CN107955332A - A kind of neutron shield superhybrid composite laminate and preparation method thereof - Google Patents

A kind of neutron shield superhybrid composite laminate and preparation method thereof Download PDF

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Publication number
CN107955332A
CN107955332A CN201711256776.XA CN201711256776A CN107955332A CN 107955332 A CN107955332 A CN 107955332A CN 201711256776 A CN201711256776 A CN 201711256776A CN 107955332 A CN107955332 A CN 107955332A
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hot pressing
epoxy resin
preparation
neutron
temperature
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CN107955332B (en
Inventor
杨中甲
顾轶卓
李敏
王绍凯
张佐光
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Chengde Wide Sail New Material Co Ltd
Beihang University
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Chengde Wide Sail New Material Co Ltd
Beihang University
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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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B32B15/092—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising epoxy resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/26—Layered products comprising a layer of synthetic resin characterised by the use of special additives using curing agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/26—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer which influences the bonding during the lamination process, e.g. release layers or pressure equalising layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/08—Interconnection of layers by mechanical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/10—Organic substances; Dispersions in organic carriers
    • G21F1/103—Dispersions in organic carriers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/24—Aluminium
    • 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
    • B32B2363/00—Epoxy resins
    • 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
    • C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • 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
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/06—Polyethene
    • 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
    • C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C08J2491/06—Waxes
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates
    • 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
    • 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
    • C08K3/34—Silicon-containing compounds
    • 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
    • C08K3/38—Boron-containing compounds
    • 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
    • C08K7/10—Silicon-containing compounds
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds

Abstract

The present invention provides a kind of neutron shield superhybrid composite laminate, the metallic plate comprising alternately laminated setting and fiber-reinforced resin matrix compound material layer；The fiber-reinforced resin matrix compound material layer includes basalt fibre, epoxy resin, modified boron carbide, curing agent, moderator and neutron-absorbing material component.Fiber-reinforced resin matrix compound material layer provided by the invention has excellent shielding properties and mechanical property at the same time, and density is 2.36~2.42g/cm3, tensile strength is 1120~1160MPa, and stretch modulus is 82~85GPa, and it is 78~85MPa that layer, which cuts intensity, right252CF neutron source screening factors Kf(15mm) is 2.65~3.02, neutron shield rate Ath10 (10mm) are up to 99.88~99.89%.Present invention also offers the preparation method of the composite-material laminates, this method is easy to operate, easy to implement.

Description

A kind of neutron shield superhybrid composite laminate and preparation method thereof
Technical field
The present invention relates to shielding material technical field, more particularly to a kind of neutron shield superhybrid composite laminate and its Preparation method.
Background technology
With developing rapidly for national defence scientific research, Radiation Medicine and atomic energy industry, more and more fields are being adopted gradually New energy resource supply mode is used as by the use of nuclear energy substitution traditional energy.While bringing many convenient to the mankind, it makes nuclear energy The radiation injury of association increasingly attracts people's attention during.Such as the neutron irradiation with strong penetrating power, can be to people Class life security, environment and instrument and equipment cause greatly to threaten.Therefore, it is to make nuclear energy more preferably to carry out shielding to this kind of radiation The necessary means of mankind's service.
Shielding material of the prior art, basis material are mainly cement and polyolefin.Wherein, the shielding material of cement base It is chiefly used in the radiation shield of large-scale protective device, still, shielding properties and the mechanical property of this kind of material are difficult to take into account.
The content of the invention
It is an object of the invention to provide neutron shield that is a kind of while having excellent shielding properties and mechanical property to surpass Mixed composite material laminate and preparation method thereof.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The present invention provides a kind of preparation method of neutron shield superhybrid composite laminate, comprise the following steps：
(1) epoxy resin, curing agent and acetone are mixed, obtains resin matrix solution；
Boron carbide, coupling agent and acetone are mixed into post activation, obtain modified boron carbide；
(2) after mixing the resin matrix solution, modified boron carbide, moderator and neutron-absorbing material, acetone tune is added Section density is 0.94~1.10g/cm3, obtain basic mixture；
(3) wet type prepreg is prepared as raw material using the basic mixture and basalt fibre, it is pre- to obtain solid after dry Leaching material；
(4) it is the solid prepreg and metallic plate progress is alternately laminated, obtain basic molding structure；
The metallic plate is aluminium sheet or aluminium alloy plate；
(5) hot pressing is carried out to the basic molding structure, obtains neutron shield superhybrid composite laminate.
Preferably, the epoxy resin contains phenyl ring for glycidyl ether type epoxy resin of the main chain containing benzene ring structure, main chain One kind or several in the glycidyl amine epoxy resin of glycidyl ester epoxy resin and main chain containing benzene ring structure of structure Kind；
The curing agent is polyhydric aliphatic amine, polynary aromatic amine, anhydrides, ionic class and dicyandiamide class curing agent In one or more；
The mass ratio of the epoxy resin and curing agent is 100:(30~90).
Preferably, the coupling agent is silane coupling agent and/or titanate coupling agent；
The mass ratio of the boron carbide and coupling agent is (4~6):1.
Preferably, the temperature of the activation is 5~15 DEG C, and the time is 5~15min.
Preferably, the mass ratio of the epoxy resin and moderator is 100:(10~20)；
The mass ratio of the epoxy resin and neutron-absorbing material is 100:(10~20).
Preferably, the basic mixture epoxy resin and the gross mass of curing agent are the 25 of wet type prepreg gross mass ~35%.
Preferably, the temperature of the hot pressing is 115~125 DEG C；
The pressure of the hot pressing is 0.4~0.8MPa；
The time of the hot pressing is 1~5h.
Preferably, the hot pressing include sequentially carry out and temperature sequentially elevated level-one hot pressing, two level hot pressing and three-level heat Pressure；
The temperature of the level-one hot pressing is 125~135 DEG C；
The temperature of the two level hot pressing is 145~155 DEG C；
The temperature of the three-level hot pressing is 175~185 DEG C.
Preferably, the time of the level-one hot pressing is 0.5~3h；
The time of the two level hot pressing is 1~3h, and pressure is 0.4~0.8MPa；
The time of the three-level hot pressing is 1~3h, and pressure is 0.4~0.8MPa.
The neutron shield obtained present invention also offers the preparation method described in a kind of above-mentioned technical proposal surpasses hybrid composite manner Material laminate, the metallic plate comprising alternately laminated setting and fiber-reinforced resin matrix compound material layer；
The fiber-reinforced resin matrix compound material layer includes basalt fibre, epoxy resin, modified boron carbide, curing Agent, moderator and neutron-absorbing material component.
The present invention provides a kind of neutron shield superhybrid composite laminate, the metallic plate comprising alternately laminated setting and Fiber-reinforced resin matrix compound material layer；The fiber-reinforced resin matrix compound material layer include basalt fibre, epoxy resin, Modified boron carbide, curing agent, moderator and neutron-absorbing material component.The present invention, can be significantly using metallic plate as mechanical support layer Improve the mechanical strength of material；Basalt fibre contains the heavy nucleus element such as iron, manganese in fiber-reinforced resin matrix compound material layer, carries Absorption and scattering process of the material to high-energy ionization radiation have been supplied, there is good alpha ray shield performance；Boron carbide can absorb Substantial amounts of neutron is without generating any transmitting line element；And due to the presence of epoxy resin, metallic plate and fiber reinforcement tree Bond strength is strong between resin-based composite layer.Therefore, the composite-material laminates that invention provides have excellent at the same time Shielding properties and mechanical property.From the result of embodiment, the density of neutron shield superhybrid composite laminate is 2.36~2.42g/cm3, tensile strength is 1120~1160MPa, and stretch modulus is 82~85GPa, layer cut intensity for 78~ 85MPa is right252CF neutron source screening factors Kf(15mm) is 2.65~3.02, neutron shield rate Ath10 (10mm) up to 99.88~ 99.89%.
Present invention also offers the preparation method of the neutron shield superhybrid composite laminate, this method operation letter Just, it is easy to implement.
Embodiment
The present invention provides a kind of preparation method of neutron shield superhybrid composite laminate, comprise the following steps：
(1) epoxy resin, curing agent and acetone are mixed, obtains resin matrix solution；
Boron carbide, coupling agent and acetone are mixed into post activation, obtain modified boron carbide；
(2) after mixing the resin matrix solution, modified boron carbide, moderator and neutron-absorbing material, acetone tune is added Section density is 0.94~1.10g/cm3, obtain basic mixture；
(3) wet type prepreg is prepared as raw material using the basic mixture and basalt fibre, it is pre- to obtain solid after dry Leaching material；
(4) it is the solid prepreg and metallic plate progress is alternately laminated, obtain basic molding structure；
The metallic plate is aluminium sheet or aluminium alloy plate；
(5) hot pressing is carried out to the basic molding structure, obtains neutron shield superhybrid composite laminate.
The present invention mixes epoxy resin, curing agent and acetone, obtains resin matrix solution.In the present invention, the ring Oxygen tree fat is preferably glycidyl ether type epoxy resin of the main chain containing benzene ring structure, glycidol esters of the main chain containing benzene ring structure One or more in the glycidyl amine epoxy resin of epoxy resin and main chain containing benzene ring structure.In the present invention, it is described Glycidyl ether type epoxy resin of the main chain containing benzene ring structure is preferably in bisphenol-A 2-glycidyl ester product E 51, E44 and E20 One kind, two or three；Glycidyl ester epoxy resin of the main chain containing benzene ring structure is preferably that phthalic acid shrinks Glyceride, tetrahydrophthalic acid ethylene oxidic ester and one kind in hexahydrophthalic acid ethylene oxidic ester, two or three； Glycidyl amine epoxy resin of the main chain containing benzene ring structure is preferably 4,4 '-diaminodiphenylmethane epoxy resin (AG80) and/or para-aminophenol epoxy resin (AFG90).
In the present invention, the curing agent is preferably polyhydric aliphatic amine, polynary aromatic amine, anhydrides, ionic class With the one or more in dicyandiamide class curing agent, more preferably 4,4 '-diamino diphenyl sulfone (DDS), 4,4 '-diaminourea two Phenylmethane (DDM), methylnadic anhydride, methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride, ethylenediamine and one kind in dicyandiamide or It is several.
Curing agent is preferably first dissolved in acetone by the present invention, is then mixed again with epoxy resin.The present invention is to the acetone Dosage there is no particular/special requirement, curing agent can be dissolved.
In the present invention, the mass ratio of the epoxy resin and curing agent is preferably 100:(30~90), more preferably 100:(40~80), are most preferably 100:(50~70).
The present invention is not particularly limited the source of the epoxy resin, curing agent and acetone, using people in the art The above-mentioned substance in source known to member, can be specifically the commercial product of above-mentioned substance.
Boron carbide, coupling agent and acetone are mixed post activation by the present invention, obtain modified boron carbide.In the present invention, it is described Coupling agent is preferably silane coupling agent and/or titanate coupling agent；The silane coupling agent is preferably gamma-aminopropyl-triethoxy Silane (KH550), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), γ-(methacryloxypropyl) methoxyl group silicon Alkane (KH570), N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane (KH792, DL602) and vinyltrimethoxysilane (DL171) one or more in；The titanate coupling agent is preferably monoalkoxy unrighted acid titanate esters (KR- TTS), pyrophosphoric acid type monoalkoxy class titanate esters (KR-38S), tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters (KR-41B) and multi-active base group chelating type phosphate titanium coupling agent (KR-238S) in one or more.
The coupling agent is preferably dissolved in acetone by the present invention, is then mixed again with boron carbide.In the present invention, the idol The mass ratio for joining agent and acetone is preferably 1:(2~5), more preferably 1:3；The mass ratio of the boron carbide and coupling agent is preferably (4~6):1, more preferably 5:1.
In the present invention, the activation process is specially that coupling agent carries out surface modification to carbonization boron surface, increases surface Activation energy；The temperature of the activation is preferably 5~15 DEG C, more preferably 8~13 DEG C, is most preferably 10 DEG C；The activation when Between be preferably 5~15min, more preferably 8~13min, be most preferably 10min.In the present invention, the activation process can make Boron surface must be nitrogenized chemical coupling reaction occurs, and then more preferable compatibility is produced with organic matter.
The present invention is not particularly limited the source of the boron carbide, coupling agent and acetone, using those skilled in the art The above-mentioned substance in known source, can be specifically the commercial product of above-mentioned substance.
After obtaining resin matrix solution and modified boron carbide, the present invention is by the resin matrix solution, modified boron carbide, slow After agent and neutron-absorbing material mixing, it is 0.94~1.10g/cm to add acetone and adjust density3, obtain basic mixture.At this In invention, the moderator is preferably the one or more in polyethylene, polypropylene, paraffin and graphite, the grain of the moderator Footpath is preferably 3~800 μm, more preferably 100~700 μm, is most preferably 300~500 μm.In the present invention, the neutron is inhaled It is preferably the one or more in boron, boron oxide, borax, iron and micaceous iron oxide to receive agent；The particle diameter of the neutron-absorbing material is excellent Elect 3~500 μm as, more preferably 100~400 μm, be most preferably 200~300 μm.The present invention inhales the moderator and neutron The source for receiving agent is not particularly limited, specifically can be with using the above-mentioned substance in source well known to those skilled in the art For the commercial product of above-mentioned substance.In the present invention, the mass ratio of the epoxy resin and moderator is preferably 100:(10~ 20) 100, are more preferably:(12~18), are most preferably 100:(14~16)；The quality of the epoxy resin and neutron-absorbing material Than being preferably 100:(10~20), more preferably 100:(12~18), are most preferably 100:(14~16).
In the present invention, the density of the basic mixture is 0.94~1.10g/cm3, it is preferably 0.96~1.05g/ cm3, more preferably 1~1.03g/cm3.It is 0.94~1.10g/cm that the present invention, which adjusts density,3It can be good at controlling basic mixing The glue content of thing so that basic mixture infiltrates basalt fibre more uniform in subsequent process.
After obtaining basic mixture, the present invention prepares wet type preimpregnation using the basic mixture and basalt fibre as raw material Material, solid prepreg is obtained after dry.The present invention does not have any particular/special requirement to the preparation method of the wet type prepreg, adopts Prepared with the pre- dipping machine of wet method according to the common method of those skilled in the art institute.In the present invention, the basis is mixed Compound epoxy resin and the gross mass of curing agent are preferably the 25~35% of wet type prepreg gross mass, more preferably 28~ 33%, it is most preferably 30%；Surface density is preferably 330~350g/m2, more preferably 335~345g/m2, it is most preferably 340g/ m2。
The present invention does not have any particular/special requirement to the size of the basalt fibre, ripe using those skilled in the art institute The basalt fibre for the commercially available size known.
In the present invention, the temperature of the drying is preferably 20~30 DEG C, more preferably 22~28 DEG C, most preferably 24~ 26℃；The time of the drying is preferably 10~15h, more preferably 12~13h；The ambient humidity of the drying is preferably shorter than 50%, more preferably lower than 45%, most preferably less than 40%.The present invention does not appoint the degree of drying of the solid prepreg What particular/special requirement, can volatilize the acetone in prepreg clean.In the present invention, the Black Warrior in the solid prepreg Rock fiber can be unidirectional array, or random disordered arrangements.
After obtaining solid prepreg, the present invention is alternately laminated by the solid prepreg and metallic plate progress, obtains basis Molding structure.In the present invention, the metallic plate is preferably aluminium sheet or aluminium alloy plate.Kind of the present invention to the aluminium alloy plate Class does not have any particular/special requirement, can use the aluminium alloy plate of any kind on the market.In the present invention, the gold The thickness for belonging to plate is preferably 0.05~0.3mm, more preferably 0.1~0.2mm.
In the present invention, when basalt fibre is unidirectional regularly arranged in the solid prepreg, any unidirectional solid The row of basalt fibre is to can be towards any direction, without any particular/special requirement in prepreg.
The present invention does not have any particular/special requirement to the number of plies of the basic molding structure, can be wanted according to actual technology Ask and be configured；In the specific embodiment of the invention, the number of plies of the basis molding structure is preferably 3~10 layers, and more preferably 5 ~8 layers.In the present invention, the both ends of the basic molding structure are preferably all solid prepreg.
After obtaining basic molding structure, the present invention carries out hot pressing to the basic molding structure, and it is super mixed to obtain neutron shield Miscellaneous composite-material laminates.In the present invention, the hot pressing can be a step hot pressing or three step hot pressing.
In the present invention, the temperature of hot pressing is preferably 115~125 DEG C in the step hot pressing, and more preferably 118~120 ℃；The pressure of the hot pressing is preferably 0.4~0.8MPa, more preferably 0.5~0.6MPa；The time of the hot pressing is preferably 1 ~5h, more preferably 2~3h.In the specific embodiment of the invention, be warming up to the heating rate of a step hot pressing temperature for 2 DEG C/ Min, after the step hot pressing, direct furnace cooling.
In the present invention, the three steps hot pressing, which preferably comprises, sequentially carries out and temperature sequentially elevated level-one hot pressing, two level Hot pressing and three-level hot pressing；The temperature of the level-one hot pressing is preferably 125~135 DEG C, more preferably 128~130 DEG C；The level-one The time of hot pressing is preferably 0.5~3h, more preferably 1~2h；The temperature of the two level hot pressing is preferably 145~155 DEG C, more excellent Elect 150~152 DEG C as；The time of the two level hot pressing is preferably 1~3h, more preferably 2~2.5h；The pressure of the two level hot pressing Power is preferably 0.4~0.8MPa, more preferably 0.5~0.6MPa；The temperature of the three-level hot pressing is preferably 175~185 DEG C, more Preferably 179~180 DEG C；The time of the three-level hot pressing is preferably 1~3h, more preferably 2~2.5h；The three-level hot pressing Pressure is preferably 0.4~0.8MPa, more preferably 0.5~0.6MPa.In the specific embodiment of the invention, level-one hot pressing is warming up to The heating rate of temperature, the heating rate for being warming up to by level-one hot pressing temperature two level hot pressing temperature, heated up by two level hot pressing temperature Heating rate to three-level hot pressing temperature is 2 DEG C/min, after the three-level hot pressing, direct furnace cooling.
In the present invention, the hot pressing preferably carries out under vacuumized conditions, the vacuum pressure vacuumized be preferably- 0.15~-0.05MPa, more preferably -0.1MPa.
In hot pressing of the present invention, epoxy resin melt latter aspect bonded with metallic plate, on the one hand with it is profound Military rock fiber, modified boron carbide, curing agent, moderator and neutron-absorbing material component mix more uniform.
Present invention also offers the neutron shield superhybrid composite that the preparation method described in above-mentioned technical proposal obtains Laminate, the metallic plate comprising alternately laminated setting and fiber-reinforced resin matrix compound material layer；The fiber-reinforced resin base is answered Condensation material layer includes basalt fibre, epoxy resin, modified boron carbide, curing agent, moderator and neutron-absorbing material component.At this In invention, two outer layers of the neutron shield superhybrid composite laminate are preferably fiber-reinforced resin base composite wood The bed of material.The present invention can substantially improve the mechanical strength of material using metallic plate as mechanical support layer；Fiber-reinforced resin base is compound Basalt fibre contains the heavy nucleus element such as iron, manganese in material layer, there is provided absorption and scattering of the material to high-energy ionization radiation are made With having good alpha ray shield performance；Boron carbide can absorb substantial amounts of neutron without generating any transmitting line element； And due to the presence of epoxy resin, bond strength is strong between metallic plate and fiber-reinforced resin matrix compound material layer.
With reference to embodiment to neutron shield superhybrid composite laminate provided by the invention and preparation method thereof into Row detailed description, but they cannot be interpreted as limiting the scope of the present invention.
In all embodiments of the invention, unless otherwise specified, all numbers are mass parts.
Embodiment 1
By 34 parts of DDS curing agent acetone solutions, then mix until solution is uniformly clarified, obtain with 100 parts of E51 resins To resin matrix solution.
25 parts of boron carbide powders, 15 parts of acetone and 5 parts of KH560 coupling agents are weighed, the KH560 coupling agents are dissolved in In acetone, it is then added in the boron carbide powder, is stirred evenly under conditions of being 10 DEG C in temperature, and constant temperature activates 10 points Clock, is made surface modified carbon boron powder.
Surface modified carbon boron powder, the polyethylene of 10 parts by weight and 10 parts by weight boron oxides and resin matrix solution are mixed Close, adjusted solution density to 0.96/cm with acetone3。
Unidirectional wet type prepreg is prepared using wet method preimpregnation machine, the gross mass of wet type prepreg epoxy resin and curing agent contains Amount is 28wt%, and surface density is 340g/m2。
Prepared wet type prepreg is hung to volatilize and remove included acetone solvent at room temperature, and controls phase To humidity below 50%, open assembly time 12h is spare.
Heat is carried out after the aluminium alloy core plate of three layers of 0.1mm and four layers of solid-state prepreg are distinguished alternately laminated settings Pressure, wherein the direction of the basalt fibre of unidirectional array is consistent in four layers of solid-state prepreg.
Hot pressing temperature system is：130 DEG C are warming up to from room temperature (25 DEG C), heating rate is 2 DEG C/min, and 130 DEG C keep the temperature 1h, Then 150 DEG C are warming up to, heating rate is 2 DEG C/min, and 2h is kept the temperature under the conditions of 150 DEG C, is subsequently warming up to 180 DEG C, heating speed Rate is 2 DEG C/min, keeps the temperature 2h under the conditions of 180 DEG C, cools to 60 DEG C, with furnace cooling.
Hot pressing pressure system is：When solidification temperature is raised to 130 DEG C, do not apply external pressure；When solidification temperature is raised to 150 DEG C, apply Add 0.6MPa external pressures.
The performance for the neutron shield superhybrid composite laminate that the present invention obtains the present embodiment is tested, and experiment is surveyed , density 2.36g/cm3, tensile strength 1120MPa, stretch modulus 82GPa, it is 80MPa that layer, which cuts intensity, right252CF neutrons Source screening factor Kf(15mm) is 2.65, neutron shield rate Ath10 (10mm) are up to 99.88%.
Embodiment 2
By 34 parts of DDS curing agent acetone solutions, then mix until solution is uniformly clarified, obtain with 100 parts of E51 resins To resin matrix solution.
50 parts of boron carbide powders, 30 parts of acetone and 10 parts of KH560 coupling agents are weighed, the KH560 coupling agents are dissolved In acetone, it is then added in the boron carbide powder, is stirred evenly under conditions of being 10 DEG C in temperature, and constant temperature activation 10 Minute, surface modified carbon boron powder is made.
Surface modified carbon boron powder, the paraffin of 20 parts by weight and 20 parts by weight mica iron oxide and resin matrix solution are mixed Close, adjusted solution density to 1.06/cm with acetone3。
Random wet type prepreg is prepared using wet method preimpregnation machine, the gross mass of wet type prepreg epoxy resin and curing agent contains Amount is 32wt%, and surface density is 390g/m2。
Prepared wet type prepreg is hung to volatilize and remove included acetone solvent at room temperature, and controls phase To humidity below 50%, open assembly time 12h is spare.
Hot pressing is carried out after the core plate of two layers 0.1mm and three layers of solid-state prepreg are distinguished alternately laminated setting.
Hot pressing temperature system is：130 DEG C are warming up to from room temperature (25 DEG C), heating rate is 2 DEG C/min, and 130 DEG C keep the temperature 1h, Then 150 DEG C are warming up to, heating rate is 2 DEG C/min, and 2h is kept the temperature under the conditions of 150 DEG C, is subsequently warming up to 180 DEG C, heating speed Rate is 2 DEG C/min, keeps the temperature 2h under the conditions of 180 DEG C, cools to 60 DEG C, with furnace cooling.
Hot pressing pressure system is：When solidification temperature is raised to 130 DEG C, do not apply external pressure；When solidification temperature is raised to 150 DEG C, apply Add 0.6MPa external pressures.
The performance for the neutron shield superhybrid composite laminate that the present invention obtains the present embodiment is tested, and experiment is surveyed , density 2.42g/cm3, tensile strength 1160MPa, stretch modulus 84GPa, it is 78MPa that layer, which cuts intensity, right252CF neutrons Source screening factor Kf(15mm) is 2.97, neutron shield rate Ath10 (10mm) are up to 99.98%.
Embodiment 3
Then 84 parts of BC12 curing agent acetone solutions are mixed until solution is uniformly clarified with 100 parts of E44 resins, Obtain resin matrix solution.
30 parts of boron carbide powders, 15 parts of acetone and 5 parts of KH560 coupling agents are weighed, the KH560 coupling agents are dissolved in In acetone, it is then added in the boron carbide powder, is stirred evenly under conditions of being 10 DEG C in temperature, and constant temperature activates 10 points Clock, is made surface modified carbon boron powder.
Surface modified carbon boron powder, the graphite of 15 parts by weight and 15 parts by weight boraxs are mixed with resin matrix solution, are used Acetone adjusts solution density to 0.96/cm3。
Unidirectional wet type prepreg is prepared using wet method preimpregnation machine, the gross mass of wet type prepreg epoxy resin and curing agent contains Amount is 30wt%, and surface density is 345g/m2。
Prepared wet type prepreg is hung to volatilize and remove included acetone solvent at room temperature, and controls phase To humidity below 50%, open assembly time 12h is spare.
Hot pressing is carried out after the core plate of two layers 0.1mm and two layers of solid-state prepreg are distinguished alternately laminated setting, wherein The direction of the basalt fibre of unidirectional array is orthogonal in two layers of solid-state prepreg.
Hot pressing temperature system is：120 DEG C are warming up to from room temperature (25 DEG C), heating rate is 2 DEG C/min, and 120 DEG C keep the temperature 3h, Cool to 60 DEG C, with furnace cooling.
Hot pressing pressure system is：When solidification temperature is raised to 120 DEG C, apply 0.6MPa external pressures.
The performance for the neutron shield superhybrid composite laminate that the present invention obtains the present embodiment is tested, and experiment is surveyed , density 2.40g/cm3, tensile strength 1132MPa, stretch modulus 85GPa, it is 85MPa that layer, which cuts intensity, right252In CF Component screening factor Kf(15mm) is 3.02, neutron shield rate Ath10 (10mm) are up to 99.89%.
As seen from the above embodiment, fiber-reinforced resin matrix compound material layer provided by the invention has excellent screen at the same time Performance and mechanical property are covered, density is 2.36~2.42g/cm3, tensile strength is 1120~1160MPa, stretch modulus for 82~ 85GPa, it is 78~85MPa that layer, which cuts intensity, right252CF neutron source screening factors Kf(15mm) is 2.65~3.02, neutron shield rate Ath10 (10mm) are up to 99.88~99.89%.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of neutron shield superhybrid composite laminate, comprises the following steps：
(1) epoxy resin, curing agent and acetone are mixed, obtains resin matrix solution；
Boron carbide, coupling agent and acetone are mixed into post activation, obtain modified boron carbide；
(2) after mixing the resin matrix solution, modified boron carbide, moderator and neutron-absorbing material, it is close to add acetone adjusting Spend for 0.94~1.10g/cm3, obtain basic mixture；
(3) wet type prepreg is prepared as raw material using the basic mixture and basalt fibre, solid prepreg is obtained after dry；
(4) it is the solid prepreg and metallic plate progress is alternately laminated, obtain basic molding structure；
The metallic plate is aluminium sheet or aluminium alloy plate；
(5) hot pressing is carried out to the basic molding structure, obtains neutron shield superhybrid composite laminate.
2. preparation method according to claim 1, it is characterised in that the epoxy resin is contracting of the main chain containing benzene ring structure The shrink of glycidyl ester epoxy resin and main chain containing benzene ring structure of water glycerine ether type epoxy resins, main chain containing benzene ring structure One or more in glycerine amine epoxy resin；
The curing agent is in polyhydric aliphatic amine, polynary aromatic amine, anhydrides, ionic class and dicyandiamide class curing agent It is one or more of；
The mass ratio of the epoxy resin and curing agent is 100:(30~90).
3. preparation method according to claim 1, it is characterised in that the coupling agent is silane coupling agent and/or metatitanic acid Ester coupling agent；
The mass ratio of the boron carbide and coupling agent is (4~6):1.
4. the preparation method according to claim 1 or 3, it is characterised in that the temperature of the activation is 5~15 DEG C, the time For 5~15min.
5. preparation method according to claim 1 or 2, it is characterised in that the mass ratio of the epoxy resin and moderator For 100:(10~20)；
The mass ratio of the epoxy resin and neutron-absorbing material is 100:(10~20).
6. preparation method according to claim 1, it is characterised in that the basic mixture epoxy resin and curing agent Gross mass be wet type prepreg gross mass 25~35%.
7. preparation method according to claim 1, it is characterised in that the temperature of the hot pressing is 115~125 DEG C；
The pressure of the hot pressing is 0.4~0.8MPa；
The time of the hot pressing is 1~5h.
8. preparation method according to claim 1, it is characterised in that the hot pressing includes sequentially progress and temperature sequentially rises High level-one hot pressing, two level hot pressing and three-level hot pressing；
The temperature of the level-one hot pressing is 125~135 DEG C；
The temperature of the two level hot pressing is 145~155 DEG C；
The temperature of the three-level hot pressing is 175~185 DEG C.
9. preparation method according to claim 8, it is characterised in that the time of the level-one hot pressing is 0.5~3h；
The time of the two level hot pressing is 1~3h, and pressure is 0.4~0.8MPa；
The time of the three-level hot pressing is 1~3h, and pressure is 0.4~0.8MPa.
10. the neutron shield superhybrid composite laminate that the preparation method described in claim 1~9 any one obtains, bag Metallic plate and fiber-reinforced resin matrix compound material layer containing alternately laminated setting；
The fiber-reinforced resin matrix compound material layer includes basalt fibre, epoxy resin, modified boron carbide, curing agent, slow Agent and neutron-absorbing material component.
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CN109354826A (en) * 2018-09-25 2019-02-19 北航（四川）西部国际创新港科技有限公司 Nuclear screening material and its manufacturing method
CN109575606A (en) * 2019-01-16 2019-04-05 东莞理工学院 A kind of neutron shielding material and preparation method thereof
CN110619969A (en) * 2019-09-23 2019-12-27 中国核动力研究设计院 Radiation shielding container and preparation method thereof
CN111009332A (en) * 2019-12-20 2020-04-14 北航（四川）西部国际创新港科技有限公司 Nuclear radiation shielding structure and manufacturing method thereof
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CN111892695B (en) * 2020-07-13 2022-12-30 四川省玻纤集团有限公司 Gamma irradiation resistant modified resin and preparation method thereof, laminated board and preparation process and application thereof
CN112356534A (en) * 2020-11-09 2021-02-12 哈尔滨工业大学 Radiation protection composite material and preparation method thereof
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CN112331375A (en) * 2020-11-23 2021-02-05 四川玄武岩纤维新材料研究院(创新中心) Basalt and other fiber honeycomb fabric nuclear shielding composite material and preparation method and application thereof
CN113513945A (en) * 2021-03-31 2021-10-19 北京理工艾尔安全科技有限公司 Composite armor plate forming method
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