plane , with the layer of surface film 2 facing downwards ;
  • each specimen thus obtained is constituted by two gripping areas with dimensions of approximately 25x25 mm, one corresponding to the sole reinforcement (CZ1) and one to the sole surface film (CZ2) , and an overlapping area between the two layers (TZ) with dimensions of approximately 200x25 mm.
  • the stress indicates the connection stress, which is calculated by dividing the connection force of each specimen by the overlapping area between the layers (expressing the results in kPa) .
  • the two versions of composite material 1 characterised by a different areal weight of the layer of binder 3, they provided a different force value in the test configuration adopted.
  • the version with 17 g/m 2 provided a significantly lower value of 1.6 N (average value) .
  • thermosetting resin i . e . the ability of the material to be easily deformed in order to adhere and conform to the shape and geometry of the mould .
  • a high drapability of fers in fact , the advantage of being able to carry out laminations on moulds with complex geometries in a shorter time , reducing the overall production time of the component .
  • Aim of the present example consists in evaluating the drapability of the composite material 1 with respect to the comparison materials , through the moulding of a laminate according to an appropriate geometry .
  • the tested solutions di f fer based on the level of impregnation of the reinforcements , their possible prelayering format and the nature , quantity and distribution of the resin matrices .
  • pre-layering refers to the practice of j oining two or more layers , whether they are prepregs , resin layers or dry fabrics or a combination thereof , into a single roll . These pre-layered are typically available from prepreg manufacturers .
  • the moulding can then be carried out by sequentially laminating the distinct layers or the pre-layered materials on the mould .
  • the loss of drapability of the prelayered systems is a very common fact that has greatly limited their spread .
  • the increased di f ficulty of the laminator to follow the shapes of the mould results in a greater overall lamination time and/or a lower quality in terms of finishing of the moulded component.
  • resin FS011 resin areal weight 200 g/m 2 , polyester fibre support, support areal weight 20 g/m 2 , theoretical sheet thickness 0.15 mm.
  • the resin FS011 product manufactured by Delta-Tech SpA
  • thermosetting resin system It is a multiaxial fabric impregnated with a thermosetting resin system and has the following characteristics: the carbon fibre reinforcement, having an areal weight of 265 g/m 2 , biaxial weaving style ⁇ 45°, first layer with a weight of 125 gsm, fibre T700SC 12K 50C and angle -45°, second layer with a weight of 125 gsm, fibre T700SC 12K 50C and angle +45°, stabilisation thread E glass, polyester stitching thread, chain stitching mode, is impregnated with the resin system DT150; the material has a nominal resin content of 40% by weight and a theoretical moulded sheet thickness of 0.28 mm.
  • the resin DT150 (product manufactured by Delta-Tech SpA) has the following characteristics: maximum achievable DMA tg of 140 °C; processing through curing in vacuum bag in autoclave and compression moulding; 30 days of preservability at 21 °C; average tackiness; chemical nature Thermosetting Epoxy Resin; polymerisation temperature interval from 120 to 150 °C; density of the pure polymerised resin 1.24 g/cm 3 ; average dynamic viscosity, 500-1000 Poise at 60 °C.
  • thermosetting resin system It is a woven fabric impregnated with a thermosetting resin system and has the following characteristics: the carbon fibre reinforcement, having an areal weight of 600 g/m 2 , type of yarn T700SC 24K 50C, weaving style Twill 2x2, warp 1.80 threads/cm, weft 1.80 threads/cm, is impregnated with the resin system DT150; the material has a nominal resin content of 38% by weight and a theoretical moulded sheet thickness of 0.63 mm.
  • the characteristics of the resin system DT150 are similar to those described for Material P2.
  • the surface film is represented by FS011-200-20-1260 G (code MF020001200) , corresponding to Material Pl described above.
  • the carbon reinforcement impregnated with thermosetting resin is represented by GG250X (T700) -DT150-40 (code PGG250B0340) , corresponding to Material P2 described above.
  • the lamination provides for the less resinrich side of the surface film FS011-200-20-1260 G (code MF020001200) to be placed in direct contact with the GG250X (T700) -DT150-40 (H 127 cm) (code PGG250B0340 ) .
  • the moulding tests were carried out by using a disc-shaped aluminium mould (diameter 180 mm) , characterised by the presence in the centre of a convex paraboloid relief with a height of 31.5 mm ( Figure 10) . Before each test, the mould was suitably treated following the procedure described below. The aluminium mould was cleaned with a cloth and a thinner
  • the release agent Marbocote® PK4 was applied, which i s produced by Marbocote Ltd (Unit 9 , Dalton Way, Middlewich Cheshire , CW10 OHU, United Kingdom) and has the following characteristics : transparent liquid appearance , composition polymeric resin in a mixture of non-chlorinated organic solvents , speci fic weight 0 . 756 g/cm 3 , ideal application temperature between 20-30 ° C, thermal stability 250 ° C, coverage 80- 100 m 2 /L, storage time 12 months .
  • the Marbocote PK4 was applied with a clean and dry cloth in a homogeneous manner, covering the entire surface of the mould; overall , five coats were applied, awaiting 10 minutes between one coat and the other . After applying the last coat and having observed the complete drying of the film of release agent , the mould was left at room temperature for 60 minutes , in order to obtain a complete cure of the product .
  • the material Pl was laminated in direct contact with the mould (having taken care to laminate the resinrich side in direct contact with the mould Figure 11A) ;
  • the material P2 was laminated in contact with the first layer ( Figure 11B) ;
  • the material P3 was laminated in contact with the second layer ( Figure 11C) .
  • the material P4 was laminated in direct contact with the mould (having taken care to place the side of the surface film FS011-200-20-1260 G (code MF020001200) in direct contact with the mould Figure 12A) ;
  • the material P3 was laminated in contact with the first layer ( Figure 12B) .
  • the material P5 was laminated in direct contact with the mould (having taken care to place the side of the surface film FS011-200-20-1260 G (code MF020001200) in direct contact with the mould Figure 13A) .
  • the material P3 was laminated in contact with the first layer, i.e. the material P5 ( Figure 13B) .
  • Vacuum Bag G Airtech Wrightlon® 600V-LFT , 50 pm
  • Aerator H Airtech Airwave® N10
  • the actual moulding step began, i.e. the step of curing the thermosetting matrix of the moulding material.
  • the sealed mould was placed inside an autoclave, model AIC 1300X3000 produced by Italmatic Presse Stamp! srl, and subjected to the curing cycle, by applying the following parameters :
  • the particular geometry of the mould used requires a strong drapability of the material to be laminated, in order to obtain a moulded piece without wrinkles and with a good superficial finish .
  • i f the layer to be laminated has a low drapability
  • the presence of the relief in the centre of the mould results in the immediate formation of folds during the deposition step of the layers , due to the impossibility of adequately conforming each layer to the peculiar geometry .
  • the superior drapability and softness of the composite material 1 (P5) is to be attributed to the presence of dry and non-impregnated fibres of the reinforcement 4.
  • the (at least partial) absence of a resin matrix inside the reinforcement confers an exceptional mobility of the fibres that can therefore deform during the lamination step, offering a high capability of adaptation of the material to the geometry of the mould, albeit complex.
  • the presence of the resin matrix inevitably imparts less mobility to the fibres . Consequently, each layer experiences a higher sti f fness during lamination that corresponds to a higher resistance to conforming to the geometry of the mould .
  • Aim of present test consists in evaluating the quality of the moulded components and measuring the saving in terms of lamination time of fered by the composite material 1 compared to the traditional materials , using the 3 di f ferent configurations o f moulding material shown in the previous example .
  • the moulding tests were carried out using a composite mould ( Figure 18 ) , whose geometry, by shape and dimensions , can probably represent a medium complexity component of a body of a motor vehicle . Before each test , the mould was suitably treated following the procedure described below relative to the preparation of the mould .
  • the carbon mould was cleaned initially with a thinner ( acetone ) and then with the cleaner Chemiease® Mold Cleaner EZ .
  • the pore sealer Marbocote® Mould Sealer was applied which is produced by Marbocote Ltd (Unit 9 , Dalton Way, Middlewich Cheshire , CW10 OHU, United Kingdom) and has the following characteristics : transparent and colourless liquid appearance , aliphatic hydrocarbon composition, flash point ⁇ 10 ° C, stability of the cured film 250 ° C, coverage 80- 100 m 2 /L per coat , type of application rubbing and spreading, storage time 12 months .
  • the use of the pore sealer eliminates the microporosities and the small scratches potentially present on the surface of the composite moulds , providing a smooth and glossy surface .
  • two coats of Marbocote Mould Sealer were appl ied to the mould 10 minutes apart from each other and finally the mould was placed in the furnace for 10 minutes at 60 ° C in order to obtain complete polymerisation of the product .
  • the release agent Marbocote® PK4 was applied, similarly to what is reported in Example 5 ; overall , three coats were applied, awaiting 10 minutes between one coat and the other . After applying the last coat and having observed the complete drying of the film of release agent , the mould was left at room temperature for 60 minutes , in order to obtain a complete cure of the product .
  • the lamination step of the moulding material was implemented on the mould, reali zing the three configurations A, B, C reported in Example 5 on the basis of the procedure detailed above .
  • the autoclave moulding was performed, by applying the curing cycle described in Example 5 .
  • the various tests have provided cured laminates with completely comparable structural characteristics and superficial finishes . More in particular, as shown in Figure 19 , in terms of superficial quality, the three di f ferent moulding tests led to cured pieces having a similar superficial finish, without porosity and with a homogeneous coverage of the surface film .
  • Test N3 thanks to the presence of the composite material 1 (P5) , provided the best result, requiring less "operator's time".
  • the reduction by about 58% in the lamination time recorded in Test N3 is to be attributed to a lower number of layers to be laminated and to the higher drapability of the composite material 1 (P5) compared to the material Pl which results in an easier and faster placement of the first layer against the mould.
  • Test N2 in which the number of layers to be laminated is the same as Test N3, the reduction by about 55% in the lamination time is offered by a higher drapability of the composite material 1 (P5) compared to the material P4.
  • the use of the composite material 1 (P5) allows, in general, to avoid long intermediate air removal (debulking) operations during the lamination step.
  • air removal cycles through the vacuum bag and pump are often essential, which cause a lengthening of the lamination times and loss of production efficiency.
  • the composite material 1 (P5) instead, of the composite material 1 (P5) , the debulking operations can be conveniently avoided, consequently obtaining a greater production efficiency with the same superficial quality.
  • the presence of the reinforcement 4 at least partially not impregnated in the composite material 1 (P5) guarantees an effective medium of evacuation of all the air present between the layers at the time of lamination, which is removed directly in the moulding step.
  • the moulding process performed for this example is represented by the autoclave moulding.
  • Alternative moulding processes, such as for example compression moulding differ in the fact that they do not provide for the presence of the vacuum bag.
  • the comparison in terms of the lamination times object and main objective of present example still remains valid.

Abstract

Matériau composite (1) servant à fabriquer des articles par moulage ; le matériau composite (1) possède un film de surface (2) qui comprend une formulation de résine présentant un poids surfacique allant jusqu'à environ 700 g/m2 ; un renfort (4) qui est constitué d'un premier matériau fibreux au moins partiellement sec présentant un poids surfacique allant jusqu'à environ 900 g/m2 ; et au moins un liant (3) qui lie le film de surface (2) au renfort (4) et qui, selon certains modes de réalisation, équivaut à une résine interposée entre le film de surface (2) et le renfort (4).
PCT/IB2023/058222 2022-08-19 2023-08-16 Matériau composite WO2024038387A1 (fr)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3330081A1 (fr) * 2016-12-05 2018-06-06 Gurit (UK) Ltd. Panneaux composites
EP3331689B1 (fr) * 2015-08-05 2021-06-09 Hexcel Composites Limited Matériaux de moulage à finition de surface améliorée

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3331689B1 (fr) * 2015-08-05 2021-06-09 Hexcel Composites Limited Matériaux de moulage à finition de surface améliorée
EP3330081A1 (fr) * 2016-12-05 2018-06-06 Gurit (UK) Ltd. Panneaux composites

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