CN106883445A - Preparation method based on modified graphene Wave suction composite material - Google Patents
Preparation method based on modified graphene Wave suction composite material Download PDFInfo
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- CN106883445A CN106883445A CN201710232878.1A CN201710232878A CN106883445A CN 106883445 A CN106883445 A CN 106883445A CN 201710232878 A CN201710232878 A CN 201710232878A CN 106883445 A CN106883445 A CN 106883445A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004744 fabric Substances 0.000 claims abstract description 64
- 239000000835 fiber Substances 0.000 claims abstract description 52
- 230000002787 reinforcement Effects 0.000 claims abstract description 44
- 229920005989 resin Polymers 0.000 claims abstract description 44
- 239000011347 resin Substances 0.000 claims abstract description 44
- 239000006260 foam Substances 0.000 claims abstract description 40
- 239000011159 matrix material Substances 0.000 claims abstract description 22
- 239000003292 glue Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000002347 injection Methods 0.000 claims abstract description 7
- 239000007924 injection Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 21
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims description 19
- 229920003192 poly(bis maleimide) Polymers 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 229910021389 graphene Inorganic materials 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229920001577 copolymer Polymers 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000007711 solidification Methods 0.000 claims description 12
- 230000008023 solidification Effects 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004697 Polyetherimide Substances 0.000 claims description 8
- 239000003431 cross linking reagent Substances 0.000 claims description 8
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- 239000003822 epoxy resin Substances 0.000 claims description 7
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
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- 238000010792 warming Methods 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical class CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 claims 1
- 239000009719 polyimide resin Substances 0.000 claims 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 3
- 239000010439 graphite Substances 0.000 abstract description 3
- 239000006096 absorbing agent Substances 0.000 abstract description 2
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- 229910000859 α-Fe Inorganic materials 0.000 abstract description 2
- 238000005452 bending Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- -1 modified graphene Alkene Chemical class 0.000 description 5
- 239000004800 polyvinyl chloride Substances 0.000 description 5
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- 238000010521 absorption reaction Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002513 implantation Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 2
- 238000005576 amination reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- 230000018109 developmental process Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 208000020442 loss of weight Diseases 0.000 description 1
- 230000007903 penetration ability Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
-
- 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
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
-
- 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
- B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
- B29C70/681—Component parts, details or accessories; Auxiliary operations
-
- 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
- B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
- B29C70/681—Component parts, details or accessories; Auxiliary operations
- B29C70/682—Preformed parts characterised by their structure, e.g. form
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/04—Ingredients treated with organic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C08J2333/18—Homopolymers or copolymers of nitriles
- C08J2333/20—Homopolymers or copolymers of acrylonitrile
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Reinforced Plastic Materials (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a kind of preparation method based on modified graphene Wave suction composite material, 1) the foam flat board of modified graphene is prepared, 2) modified graphene is dispersed in liquid resin matrix, 3) preform that cloth of reinforcement fibers wraps up foam is prepared, 4) preform is fitted into mould cavity, 5) the liquid resin matrix injection for containing modified graphene by the way of the vacuum pressed injecting glue enters the upper and lower surface of preform in mould, then solidified, the demoulding be obtained three-decker based on modified graphene Wave suction composite material.The present invention is using modified graphene as New Radar Absorbing agent, break through original limitation, ripple principle is inhaled in combination with 3-layer composite material structure, meet the good requirement of Wave suction composite material lightweight, wide-band and wave-absorbing, intensity, overcoming traditional absorbing material such as ferrite, manganese dioxide, graphite etc. has the shortcomings that density is big, it is narrow to inhale wave frequency band, has a good application prospect.
Description
Technical field
The invention belongs to Wave suction composite material technical field, modified graphene Wave suction composite material is based in particular to one kind
Preparation method.
Background technology
It is radar, millimeter wave, infrared, laser, multispectral with developing rapidly for modern military Detection Techniques and guidance technology
It is widely used in armament systems with the modern detection such as sound wave and guidance technology, prevents and survive to dashing forward for guided missile, aircraft, naval vessels etc.
Ability causes greatly threat.Wave-absorbing and camouflage material technology improves weapon as armament systems existence and penetration ability is improved
Equipment stealth capabilities, improve the effective means of overall fighting efficiency, are paid much attention to by each military power of the world.Preferably inhale
The characteristics of wave material requirement has " thin ", " light ", " width ", " strong ".Traditional single antiradar coatings, inhale ripple band limiting, efficiency
The limitation such as low, weight is big, temperature tolerance is poor, can not meet the requirement of modern weapons structure wave-absorbing and camouflage integration.Therefore, lightweight
The good Wave suction composite material of change, broadband, efficiency high, intensity has turned into the focus of whole world research.
Structure Wave suction composite material is while having the structure/function integration composite wood of bearing capacity and absorbing property
Material, external advanced invisbile plane has started to widely apply structure Wave suction composite material.It can be said that the development of structural wave-absorbing material
Largely affect the future of stealth material or even whole stealth technology.Wherein, light foam sandwich type is inhaled ripple and is combined
Material is because its intensity is high, good toughness, light weight the features such as, can make the obvious loss of weight of armament systems, enhancing mobility and increasingly
Many is applied to stealthy aircraft structural member.
The content of the invention
Deficiency present invention aim to be directed to traditional diamond-making technique, there is provided a kind of low-density, lighting and mechanics
The good preparation method based on modified graphene Wave suction composite material of performance.
To achieve the above object, the preparation method based on modified graphene Wave suction composite material designed by the present invention, institute
Preparation method is stated to comprise the following steps：
1) modified graphene, expanded material monomer, initiator, foaming agent and crosslinking agent are well mixed according to preset ratio
Form mixed solution；Then mixed solution is injected in die cavity react and obtains copolymer plate；It is cold after copolymer plate is foamed
But foamed board is formed to room temperature；Foamed board finally be thermally treated resulting in the foam flat board of modified graphene；
2) weigh resin matrix according to preset ratio and be warming up to resin matrix fusing point formation liquid resin matrix, so
Modified graphene is dispersed in liquid resin matrix afterwards；
3) cloth of reinforcement fibers is successively covered in step 1) in foam flat board upper and lower surface, until foam flat board upper surface
Preset thickness is reached with the thickness of the cloth of reinforcement fibers of lower surface, then rolls flat with flatiron, it is to avoid cloth of reinforcement fibers fold or line
Road distorts, and prepares the preform that cloth of reinforcement fibers wraps up foam；
4) by step 3) in preform be fitted into mould cavity, load mould cavity when, it is to avoid it is preforming
There is fold or is squeezed in body surface face, closed die, and checks air-tightness, after 4~6min of pressurize under 0.4~0.6MPa,
Then pressure vacuumizes 10~20min under being not less than 0.3MPa again；
5) by step 2 by the way of vacuum pressed injecting glue) the middle liquid resin matrix containing modified graphene for preparing
Injection enters step 4) in mould preform upper and lower surface, then solidified, the demoulding is obtained three-decker
Based on modified graphene Wave suction composite material.
Further, the step 1) and the step 2) in, the modifying process of modified graphene is：Graphene is added
Ultrasonic disperse is carried out in absolute ethyl alcohol, inorganic agent is subsequently adding, centrifugation and washed, dried modified stone is obtained after magnetic agitation
Black alkene；Wherein, Graphene and the mass volume ratio of absolute ethyl alcohol are 20~30g：The volume ratio of 15ml, inorganic agent and absolute ethyl alcohol
It is 1~2:5.Modified purpose is in order to realize graphenic surface amination graft modification, so as to improve Graphene and resin
The compatibility of matrix.
Further, the Graphene is graphene oxide；The inorganic agent is poly- 2- dimethylamino methyls acrylic acid second
Ester or polymethyl methacrylate.
Further, the step 1) in, modified graphene, expanded material monomer, initiator, foaming agent and crosslinking agent
Percentage by weight is 10~30%：65~83%：0.1~2%：2~5%：2~5%.
Further, the step 1) in, the foamed material monomer includes methacrylic acid, methacrylonitrile, azo
One kind in bis-isobutyronitrile, isopropanol, polyvinyl chloride, polyurethane, polystyrene, PEI, Polymethacrylimide
Or more than one.
Further, the step 2) in resin matrix be epoxy resin, bismaleimide resin, phenolic resin, polyimides tree
Fat or polyetherimide resin；The step 2) in the weight ratio of modified graphene and resin matrix be (1~4)：10.
Further, the step 5) in vacuum pressed injecting glue when：The pressure of vacuum injecting glue is progressively boosted by 0~0.1MPa
To 0.7~0.8MPa, after after the uniform plastic emitting of gum outlet, gum outlet, 5~15min of pressurize under 0.7~0.8MPa pressure are closed.
Further, the step 5) in curing cycle be：First 150~180 DEG C of 1~3h of solidification, then heat to 240~
300 DEG C of 2~4h of solidification.
Further, the step 3) in, the thickness of foam flat board upper surface cloth of reinforcement fibers is 1~8mm, foam flat board
The thickness of lower surface cloth of reinforcement fibers is 1~13mm.
Further, the step 5) in, the resin matrix of preform upper surface and the cloth of reinforcement fibers of upper surface
Percentage by weight is 65~75%：25~35%, the resin matrix of preform lower surface and the cloth of reinforcement fibers of lower surface
Percentage by weight is 55~65%：35~45%.
The present invention compared with prior art, with advantages below：
1st, the present invention breaks through original limitation using modified graphene as New Radar Absorbing agent, compound in combination with three layers
Material structure inhales ripple principle, meets the good requirement of Wave suction composite material lightweight, wide-band and wave-absorbing, intensity, overcomes traditional suction
Wave material such as ferrite, manganese dioxide, graphite etc. have the shortcomings that density is big, it is narrow to inhale wave frequency band, have a good application prospect；
2nd, it is modified by carrying out grafting to Graphene, is then dispersed in liquid resin, then carry out foamed solidification
And forming and hardening, realize modified graphene dispersed in sandwich foam and upper and lower skin layer composite material.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, is easy to more clearly understand the present invention,
But they do not constitute to the present invention and limit.
Using modified graphene, the modifying process of Graphene is following examples：It is 20~30g by mass volume ratio：
15ml (preferably 25g：15ml) by Graphene add absolute ethyl alcohol in, 20~40min of ultrasonic disperse (preferably 25~30min), so
After add inorganic agent, inorganic agent is 1~2 with the volume ratio of absolute ethyl alcohol:5 (preferably 1.5:5), it is centrifuged after 4~6h of magnetic agitation
Separate and wash, 50~80 DEG C (preferably 70~75 DEG C) are placed in after washing and dry 20~30h, modified graphene is obtained；Realize stone
Black alkene surface amination graft modification, so as to improve the compatibility of Graphene and resin matrix.And the graphite in modified graphene
Alkene is graphene oxide, and inorganic agent is poly- 2- dimethylaminoethyl methacrylates or polymethyl methacrylate.
Embodiment 1
1) according to percentage by weight 10%：83%：0.1%：4%：2.9% by modified graphene, expanded material monomer, draw
Hair agent, foaming agent and crosslinking agent mixing, are well mixed using ultrasonic wave dispersion and churned mechanically mode and form mixed solution；
Then reacted in the die cavity for mixed solution implantation glass plate being made, 30h is reacted in 70 DEG C of water-baths, obtained copolymer
Plate；Copolymer plate is cooled to room temperature after foaming 60min at 150 DEG C and forms foamed board；Finally by foamed board 0.1Mpa,
160 DEG C of heat treatment 2h, obtain the foam flat board of modified graphene；Wherein, foamed material monomer includes methacrylic acid, methyl-prop
Alkene nitrile, azodiisobutyronitrile, isopropanol, polyvinyl chloride, polyurethane, polystyrene, PEI, Polymethacrylimide
In one or more；
2) it is 1 according to weight ratio：10 weigh bismaleimide resin and are warming up to bismaleimide resin fusing point formation liquid span tree
, then be dispersed in modified graphene in liquid bismaleimide resin by fat；
3) setting agent is coated uniformly in cloth of reinforcement fibers, and cloth of reinforcement fibers is successively covered in step 1) in foam
The upper and lower surface of flat board, until the thickness of the cloth of reinforcement fibers of foam flat board upper surface reaches 5mm, until foam flat board lower surface
The thickness of cloth of reinforcement fibers reach 8mm, then roll flat with flatiron, it is to avoid carbon cloth fold or lines are distorted, and prepare increasing
Strong fiber cloth wraps up the preform of foam；Wherein, cloth of reinforcement fibers is carbon cloth, quartz fiber cloth or glass fabric；
4) by step 3) in preform be fitted into mould cavity, preform load mould cavity when need to keep away
Exempt from pre-form surface fold occur or be squeezed, closed die, and check air-tightness, after pressurize 5min under 0.5MPa,
Then pressure vacuumizes 10~20min under being not less than 0.3MPa again；
5) by step 2 by the way of vacuum pressed injecting glue) the middle injection of the bismaleimide resin containing modified graphene for preparing
Into step 4) in mould preform upper and lower surface, during vacuum pressed injecting glue the pressure of vacuum injecting glue by 0MPa by
Step boosts to 0.8MPa, after after the uniform plastic emitting of gum outlet, closes gum outlet, 5~15min of pressurize under 0.8MPa pressure, until
The bismaleimide resin of preform upper surface is 65% with the percentage by weight of the cloth of reinforcement fibers of upper surface：35%, preform
The bismaleimide resin of lower surface is 65% with the percentage by weight of the cloth of reinforcement fibers of lower surface：35%；Then solidified, the demoulding
Be obtained three-decker based on modified graphene Wave suction composite material, its curing cycle is：First 160 DEG C of solidification 2h, then heat up
To 280 DEG C of solidification 3h.
The density 0.124g/cm of the foam flat board of modified graphene3, tensile strength 3MPa, bending strength 4.2MPa；It is modified
The density of Graphene bismaleimide resin pour mass is 1.263g/cm3, bending strength be 172MPa, impact strength be 9.12KJ/m2；System
The standby effective frequency range for inhaling ripple based on modified graphene Wave suction composite material covers 4.61~14.8GHz, wherein maximum absorption band
Reachable-the 34.18d of value.
Embodiment 2
1) according to percentage by weight 15%：75%：1%：4%：5% by modified graphene, expanded material monomer, trigger
The mixing of agent, foaming agent and crosslinking agent, is well mixed using ultrasonic wave dispersion and churned mechanically mode and forms mixed solution；So
Reacted in mixed solution implantation glass plate is made die cavity afterwards, 28h is reacted in 75 DEG C of water-baths, obtained copolymer plate；
Copolymer plate is cooled to room temperature after foaming 70min at 140 DEG C and forms foamed board；Finally by foamed board 0.1Mpa, 180 DEG C
Heat treatment 2h, obtains the foam flat board of modified graphene；Wherein, foamed material monomer include methacrylic acid, methacrylonitrile,
In azodiisobutyronitrile, isopropanol, polyvinyl chloride, polyurethane, polystyrene, PEI, Polymethacrylimide
One or more；
2) it is 2 according to weight ratio：10 weigh phenolic resin and are warming up to phenolic resin fusing point formation liquid phenolic aldehyde tree
, then be dispersed in modified graphene in liquid phenolic resin by fat；
3) setting agent is coated uniformly in cloth of reinforcement fibers, and cloth of reinforcement fibers is successively covered in step 1) in foam
The upper and lower surface of flat board, until the thickness of the cloth of reinforcement fibers of foam flat board upper surface reaches 8mm, until foam flat board lower surface
The thickness of cloth of reinforcement fibers reach 12mm, then roll flat with flatiron, it is to avoid carbon cloth fold or lines are distorted, and prepare increasing
Strong fiber cloth wraps up the preform of foam；Wherein, cloth of reinforcement fibers is carbon cloth, quartz fiber cloth or glass fabric；
4) by step 3) in preform be fitted into mould cavity, preform load mould cavity when need to keep away
Exempt from pre-form surface fold occur or be squeezed, closed die, and check air-tightness, after pressurize 6min under 0.4MPa,
Then pressure vacuumizes 15min under being not less than 0.4MPa again；
5) by step 2 by the way of vacuum pressed injecting glue) the middle injection of the bismaleimide resin containing modified graphene for preparing
Into step 4) in mould preform upper and lower surface, during vacuum pressed injecting glue the pressure of vacuum injecting glue by 0MPa by
Step boosts to 0.8MPa, after after the uniform plastic emitting of gum outlet, closes gum outlet, 5~15min of pressurize under 0.8MPa pressure, until
The bismaleimide resin of preform upper surface is 70% with the percentage by weight of the cloth of reinforcement fibers of upper surface：30%, preform
The bismaleimide resin of lower surface is 70% with the percentage by weight of the cloth of reinforcement fibers of lower surface：30%；Then solidified, the demoulding
Be obtained three-decker based on modified graphene Wave suction composite material, its curing cycle is：First 180 DEG C of solidification 1h, then heat up
To 240 DEG C of solidification 4h.
The density 0.135g/cm of the foam flat board of modified graphene3, tensile strength 3.9MPa, bending strength 4.9MPa；Stone
The density of black alkene phenol-formaldehyde resin modified pour mass is 1.271g/cm3, bending strength be 183MPa, impact strength be 9.65KJ/m2；
The effective frequency range for inhaling ripple based on modified graphene Wave suction composite material for preparing covers 2.61~17.8GHz, wherein absorption maximum
Reachable-the 39.86dB of peak value.
Embodiment 3
1) according to percentage by weight 27%：65%：1%：4%：3% by modified graphene, expanded material monomer, trigger
The mixing of agent, foaming agent and crosslinking agent, is well mixed using ultrasonic wave dispersion and churned mechanically mode and forms mixed solution；So
Reacted in mixed solution implantation glass plate is made die cavity afterwards, 20h is reacted in 90 DEG C of water-baths, obtained copolymer plate；
Copolymer plate is cooled to room temperature after foaming 50min at 140 DEG C and forms foamed board；Finally by foamed board 0.1Mpa, 170 DEG C
Heat treatment 2h, obtains the foam flat board of modified graphene；Wherein, foamed material monomer include methacrylic acid, methacrylonitrile,
In azodiisobutyronitrile, isopropanol, polyvinyl chloride, polyurethane, polystyrene, PEI, Polymethacrylimide
One or more；
2) it is 3 according to weight ratio：10 weigh bismaleimide resin and are warming up to bismaleimide resin fusing point formation liquid span tree
, then be dispersed in modified graphene in liquid bismaleimide resin by fat；
3) setting agent is coated uniformly in cloth of reinforcement fibers, and cloth of reinforcement fibers is successively covered in step 1) in foam
The upper and lower surface of flat board, until the thickness of the cloth of reinforcement fibers of foam flat board upper surface reaches 8mm, until foam flat board lower surface
The thickness of cloth of reinforcement fibers reach 13mm, then roll flat with flatiron, it is to avoid carbon cloth fold or lines are distorted, and prepare increasing
Strong fiber cloth wraps up the preform of foam；Wherein, cloth of reinforcement fibers is carbon cloth, quartz fiber cloth or glass fabric；
4) by step 3) in preform be fitted into mould cavity, preform load mould cavity when need to keep away
Exempt from pre-form surface fold occur or be squeezed, closed die, and check air-tightness, after pressurize 4min under 0.6MPa,
Then pressure vacuumizes 10~20min under being not less than 0.3MPa again；
5) by step 2 by the way of vacuum pressed injecting glue) the middle injection of the bismaleimide resin containing modified graphene for preparing
Into step 4) in mould preform upper and lower surface, during vacuum pressed injecting glue the pressure of vacuum injecting glue by 0MPa by
Step boosts to 0.8MPa, after after the uniform plastic emitting of gum outlet, closes gum outlet, 5~15min of pressurize under 0.8MPa pressure, until
The bismaleimide resin of preform upper surface is 75% with the percentage by weight of the cloth of reinforcement fibers of upper surface：25%, preform
The bismaleimide resin of lower surface is 60% with the percentage by weight of the cloth of reinforcement fibers of lower surface：40%；Then solidified, the demoulding
Be obtained three-decker based on modified graphene Wave suction composite material, its curing cycle is：First 170 DEG C solidify 1.5h, Ran Housheng
Warm to 300 DEG C solidification 2h.
The density 0.128g/cm of the foam flat board of modified graphene3, tensile strength 3.7MPa, bending strength 4.0MPa；Stone
The density of black alkene modified quartz sand pour mass is 1.257g/cm3, bending strength be 176MPa, impact strength be 8.96KJ/m2；
The effective frequency range for inhaling ripple based on modified graphene Wave suction composite material for preparing covers 3.52~15.8GHz, wherein absorption maximum
Reachable-the 36.58dB of peak value.
Embodiment 4
1) according to percentage by weight 20%：70%：1.5%：4.5%：4% by modified graphene, expanded material monomer, draw
Hair agent, foaming agent and crosslinking agent mixing, are well mixed using ultrasonic wave dispersion and churned mechanically mode and form mixed solution；
Then reacted in the die cavity for mixed solution implantation glass plate being made, 18h is reacted in 100 DEG C of water-baths, obtained copolymer
Plate；Copolymer plate is cooled to room temperature after foaming 45min at 145 DEG C and forms foamed board；Finally by foamed board 0.1Mpa,
160 DEG C of heat treatment 2h, obtain the foam flat board of modified graphene；Wherein, foamed material monomer includes methacrylic acid, methyl-prop
Alkene nitrile, azodiisobutyronitrile, isopropanol, polyvinyl chloride, polyurethane, polystyrene, PEI, Polymethacrylimide
In one or more；
2) it is 4 according to weight ratio：10 weigh epoxy resin and are warming up to epoxy resin fusing point formation liquid epoxy tree
, then be dispersed in modified graphene in liquid-state epoxy resin by fat；
3) setting agent is coated uniformly in cloth of reinforcement fibers, and cloth of reinforcement fibers is successively covered in step 1) in foam
The upper and lower surface of flat board, until the thickness of the cloth of reinforcement fibers of foam flat board upper surface reaches 2mm, until foam flat board lower surface
The thickness of cloth of reinforcement fibers reach 5mm, then roll flat with flatiron, it is to avoid carbon cloth fold or lines are distorted, and prepare increasing
Strong fiber cloth wraps up the preform of foam；Wherein, cloth of reinforcement fibers is carbon cloth, quartz fiber cloth or glass fabric；
4) by step 3) in preform be fitted into mould cavity, preform load mould cavity when need to keep away
Exempt from pre-form surface fold occur or be squeezed, closed die, and check air-tightness, after pressurize 4min under 0.6MPa,
Then pressure vacuumizes 10~20min under being not less than 0.3MPa again；
5) by step 2 by the way of vacuum pressed injecting glue) the middle injection of the bismaleimide resin containing modified graphene for preparing
Into step 4) in mould preform upper and lower surface, during vacuum pressed injecting glue the pressure of vacuum injecting glue by 0MPa by
Step boosts to 0.8MPa, after after the uniform plastic emitting of gum outlet, closes gum outlet, 5~15min of pressurize under 0.8MPa pressure, until
The epoxy resin of preform upper surface is 75% with the percentage by weight of the cloth of reinforcement fibers of upper surface：25%, preform
The epoxy resin of lower surface is 57% with the percentage by weight of the cloth of reinforcement fibers of lower surface：43%；Then solidified, the demoulding
Be obtained three-decker based on modified graphene Wave suction composite material, its curing cycle is：First 150 DEG C of solidification 3h, then heat up
To 260 DEG C of solidification 3.5h.
The density 0.121g/cm of the foam flat board of modified graphene3, tensile strength 3.6MPa, bending strength 4.1MPa；Stone
The density of black alkene modified epoxy pour mass is 1.249g/cm3, bending strength is 190MPa, and impact strength is 7.92KJ/m2。
The effective frequency range for inhaling ripple based on modified graphene Wave suction composite material for preparing covers 2.82~14.96GHz, wherein absorption maximum
Reachable-the 32.57dB of peak value.
Claims (10)
1. a kind of preparation method based on modified graphene Wave suction composite material, it is characterised in that：The preparation method is included such as
Lower step：
1) modified graphene, expanded material monomer, initiator, foaming agent and crosslinking agent are well mixed according to preset ratio and are formed
Mixed solution；Then mixed solution is injected in die cavity react and obtains copolymer plate；It is cooled to after copolymer plate is foamed
Room temperature forms foamed board；Foamed board finally be thermally treated resulting in the foam flat board of modified graphene；
2) weigh resin matrix according to preset ratio and be warming up to resin matrix fusing point formation liquid resin matrix, then will
Modified graphene is dispersed in liquid resin matrix；
3) cloth of reinforcement fibers is successively covered in step 1) in foam flat board upper and lower surface, until foam flat board upper surface and under
The thickness of the cloth of reinforcement fibers on surface reaches preset thickness, prepares the preform that cloth of reinforcement fibers wraps up foam；
4) by step 3) in preform be fitted into mould cavity, after 4~6min of pressurize under 0.4~0.6MPa, then
Pressure vacuumizes 10~20min under being not less than 0.3MPa again；
5) by step 2 by the way of vacuum pressed injecting glue) the middle injection of the liquid resin matrix containing modified graphene for preparing
Into step 4) in mould preform upper and lower surface, then solidified, the demoulding be obtained three-decker based on
Modified graphene Wave suction composite material.
2. the preparation method of modified graphene Wave suction composite material is based on according to claim 1, it is characterised in that：The step
It is rapid 1) and the step 2) in, the modifying process of modified graphene is：Ultrasonic disperse is carried out during Graphene is added into absolute ethyl alcohol,
Inorganic agent is subsequently adding, centrifugation and is washed, dried prepared modified graphene after magnetic agitation；Wherein, Graphene with it is anhydrous
The mass volume ratio of ethanol is 20~30g：15ml, inorganic agent is 1~2 with the volume ratio of absolute ethyl alcohol:5.
3. the preparation method of modified graphene Wave suction composite material is based on according to claim 2, it is characterised in that：The stone
Black alkene is graphene oxide；The inorganic agent is poly- 2- dimethylaminoethyl methacrylates or polymethyl methacrylate.
4. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 1) in, the percentage by weight of modified graphene, expanded material monomer, initiator, foaming agent and crosslinking agent for 10~
30%：65~83%：0.1~2%：2~5%：2~5%.
5. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 1) in, the foamed material monomer includes methacrylic acid, methacrylonitrile, azodiisobutyronitrile, isopropanol, polychlorostyrene
One or more in ethene, polyurethane, polystyrene, PEI, Polymethacrylimide.
6. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 2) in resin matrix be epoxy resin, bismaleimide resin, phenolic resin, polyimide resin or polyetherimide resin；
The step 2) in the weight ratio of modified graphene and resin matrix be (1~4)：10.
7. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 5) in vacuum pressed injecting glue when：The pressure of vacuum injecting glue progressively boosts to 0.7~0.8MPa by 0~0.1MPa, treats out
After the uniform plastic emittings of Jiao Kou, gum outlet, 5~15min of pressurize under 0.7~0.8MPa pressure are closed.
8. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 5) in curing cycle be：First 150~180 DEG C of 1~3h of solidification, then heat to 240~300 DEG C of 2~4h of solidification.
9. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 3) in, the thickness of foam flat board upper surface cloth of reinforcement fibers is 1~8mm, foam flat board lower surface cloth of reinforcement fibers
Thickness is 1~13mm.
10. the preparation method based on modified graphene Wave suction composite material according to claim 1 or claim 2, it is characterised in that：Institute
State step 5) in, the percentage by weight of the resin matrix of preform upper surface and the cloth of reinforcement fibers of upper surface for 65~
75%：25~35%, the percentage by weight of the resin matrix of preform lower surface and the cloth of reinforcement fibers of lower surface for 55~
65%：35~45%.
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