WO2017042921A1 - 複合材料の製造方法、複合材料の製造装置および複合材料用プリフォーム - Google Patents
複合材料の製造方法、複合材料の製造装置および複合材料用プリフォーム Download PDFInfo
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- WO2017042921A1 WO2017042921A1 PCT/JP2015/075648 JP2015075648W WO2017042921A1 WO 2017042921 A1 WO2017042921 A1 WO 2017042921A1 JP 2015075648 W JP2015075648 W JP 2015075648W WO 2017042921 A1 WO2017042921 A1 WO 2017042921A1
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- adhesive
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- preform
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—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
- B29C70/48—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 and impregnating the reinforcements in the closed mould, e.g. resin transfer moulding [RTM], e.g. by vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
- B29C39/10—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles incorporating preformed parts or layers, e.g. casting around inserts or for coating articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/24—Feeding the material into the mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/38—Heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—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
- B29C70/44—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding
- B29C70/443—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding and impregnating by vacuum or injection
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
- B29C70/546—Measures for feeding or distributing the matrix material in the reinforcing structure
-
- 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
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
- B29C70/546—Measures for feeding or distributing the matrix material in the reinforcing structure
- B29C70/547—Measures for feeding or distributing the matrix material in the reinforcing structure using channels or porous distribution layers incorporated in or associated with the product
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
- B29C70/541—Positioning reinforcements in a mould, e.g. using clamping means for the reinforcement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/106—Carbon fibres, e.g. graphite fibres
Definitions
- the present invention relates to a composite material manufacturing method, a composite material manufacturing apparatus, and a composite material preform.
- a preform formed by laminating a reinforced base material and preformed into a predetermined shape is placed in a cavity in a mold.
- a resin is injected into the cavity from the injection port, and the reinforced base material is impregnated with the resin.
- the composite material is completed by curing the resin injected into the cavity. While the resin is being injected, a clamping pressure is applied using a predetermined press so that unintended mold opening of the mold due to an increase in the pressure in the cavity does not occur (Patent Document 1). See).
- the resin injected into the cavity flows while spreading in the cavity, and the preform from the region where the resin near the injection port easily flows in the preform disposed in the cavity. It moves to the region where the resin is difficult to flow, such as the peripheral edge of. Since the injected resin passes while impregnating the inside of the reinforced base material in the process of flowing in the cavity, it takes a long time for injection to reach the resin in a region where the resin is difficult to flow, Prolongs molding time. For this reason, in order to inject the resin in a short time, since the injection pressure must be set to a high pressure, a large press machine capable of applying a larger mold clamping pressure must be used. In addition, since the equipment for injecting the resin needs to have high performance capable of high-pressure injection, an increase in capital investment cost due to the use of the equipment for high-pressure injection is also a problem.
- the present invention has been made to solve the above-described problems, and by controlling the resin flow in the cavity, the molding time can be shortened and the capital investment cost can be reduced. It is an object of the present invention to provide a composite material manufacturing method, a composite material manufacturing apparatus, and a composite material preform.
- the method for producing a composite material according to the present invention for achieving the above object is a method for producing a composite material comprising a reinforced base material and a resin impregnated in the reinforced base material.
- the adhesive is applied to the sheet-shaped reinforced base material including the first region and the second region so that the density of the adhesive in the second region is lower than that of the first region.
- Preforming the reinforced base material to form a preform placing the preform in a cavity in the mold, injecting the resin into the cavity from the injection port of the mold,
- the composite material is molded by impregnating the resin. Compared to the portion of the cavity where the second region of the reinforced substrate is disposed, the resin injected into the cavity is more likely to flow than the portion of the reinforced substrate where the first region is disposed. To do.
- An apparatus for manufacturing a composite material according to the present invention includes a provision unit that applies an adhesive to a sheet-shaped reinforcing base material including a first region and a second region, and reserves the reinforcing base material.
- a control unit for controlling the operation. The controller controls the operation of the application unit so that the adhesive density of the second region of the reinforced base material is lower than that of the first region of the reinforced base material and the adhesive is applied. Controlling the portion of the cavity where the second region of the reinforced substrate is disposed compared to the portion of the reinforced substrate where the first region is disposed, Make the resin easier to flow.
- the composite material preform according to the present invention that achieves the above object is formed by impregnating an adhesive into a sheet-like reinforced substrate having a first region and a second region.
- the second region is formed so that the density of the adhesive is lower than that of the first region.
- FIG. 2 (A) is a general
- FIG. 2 (B) is a general
- FIGS. 3A and 3B are views for explaining a preforming apparatus for molding a preform according to an embodiment of the present invention
- FIG. 3A is an overview perspective view of a cutting portion
- FIG. 3B is an overview of a preforming die. It is a perspective view.
- FIG. 6 is a conceptual diagram illustrating the principle of the present invention, and is a view of a state in which a resin flows between layers of a laminate of a reinforced base material as viewed from the side
- FIG. 6B is a diagram illustrating a state of the preform according to the embodiment
- FIG. 6B is a diagram illustrating a state in which resin is injected into the preform according to the embodiment of the present invention
- FIG. 6B is a diagram illustrating a state in which resin is injected into the preform according to the embodiment of the present invention.
- FIG. 7 is a conceptual diagram for explaining the principle of the present invention.
- FIG. 7 is a view of the flow of the resin in the mold in which the reinforcing base material is disposed, as viewed from the upper surface.
- FIG. 7 It is a figure which shows the state which inject
- FIG. 7 (B) is a figure which shows the state which inject
- FIG. 8 is a photograph for showing the evaluation result of the disordered state of the orientation of the reinforced substrate due to the flow of the resin, and FIG.
- FIG. 8A is a state in which the resin is flowed through the preform according to the embodiment of the present invention.
- FIG. 8B shows a state in which a resin is flowed through the preform according to the comparative example. It is a figure which shows the time transition of the pressure in the cavity at the time of implementing the manufacturing method of the composite material which concerns on embodiment. It is a flowchart which shows the shaping
- FIG. 1 is a diagram for explaining the overall flow of a manufacturing apparatus 100 and a manufacturing method for a composite material 400 according to an embodiment of the present invention.
- 2 and 3 are views for explaining a preforming apparatus 200 for forming a preform 500 (corresponding to a composite material preform) according to an embodiment of the present invention.
- FIG. 4 is a schematic view of a molding apparatus 300 that molds the composite material 400 using the preform 500 according to the embodiment of the present invention.
- FIG. 5 is a diagram schematically illustrating a state in which the preform 500 according to the embodiment of the present invention is placed in the mold 310 and the resin 600 is injected.
- 6 and 7 are conceptual diagrams for explaining the principle of the present invention.
- FIG. 1 is a diagram for explaining the overall flow of a manufacturing apparatus 100 and a manufacturing method for a composite material 400 according to an embodiment of the present invention.
- 2 and 3 are views for explaining a preforming apparatus 200 for forming a preform 500 (corresponding to a composite material preform) according
- FIG. 8 is a photograph for showing an evaluation result of the disordered state of orientation of the reinforced substrate 510 due to the flow of the resin 600.
- FIG. 9 is a diagram illustrating a time transition of the pressure in the cavity 350 when the method for manufacturing the composite material 400 according to the embodiment is performed.
- FIG. 10 is a flowchart showing a method of forming the preform 500 according to the embodiment of the present invention.
- FIG. 11 is a flowchart showing a method of forming the composite material 400 according to the embodiment of the present invention.
- FIG. 12 is a perspective view showing automobile parts 701 to 703 and a vehicle body 700 using the composite material 400 according to the embodiment of the present invention.
- FIG. 3 (A) has shown the conveyance direction (direction which goes to a downstream process) of the reinforced base material 510 by the conveyance part 210.
- FIG. 3 (B) has shown the shaping
- FIG. 5 and 6 indicate the flow direction of the resin 600.
- the preform 500 is formed by impregnating a reinforcing substrate 510 with an adhesive 520.
- the reinforced substrate 510 can be formed of, for example, carbon fiber, glass fiber, organic fiber, or the like.
- carbon fiber is used as the reinforcing base 510
- the carbon fiber 510 is suitable as a reinforced base material 510 for the composite material 400 such as the automobile body 700 because the carbon fiber 510 has a small coefficient of thermal expansion, excellent dimensional stability, and little deterioration in mechanical properties even at high temperatures.
- the carbon fiber 510 is, for example, a so-called NCF in which a UD (unidirectional) material in which fibers are aligned in one direction or a plurality of sheets in which fibers are aligned in one direction are stacked in different directions and integrated with auxiliary fibers.
- a sheet-like reinforcing substrate 510 such as a (non-crimp fabric) material can be used.
- the laminated structure depends on material properties required for the composite material 400 that is a molded product, but is generally laminated so as to have a plurality of orientation angles. In this embodiment, it is set as the laminated structure which laminates
- the adhesive 520 is applied to the carbon fibers 510 to bond the carbon fibers 510 to each other.
- the carbon fibers 510 can be stably maintained in a sheet-like form, and variations in the arrangement of the carbon fibers 510 can be suppressed.
- the laminated body 510b (refer FIG. 3 (B)) of the carbon fiber 510 is shape
- the adhesive 520 includes a first region 501 having a higher content density of the adhesive 520 and a content density of the adhesive 520 than that of the first region 501.
- the flow resistance of the resin 600 can be controlled by controlling the portion to which the adhesive 520 is applied and adjusting the content density distribution.
- the material constituting the adhesive 520 is not particularly limited as long as it is a material that is softened by heat, and a known material can be used.
- a known material can be used.
- thermoplastic resins such as polyolefin resins, styrene resins, nylon resins, and polyurethane resins
- thermosetting resins such as low molecular weight epoxy resins.
- a low molecular weight epoxy resin that is the same epoxy resin as that used for the composite material 400 described later, has high fluidity because of low melt viscosity, and is excellent in heat resistance and moisture resistance.
- the low molecular weight epoxy resin is not particularly limited as long as it has a viscosity low enough to impregnate the carbon fiber 510 before curing, and a known low molecular weight epoxy resin can be used.
- the composite material 400 according to the present embodiment is manufactured by impregnating a resin 500 into a preform 500 in which carbon fibers 510 are preformed in a predetermined shape and curing the preform.
- the composite material 400 has a higher strength and rigidity than a molded product composed of the resin 600 alone by combining the carbon fiber 510 and the resin 600.
- the composite material 400 is applied to a frame part such as a front side member 701 and a pillar 702 and an outer plate part such as a roof 703 used in an automobile body 700 (see FIG. 12B) as shown in FIG. By doing so, the weight of the vehicle body 700 can be reduced compared to a vehicle body constructed by assembling components made of steel materials.
- the composite material 400 according to the present embodiment is formed by impregnating the preform 500 with the resin 600.
- a core material 530 as shown in FIG. 3B is inserted into the composite material 400 to improve rigidity.
- the resin 600 is an epoxy resin, a phenol resin, or the like that is a thermosetting resin.
- an epoxy resin having excellent mechanical characteristics and dimensional stability is used.
- Epoxy resin is mainly a two-component type, and a main agent and a curing agent are mixed and used.
- the main agent is generally a bisphenol A type epoxy resin, and the curing agent is an amine-based one.
- the main agent is not particularly limited, and can be appropriately selected according to desired material characteristics.
- the resin 600 contains an internal mold release agent so that the mold can be easily removed after the composite material 400 is molded.
- the kind of internal mold release agent is not specifically limited, A well-known thing can be used.
- the core material 530 is formed inside the composite material 400 by impregnating the carbon fiber 510 with the resin 600 while being covered with the carbon fiber 510.
- the material which comprises the core material 530 is not specifically limited, A foam (foam core) is used preferably from a viewpoint of weight reduction.
- a foam made of polyurethane, vinyl chloride, polyolefin, acrylic resin, polyimide resin (PMI (polymethacrylimide), PEI (polyetherimide)) or the like is appropriately used.
- the manufacturing apparatus 100 for the composite material 400 will be described with reference to FIGS.
- the manufacturing apparatus 100 of the composite material 400 according to the present embodiment is roughly divided into a preforming apparatus 200 for forming the preform 500 shown in the upper and middle stages of FIG. 1 and a preform 500 shown in the lower stage of FIG. And a molding apparatus 300 for molding the composite material 400.
- the manufacturing apparatus 100 for the composite material 400 includes a control unit 110 that controls the operation of the entire manufacturing apparatus 100.
- the preforming apparatus 200 for forming the preform 500 will be described.
- the preforming apparatus 200 generally includes a conveying unit 210 that continuously conveys the carbon fibers 510, an applying unit 220 that applies an adhesive 520 to the carbon fibers 510, and an adhesive 520.
- a conveying unit 210 that continuously conveys the carbon fibers 510
- an applying unit 220 that applies an adhesive 520 to the carbon fibers 510
- an adhesive 520 Has a heater 230 that heats the carbon fiber 510 to which the carbon fiber 510 is applied, a cutting portion 240 that cuts the carbon fiber 510, and a preforming mold 260 that preforms the carbon fiber 510.
- the transport unit 210 continuously applies the carbon fiber 510 supplied from the base roll 510 a around which the carbon fiber 510 is wound, the application unit 220, the heater 230, and the cutting that are downstream processes.
- the conveyance unit 210 is configured by a belt conveyor.
- the imparting unit 220, the heater 230, and the cutting unit 240 are provided in accordance with the conveyance path of the belt conveyor, and are configured to be able to work continuously.
- the applying unit 220 is configured to be movable in the plane direction of the transport unit 210, and applies the adhesive 520 to the carbon fibers 510 transported from the upstream of the transport unit 210.
- the applied amount of the adhesive 520 depends on the type and physical properties of the adhesive 520 to be used, but can be set to, for example, 10 to 100 g / m 3 .
- the applying unit 220 may be a screen printing method using a powdery (solid) adhesive 520, an ink jet method using a liquid adhesive 520, or a non-woven fabric by processing the adhesive 520 into a nonwoven fabric. It can comprise by the method of laminating
- an inkjet method with high mass productivity and high application accuracy is used.
- the inkjet method is a method in which the adhesive 520 is atomized and sprayed directly onto the carbon fiber 510, and the application amount of the adhesive 520 can be adjusted depending on the portion to be applied.
- the heater 230 heats the carbon fiber 510 to which the adhesive 520 is applied by the applying unit 220.
- the heating temperature depends on the melting temperature of the adhesive 520 to be used, but is, for example, 70 ° C. to 150 ° C. Accordingly, the adhesive 520 can be softened or melted and impregnated in the carbon fiber 510.
- the content of the adhesive 520 per unit area of the carbon fiber 510 that is, the content density is determined.
- the density of the adhesive 520 depends on the shape of the composite material 400 and the thickness of the laminate 510b of the carbon fibers 510. For example, the density is 80 g / m 3 at the high density portion and 10 g at the low density density. / M 3 .
- the heater 230 is not particularly limited, it is preferable that the heater 230 is configured to be capable of heating the carbon fiber 510 instantaneously and uniformly.
- a heater such as a continuous furnace or a high-frequency coil, a far-infrared heater, or a hot air heater is used. Can be used.
- the cutting unit 240 cuts the carbon fiber 510 impregnated with the adhesive 520 along a predetermined cutting line L, as shown in FIG.
- the cutting unit 240 can use various cutting mechanisms such as ultrasonic cutting, laser cutting, circular saw cutting, press cutting, scissor cutting, and the like. In this embodiment, an ultrasonic cut that can be cut accurately in a relatively short time is used.
- the preforming mold 260 preforms the carbon fiber 510 into a predetermined three-dimensional shape.
- the lower mold 261 on which the carbon fiber 510 that is the target of the preform 500 is disposed, and the upper mold 262 that is movable toward and away from the lower mold 261 are provided.
- a molding surface corresponding to the shape matching the shape of the preform 500 of the carbon fiber 510 is formed.
- the carbon fiber 510 is molded into the preform 500 by applying an applied pressure to the carbon fiber 510 by moving the upper mold 262 closer to the lower mold 261 with the carbon fiber 510 disposed on the lower mold 261. Is possible.
- the mold 310 that forms the cavity 350 in which the preform 500 is disposed and the mold 310 that can be freely opened and closed, and a mold clamping pressure is applied to the mold 310. It has a press part 320, a resin injection part 330 for injecting molten resin 600 into the cavity 350, and a mold temperature adjusting part 340 for adjusting the temperature of the mold 310.
- the forming mold 310 has a pair of upper mold 311 (male mold) and a lower mold 312 (female mold) that can be opened and closed.
- a cavity 350 that can be sealed is formed between the upper mold 311 and the lower mold 312.
- the preform 500 is disposed in the cavity 350.
- the mold 310 further has an injection port 313 for injecting the resin 600 into the cavity 350.
- the injection port 313 communicates with the cavity 350 and the resin injection part 330.
- the surface of the mold 310 facing the cavity 350 includes a first wall surface 310a on the injection port 313 side and a second wall surface 310b on the side facing the injection port 313 as shown in FIG. .
- the second wall surface 310 b is a surface that is disposed at a position farthest from the injection port 313 on the surface facing the cavity 350 of the mold 310.
- the injection port 313 is located on the side of the preform 500 disposed in the cavity 350, the surface located on the side (left side in FIG. 4) The surface that is the first wall surface 310a and is located on the end portion (the right side in FIG. 4) of the preform 500 located on the side opposite to the side portion is the second wall surface 310b.
- the injection port 313 may be provided in the upper part of the mold 310.
- the resin 600 is impregnated from the upper part to the lower part of the preform 500.
- the lower mold 312 may be provided with a suction port for evacuating the cavity 350 to suck air.
- a sealing member or the like may be provided on the mating surface of the upper mold 311 and the lower mold 312 in order to make the inside of the cavity 350 hermetically sealed.
- the press unit 320 includes, for example, a cylinder 321 that uses fluid pressure such as hydraulic pressure, and can be configured by a press machine that can adjust the mold clamping pressure by controlling the hydraulic pressure or the like.
- the resin injection unit 330 is configured by a known circulation type pump mechanism that can be supplied to the mold 310 while circulating the main agent supplied from the main agent tank 331 and the curing agent supplied from the curing agent tank 332. Can do.
- the resin injection unit 330 communicates with the injection port 313 and injects the resin 600 into the cavity 350.
- the mold temperature adjusting unit 340 adjusts the temperature of the mold 310 so that the temperature in the cavity 350 is equal to or lower than the melting temperature of the adhesive 520 in the initial stage of the resin 600 injection. After the preform 500 is placed in the cavity 350, the resin 600 injected into the cavity 350 is cured by gradually heating to the curing temperature of the resin 600.
- a temperature adjustment mechanism that adjusts the temperature by circulating a heat medium such as oil, and the like Can be provided.
- control unit 110 controls the operation of the entire manufacturing apparatus 100.
- control unit 110 includes storage unit 111, calculation unit 112, and input / output unit 113 that transmits and receives various data and control commands.
- the input / output unit 113 is electrically connected to the applying unit 220, the heater 230, the cutting unit 240, the preforming die 260, the press unit 320, the resin injecting unit 330, and the mold temperature adjusting unit 340.
- the storage unit 111 includes a ROM and a RAM, and stores data such as the amount of adhesive 520 applied, the distribution of the first region 501 and the second region 502, the shape of the preform 500 and the composite material 400 to be molded.
- the calculation unit 112 is configured mainly with a CPU, and receives data such as a feed rate of the carbon fiber 510 by the transport unit 210 via the input / output unit 113. Based on the data read from the storage unit 111 and the data received from the input / output unit 113, the calculation unit 112 determines the application timing and amount of the adhesive 520, the heating temperature of the mold 310 by the mold temperature adjusting unit 340, and the like. Is calculated.
- a control signal based on the calculated data is transmitted to the applying unit 220, the heater 230, the cutting unit 240, the preforming die 260, the press unit 320, the resin injecting unit 330, and the mold temperature adjusting unit 340 via the input / output unit 113.
- the control unit 110 controls the application amount and application position of the adhesive 520, the operation of the preforming die 260, the clamping pressure of the molding die 310, the injection amount of the resin 600, the temperature of the molding die 310, and the like. .
- the manufacturing method of the composite material 400 is roughly divided into two steps: a step of forming the preform 500 shown in FIG. 10 and a step of forming the composite material 400 using the preform 500 shown in FIG.
- the step of forming the preform 500 is a sheet-like carbon fiber including a supply step (step S ⁇ b> 11) for supplying a carbon fiber 510 material, and a first region 501 and a second region 502. 510, an applying step (step S12) for applying the adhesive 520 so that the density of the adhesive 520 in the second region 502 is lower than that in the first region 501, and a heating step for heating the carbon fiber 510 (step S12).
- Step S13 a cutting process for cutting the carbon fibers 510 (Step S14), a stacking process for forming the stacked body 510b (Step S15), a transporting process for transporting the stacked body 510b (Step S16), and the carbon fibers 510
- a preforming step step S17 in which the preform 500 is preformed to form the preform 500;
- step S11 as shown in the upper part of FIG. 1, the carbon fiber 510 is pulled out from the base roll 510a formed by winding the carbon fiber 510, and the carbon fiber 510 is continuously supplied to the transport unit 210.
- step S12 as shown in FIG. 2A, an adhesive 520 is applied by the applying unit 220 to the carbon fibers 510 continuously sent out by the transport unit 210.
- the amount to be applied is adjusted according to a predetermined content density distribution. That is, the adhesive 520 is applied to the second region 502 of the carbon fiber 510 so that the density of the adhesive 520 is lower than that of the first region 501 of the carbon fiber 510.
- step S13 as shown in FIG. 2B, the carbon fiber 510 is heated by the heater 230, the applied adhesive 520 is softened or melted, and the adhesive 520 is impregnated between the layers of the carbon fiber 510. . By impregnating the adhesive 520, the content density distribution of the adhesive 520 is formed on the carbon fibers 510.
- step S14 as shown in FIG. 3A, the carbon fiber 510 is cut along the cutting line L in a state where the adhesive 520 is melted.
- the cutting line L is determined in advance according to the developed shape of the composite material 400 that is a molded product.
- step S15 a predetermined number of carbon fibers 510 cut by the transfer robot 250 are stacked as shown in the middle stacking step of FIG.
- carbon fibers 510 having different stacking orientations are stacked to form a predetermined stacked configuration.
- three types of fiber orientation are used: NCF material with ⁇ 45 ° direction, UD material with 90 ° direction, and UD material with 0 ° direction.
- the supplying process, the applying process, the heating process, and the cutting process are performed in lanes of different production lines, and the carbon fibers 510 cut for each orientation angle are stacked in a predetermined alignment order to form a stacked body 510b. .
- step S16 as shown in FIG. 3B, the laminated body 510b is conveyed to the lower mold 261 of the preforming mold 260 and arranged.
- the temperature during the conveyance is preferably managed so that the temperature of the carbon fiber 510 is lowered to 50 to 70 ° C., for example.
- the adhesive 520 can be brought into a semi-cured state or a cured state when the carbon fiber 510 is conveyed to the preforming mold 260. Thereby, since the adhesive 520 can be hardened in a short time at the time of preforming, the time required for preforming can be shortened.
- a preform 500 is formed by preforming a laminate 510b of carbon fibers 510 disposed on the lower mold 261 of the preforming mold 260.
- the core material 530 is disposed so as to be covered with the carbon fibers 510.
- the upper mold 262 may be constituted by a plurality of divided molds as shown in the middle preforming step of FIG. 1, or an upper mold composed of one undivided mold may be used.
- the preforming mold 260 is preferably cooled to 20 to 40 ° C., for example. As a result, the adhesive 520 is cooled at the same time as the mold is closed, and the adhesive 520 is cured to complete the preforming.
- step S18 when the preforming mold 260 is opened and the preform 500 is removed, the molding of the preform 500 is completed.
- the process of molding the composite material 400 includes a process of placing the preform 500 in the cavity 350 of the mold 310 (step S21) and a process of injecting the resin 600 into the cavity 350 (step S22). And a step of curing the resin 600 (step S23) and a step of removing the molded composite material 400 from the mold 310 (step S24).
- step S21 the preform 500 is placed in the cavity 350 of the mold 310 (see FIG. 4).
- the first region 501 of the carbon fiber 510 is disposed in the portion 351 in which the resin 600 in the cavity 350 easily flows, and the second region of the carbon fiber 510 in the portion 352 in which the resin 600 in the cavity 350 is difficult to flow.
- 502 is arranged.
- the temperature of the mold 310 is adjusted by the mold temperature adjusting unit 340 so that the temperature in the cavity 350 is equal to or lower than the melting temperature of the adhesive 520. Note that a portion 351 in which the resin 600 easily flows and a portion 352 in which the resin 600 hardly flows are obtained in advance by simulation based on the shape of the composite material 400 and the like.
- the resin 600 is easy to flow when the preform 500 including the laminate 510b of the carbon fibers 510 disposed in the cavity 350 is viewed from the side direction. It changes in the stacking direction of 510b. Specifically, a portion near the first wall surface 310a on the injection port 313 side of the mold 310 is a portion 351 where the resin 600 easily flows, and is close to the second wall surface 310b on the side facing the injection port 313. The portion is a portion 352 in which the resin 600 hardly flows. That is, the ease of flow of the resin 600 decreases from the first wall surface 310 a close to the injection port 313 toward the second wall surface 310 b far from the injection port 313. Therefore, as shown in FIG.
- the content density of the adhesive 520 decreases from the first wall surface 310a on the injection port 313 side toward the second wall surface 310b on the side facing the injection port 313.
- a first region 501 and a second region 502 of the carbon fiber 510 are disposed in the cavity 350.
- the resin 600 flows so as to spread concentrically from the injection port 313 as shown in FIG. 7B. Therefore, the vicinity of the injection port 313 is a portion 351 where the resin 600 easily flows, and the peripheral portion of the preform 500 away from the injection port 313 becomes a portion 352 where the resin 600 hardly flows.
- the resin 600 is impregnated in a fan shape from the side to the end of the preform 500. That is, the portion 351 in which the resin 600 easily flows is a side portion of the preform 500 close to the injection port 313, and the portion 352 in which the resin 600 does not easily flow is an end portion of the preform 500. Therefore, the density of the adhesive 520 on the side of the preform 500 is increased, and the density of the adhesive 520 decreases toward the end, so that the first region 501 and the second region 502 of the carbon fiber 510 decrease. Is placed in the cavity 350.
- step S22 the resin 600 is injected into the cavity 350.
- the ease of flow of the resin 600 decreases from the first wall surface 310a close to the injection port 313 toward the second wall surface 310b far from the injection port 313. Therefore, when the adhesive 520 is uniformly applied between the layers of the laminate 510b, a difference occurs in the flow rate of the resin 600, and the layer of the carbon fiber 510 may be displaced or twisted in a portion where the difference in the flow rate is large. is there. If the carbon fiber 510 layer is displaced or twisted, a resin-rich portion or a resin-only portion may be formed between the layers, which may cause a reduction in strength of the composite material 400 that is a molded product. .
- the content density of the adhesive 520 decreases from the first wall surface 310a on the injection port 313 side toward the second wall surface 310b on the side facing the injection port 313.
- the first region 501 and the second region 502 of the carbon fiber 510 are disposed in the cavity 350.
- the flow resistance of the resin 600 can be gradually decreased from the first wall surface 310a toward the second wall surface 310b. That is, the flow rate of the resin 600 that flows between the layers of the carbon fibers 510 on the first wall surface 310a side, which is the portion 351 in which the resin 600 easily flows, is slowed down, and the second wall surface that is the portion 352 in which the resin 600 hardly flows.
- the flow rate of the resin 600 flowing between the layers of the carbon fibers 510 can be gradually increased. Therefore, as shown in FIG. 6 (B), the resin 600 can easily flow between the layers of the carbon fibers 510. Thereby, the difference in the flow rate of the resin 600 between the layers of the carbon fibers 510 can be reduced, and wrinkles and kinks generated in the carbon fibers 510 can be suppressed.
- the preform 500 in which the carbon fibers 510 are disposed in the vicinity of the injection port 313 by the collision force due to the flow of the resin 600 Disturbance may occur in the orientation of the carbon fibers 510 in the surface layer.
- the flow velocity is generally high, so that the collision force due to the flow of the resin 600 tends to increase, and the orientation of the carbon fibers 510 tends to be disturbed.
- a resin-rich portion or a portion of only the resin 600 may be formed in a portion where the orientation of the carbon fiber 510 is disturbed, which may cause a decrease in strength or a design property of the composite material 400 that is a molded product. .
- the peripheral portion of the cavity 350 away from the injection port 313 is a portion 352 in which the resin 600 hardly flows because the resin 600 hardly reaches. Therefore, in order to resin 600 to reach the resin 600 in the hard portion 352 flow, as indicated by the broken line in FIG. 9, forced set the maximum injection pressure P 2 in the injection operation of the resin 600 to a high pressure . Moreover, setting the maximum injection pressure P 2 for filling the resin 600 to a high pressure, that amount is also increased pressure within the cavity 350. Therefore, in order to prevent inadvertent mold opening of the mold 310 during the pouring operation, a large press capable of applying a larger mold clamping pressure must be used.
- the portion 351 in which the resin 600 easily flows for example, the first region 501 is disposed in the vicinity of the injection port 313, and the portion 352 in which the resin 600 hardly flows, for example,
- the second region 502 is disposed at the peripheral edge of the cavity 350. Since the resin 600 hardly flows in the first region 501 disposed in the portion 351 in which the resin 600 easily flows, the resin 600 easily flows in other portions. As a result, it is possible to control the resin 600 to flow relatively easily in the second region 502 disposed in the portion 352 where the resin 600 is difficult to flow. Thus, since the resin 600 throughout the short time without increasing the injection pressure of the resin 600 can be reached, as shown in solid line in FIG.
- the resin 600 is injected from a plurality of locations by a mold having a plurality of injection ports (multi-point gates), and the resin 600 is difficult to flow into the portion 352.
- a method of reducing the maximum injection pressure of the resin 600 by facilitating the flow of 600 is also conceivable.
- a molding die having a plurality of injection ports is required, an increase in capital investment cost becomes a problem.
- equipment costs and manufacturing time increase due to maintenance such as cleaning of the resin 600 adhering to the holes of the injection ports.
- the resin 600 is easily flown into the portion 352 where the resin 600 is difficult to flow even if the mold 310 having one injection port 313 is used, and the maximum injection pressure P 1 of the resin 600 is reduced. Making it possible. Thereby, compared with the case where the shaping
- the resin 600 can reach the entire surface in a short time by controlling the resin 600 to flow easily in the portion 352 in which the resin 600 is difficult to flow.
- the resin 600 can reach the entire surface in a short time by controlling the resin 600 to flow easily in the portion 352 in which the resin 600 is difficult to flow.
- the temperature of the mold 310 is adjusted in advance so that the temperature in the cavity 350 is equal to or lower than the melting temperature of the adhesive 520.
- the adhesive 520 can be kept solid, the effect of blocking the injected resin 600 can be further enhanced, and the flow of the resin 600 can be controlled.
- step S23 the temperature of the mold 310 is gradually heated to the curing temperature of the resin 600, and the resin 600 impregnated in the carbon fiber 510 is cured.
- the temperature in the cavity 350 is increased by the heat of reaction accompanying the curing of the resin 600 and the heat of the mold 310, and the adhesive 520 is changed from solid to semi-solid or liquid. Softens.
- the effect of blocking the resin 600 by the adhesive 520 gradually decreases.
- the resin 600 is impregnated with the carbon fiber 510 where the adhesive 520 is softened when the composite material 400 is molded, and the high-quality composite material 400 is molded with the resin 600 almost uniformly impregnated throughout the carbon fiber 510. be able to.
- the resin 600 is formed of an epoxy resin
- the adhesive 520 is formed of a low molecular weight epoxy resin.
- the resin 600 and the adhesive 520 are formed of the same material when the composite material 400 is molded, the formation of the interface between the resin 600 and the adhesive 520 is suppressed, and the resin 600 and the adhesive 600 are integrated with each other.
- a homogeneous composite material 400 can be formed.
- the adhesive 520 has an effect of blocking the resin 600 and can control the flow of the resin 600.
- the adhesive 520 softens, and the resin 600 gradually spreads throughout the cavity 350, whereby the resin 600 and the adhesive 520 can be mixed more uniformly.
- step S24 after the resin 600 is cured, the molding die 310 is opened, and the composite material 400 in which the carbon fiber 510, the resin 600, and the core material 530 are integrated is removed from the mold, thereby completing the molding.
- the sheet-like carbon fiber 510 including the first region 501 and the second region 502 is provided with the first
- the adhesive 520 is applied so that the density of the adhesive 520 in the second region 502 is lower than that in the region 501, the carbon fiber 510 is preformed and preformed to form the preform 500.
- the preform 500 is placed in the cavity 350, and the preform 500 is impregnated with the resin 600 to mold the composite material 400.
- the portion of the cavity 350 where the second region 502 of the carbon fiber 510 is disposed is more easily flown through the resin 600 injected into the cavity 350 than the portion of the carbon fiber 510 where the first region 501 is disposed.
- the second region 502 is disposed in the portion 352 in which the resin 600 in the cavity 350 is difficult to flow, thereby being uniformly bonded to the carbon fiber 510.
- the resin 600 can easily flow into the portion 352 where the resin 600 hardly flows. Accordingly, the resin 600 can reach the entire carbon fiber 510 in the cavity 350 in a shorter time than when the adhesive 520 is uniformly applied to the carbon fiber 510.
- it is possible to reduce capital costs by the need to substantially increase the maximum injection pressure P 1 is eliminated.
- the adhesive 520 is applied so that the density of the adhesive 520 decreases from the first wall surface 310a on the injection port 313 side of the cavity 350 toward the second wall surface 310b on the side facing the injection port 313. .
- the flow rate of the resin 600 can be slowed by increasing the flow resistance of the resin 600 in the vicinity of the injection port 313, disorder of the orientation of the carbon fibers 510 in the vicinity of the injection port 313 can be suppressed.
- the difference in the flow rate of the resin 600 between the layers of the carbon fibers 510 can be reduced, and wrinkles and kinks generated in the carbon fibers 510 can be suppressed. Therefore, the strength and design properties of the composite material 400 can be improved.
- the adhesive 520 is formed of a material that is softened by heat. After the resin 600 is injected into the cavity 350, the mold 310 is heated, and the adhesive 520 is subjected to reaction heat and / or molding accompanying the curing of the resin 600. The mold 310 is softened by the heat. As a result, the resin 600 is impregnated with the carbon fiber 510 where the adhesive 520 is softened when the composite material 400 is molded, and the high-quality composite material 400 is molded with the resin 600 almost uniformly impregnated throughout the carbon fiber 510. be able to.
- it further includes a laminating step of laminating the carbon fibers 510 provided with the adhesive 520 to form a laminated body 510b between the applying step and the preforming step.
- the resin 600 is formed of an epoxy resin
- the adhesive 520 is formed of a low molecular weight epoxy resin.
- the second region 502 of the carbon fiber 510 is formed so that the density of the adhesive 520 is lower than that of the first region 501 of the carbon fiber 510.
- the adhesive 520 is formed of a material that is softened by heat.
- the carbon fiber 510 in the softened part of the adhesive 520 is impregnated with the resin 600, and the entire carbon fiber 510 is impregnated with the resin 600 almost uniformly.
- a high-quality composite material 400 can be formed.
- the heating step is performed before the cutting step, it may be performed after the cutting step or the laminating step.
- a composite material may be formed using a single reinforced base material.
- the composite material has the core material, it may be a composite material without the core material.
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Abstract
Description
本実施形態に係るプリフォーム500は、強化基材510に接着剤520を含浸させて形成される。
本実施形態に係る複合材料400は、炭素繊維510が予め所定の形状に予備成形されたプリフォーム500に樹脂600を含浸させて硬化させることによって製造される。
図1~4を参照して、複合材料400の製造装置100について説明する。本実施形態に係る複合材料400の製造装置100は、大きく分けて、図1の上段および中段に示すプリフォーム500を成形する予備成形装置200と、図1の下段に示すプリフォーム500を用いて複合材料400を成形する成形装置300と、から構成される。また、複合材料400の製造装置100は、製造装置100全体の動作を制御する制御部110を有する。
実施形態に係る複合材料400の製造方法を説明する。
110 制御部、
200 予備成形装置、
220 付与部、
260 予備成形型、
300 成形装置、
310 成形型、
310a 第1の壁面、
310b 第2の壁面、
313 注入口、
340 成形型温度調整部、
350 キャビティ、
400 複合材料、
500 プリフォーム(複合材料用プリフォーム)、
501 第1の領域、
502 第2の領域、
510 炭素繊維(強化基材)、
510b 積層体、
520 接着剤、
530 コア材、
600 樹脂。
Claims (11)
- 強化基材と前記強化基材に含浸された樹脂とを備える複合材料の製造方法であって、
第1の領域と第2の領域とを備えるシート状の前記強化基材に、前記第1の領域よりも前記第2の領域の接着剤の含有密度が低くなるように前記接着剤を付与し、
前記強化基材を予備成形してプリフォームを形成し、
成形型内のキャビティに前記プリフォームを配置し、
前記成形型の注入口から前記キャビティ内に前記樹脂を注入し、前記プリフォームに前記樹脂を含浸させて前記複合材料を成形してなり、
前記キャビティのうち前記強化基材の前記第2の領域が配置された部分を前記強化基材の前記第1の領域が配置された部分に比べて、前記キャビティ内に注入した前記樹脂が流れやすくする、複合材料の製造方法。 - 前記接着剤を付与する際に、前記成形型の前記注入口側の第1の壁面から前記注入口と対向する側の第2の壁面に向かって、前記接着剤の含有密度が低下するように前記接着剤を付与する、請求項1に記載の複合材料の製造方法。
- 前記接着剤は、熱によって軟化する材料によって形成され、
前記樹脂を前記キャビティ内に注入した後に、前記成形型を加熱し、
前記接着剤を前記樹脂の硬化に伴う反応熱および/または前記成形型の熱によって軟化させる、請求項1または請求項2に記載の複合材料の製造方法。 - 前記接着剤を付与した後、前記プリフォームを形成する前に、前記接着剤を付与した前記強化基材を積層して積層体を形成する、請求項1~3のいずれか1項に記載の複合材料の製造方法。
- 前記樹脂は、エポキシ樹脂によって形成され、
前記接着剤は、低分子量エポキシ樹脂によって形成される、請求項1~4のいずれか1項に記載の複合材料の製造方法。 - 第1の領域と第2の領域とを備えるシート状の強化基材に接着剤を付与する付与部と、
前記強化基材を予備成形してプリフォームを形成する予備成形型と、
前記プリフォームが配置されるキャビティを形成し、前記キャビティ内に樹脂を注入する注入口を備える成形型と、
前記付与部および前記予備成形型の作動を制御する制御部と、を有し、
前記制御部は、前記強化基材の前記第1の領域よりも前記強化基材の前記第2の領域の前記接着剤の含有密度が低く前記接着剤を付与するように前記付与部の作動を制御して、前記キャビティのうち前記強化基材の前記第2の領域が配置された部分を前記強化基材の前記第1の領域が配置された部分に比べて、前記キャビティ内に注入した前記樹脂が流れやすくする、複合材料の製造装置。 - 前記成形型は、前記注入口側の第1の壁面と、前記注入口と対向する側の第2の壁面と、を有し、
前記制御部は、前記付与部を制御して、前記第1の壁面から前記第2の壁面に向かって、前記接着剤の含有密度が低下するように前記接着剤を付与する、請求項6に記載の複合材料の製造装置。 - 前記成形型の温度を調整する型温度調整部をさらに有し、
前記制御部は、前記型温度調整部の作動を制御して前記成形型を加熱し、
前記接着剤は、熱によって軟化する材料によって形成され、前記樹脂の硬化に伴う反応熱および/または前記成形型の熱によって軟化する、請求項6または請求項7に記載の複合材料の製造装置。 - 前記樹脂は、エポキシ樹脂によって形成され、
前記接着剤は、低分子量エポキシ樹脂によって形成される、請求項6~8のいずれか1項に記載の複合材料の製造装置。 - 第1の領域と第2の領域とを備えるシート状の強化基材に接着剤を含浸させて形成される複合材料用プリフォームであって、
前記強化基材の前記第2の領域は、前記強化基材の前記第1の領域よりも前記接着剤の含有密度が低くなるように形成される、複合材料用プリフォーム。 - 前記接着剤は、熱によって軟化する材料によって形成される、請求項10に記載の複合材料用プリフォーム。
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EP3348371B1 (en) | 2020-08-12 |
JP6439879B2 (ja) | 2018-12-26 |
BR112018004669B1 (pt) | 2022-04-05 |
CN108025462A (zh) | 2018-05-11 |
BR112018004669A2 (ja) | 2018-09-25 |
RU2671346C1 (ru) | 2018-10-30 |
MX364036B (es) | 2019-04-11 |
PH12018500472A1 (en) | 2018-09-10 |
JPWO2017042921A1 (ja) | 2018-04-05 |
KR102012140B1 (ko) | 2019-10-21 |
CN108025462B (zh) | 2019-06-21 |
MX2018002855A (es) | 2018-06-15 |
US10836123B2 (en) | 2020-11-17 |
EP3348371A1 (en) | 2018-07-18 |
US20180250893A1 (en) | 2018-09-06 |
KR20180035900A (ko) | 2018-04-06 |
EP3348371A4 (en) | 2018-10-24 |
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