CN105383130B - A kind of method of nano wave-absorption film functional modification composite material laminated board - Google Patents

A kind of method of nano wave-absorption film functional modification composite material laminated board Download PDF

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CN105383130B
CN105383130B CN201510768811.0A CN201510768811A CN105383130B CN 105383130 B CN105383130 B CN 105383130B CN 201510768811 A CN201510768811 A CN 201510768811A CN 105383130 B CN105383130 B CN 105383130B
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composite material
nano
resin
absorption film
wave
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CN105383130A (en
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于祺
陈平
唐超
王荣超
陆春
马克明
熊需海
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Shenyang Aerospace University
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Shenyang Aerospace University
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin 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
    • 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
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    • B32B27/00—Layered products comprising a layer of synthetic resin
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    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/285—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
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    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
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Abstract

A kind of method of nano wave-absorption film functional modification composite material laminated board, is carried out according to the following steps：A kind of method of nano wave-absorption film functional modification composite material laminated board, comprises the following steps：(1) nano-particle and polyarylether resin are configured to the resin solution of stable homogeneous；(2) resin solution prepared is prepared into by nano wave-absorption film using thin film preparation process；(3) continuous fiber or fabric are sufficiently impregnated preparing material prepreg with resin matrix；(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning preparation structure/function integration camouflage composite material laminate.The beneficial effect that is reached of the present invention is：Wave energy layer will be inhaled to be integrated in the preparation process of composite material laminated board, significantly and at low cost the overall suction wave energy of Synchronous lifting composite and mechanical property.Product has excellent carrying and stealthy dual-use function concurrently, is had broad application prospects in Aerospace Engineering field.

Description

A kind of method of nano wave-absorption film functional modification composite material laminated board
Technical field
The present invention relates to a kind of preparation method of camouflage composite material, and in particular to a kind of nano wave-absorption film functionalization changes The preparation method of property composite material laminated board, belongs to stealth material science and technology field.
Background technology
The fast development of stealth technology proposes thin, wide, light, strong composite request to radar absorbing, and development has The efficient absorbing property and camouflage composite material of excellent in mechanical performance is to meet one of technological break-through point of this requirement.Structural type Wave suction composite material is the composite for having carrying concurrently and inhaling ripple dual-use function to grow up on advanced composite material base plinth, Its advantage is can largely to mitigate the quality of aircraft, and structure has designability, and plastic variously-shaped complicated part, has The absorption band that effect overcomes coating-type absorbing materials generally existing is narrow, increase aircraft deadweight, appearance low with housing adhesion strength Easily peel off or cracking is, it is necessary to the shortcomings of frequently repairing, thus in actual applications especially in aerospace field by more next More concerns, turn into one of the main direction of development of wave-absorbing and camouflage material.
Structure-type wave-absorption composite material is typically that nano wave-absorption agent is dispersed in into fiber-reinforced resin matrix compound material Realize its stealthy function.At present, mainly utilize blending method by nano-particles filled in the continuous tree of composite both at home and abroad Functional modification is carried out in aliphatic radical body phase, to a variety of meso-scales formed during modified resin matrix and fiber composite Fault in material, and negative influence caused by the mechanical property to fibrous composite, potential bearing capacity and preparation technology etc. Few concern.
The preparation process of nano wave-absorption composite is often main source caused by a variety of meso-scale faults in material.It is first First, the filling of wave absorbing agent can cause resin matrix viscosity to improve, mobility is deteriorated, and cause microcosmic infiltration of the resin matrix to fiber Mismatched with macroscopical flowing velocity, so as to trigger in fibre bundle and fiber interlayer forms intensive hole and lamination defect；Secondly, receive Dispersiveness and less stable of the rice wave absorbing agent in resin matrix, with easily reuniting during fiber composite, therefore The absorbing property of composite is set to be had a great influence by preparation technology, the unstability and uncontrollability that performance be present.
The content of the invention
The present invention separates nano wave-absorption agent with the continuous phase resin matrix component of composite, passes through the side introduced indirectly Formula is inserted into the interlayer of material prepreg using polyarylether resin film as carrier, and is integrated in the preparation of composite material laminated board During.This method not only makes the basic performance of the original resin system of composite be maintained, and in basic technology system On the premise of larger change need not be made, the controllability optimization design to composite wave-absorbing and camouflage function is realized, overcomes biography The deficiency of system blending method electromagnetism modified composite material.
To achieve the above object, the technical solution adopted by the present invention is：A kind of nano wave-absorption film functional modification is compound The method of laminate, comprises the following steps：(1) nano-particle and polyarylether resin are configured to the resin of stable homogeneous Solution；(2) resin solution prepared is prepared into by nano wave-absorption film using thin film preparation process；(3) by continuous fiber Or fabric is sufficiently impregnated preparing material prepreg with resin matrix；(4) nano wave-absorption film is coated with composite wood Between the laying for expecting prepreg, according to composite material process planning preparation structure/function integration camouflage composite material laminate.
In described (1) step, polyarylether resin is PAEK, polyether sulphone or poly (aryl ether sulfone ketone).
In (1) step, configure resin solution used in solvent be DMA, 1-METHYLPYRROLIDONE, Chloroform or dichloromethane.
In described (1) step, nano-particle is CNT, carbonyl iron dust, ferrite, iron, cobalt, nickel and its alloy In one or more, particle diameter is 5-60 nm.
In (2) step, described thin film preparation process refers to the tape casting technique or electrostatic spinning process.
In (3) step, described continuous fiber refers to glass fibre, carbon fiber, aramid fiber or pbo fiber, fiber Fabric is the plain or twill that above-mentioned fibrage forms.
In (3) step, described resin matrix is epoxy-resin systems or bimaleimide resin.
In (4) step, described moulding process refers to die press technology for forming or autoclave forming process.
Described (1) step is specially：The nano-particle that mass percent is 5-10% is added in a solvent, is carried out 0.5-2h ultrasonic disperse processing, sonification power 300-1000W, frequency 20-40KHz, then adds polyarylether tree Fat, resin demand are the 15-30% of solvent load, at 40-80 DEG C after mechanical agitation 1-3h, then carry out 10-40min ultrasound Decentralized processing, standing, continue after temperature is down to room temperature after stirring 1-2h, using homogenous disperse instrument at 10000-18000 revs/min Rotating speed under handle 10-30min, nano-particle finely dispersed resin solution is made；
Described (3) step is specially：Resin base by continuous fiber or its fabric with weight/mass percentage composition for 5-50% After liquid solution is sufficiently impregnated, removing solvent obtains material prepreg at a temperature of 30-50 DEG C；
Described (4) step is specially：Nano wave-absorption film is cut with material prepreg according to grinding tool size Afterwards, inserted by the ply sequence of setting in grinding tool, camouflage composite material laminate is prepared using moulding process, the temperature of shaping is 80-230 DEG C, pressure 0.5-5MPa.
The tape casting technique comprises the following steps in described (2) step：By the finely dispersed resin solution of nano-particle Plastic film mulch on smooth metallic plate is poured on, then film is placed in appropriate solvent bath after immersion removing residual solvent, then moved to Dried in air dry oven at a temperature of 50-170 DEG C, nano wave-absorption film is made.
Electrostatic spinning process comprises the following steps in described (2) step：The resin of the stable homogeneous prepared is molten Liquid injection electrostatic spinning apparatus syringe in, syringe spinning head internal diameter is 0.5-1.6mm, use stainless steel plate or aluminium foil for Receiver, spinning head to receiver distance is 5-30cm, and 10-30KV DC voltage is added between spinning head and collector, Nanofiber can be continuously produced, nano fiber non-woven fabric will be collected into from receiver and is placed in appropriate solvent bath Immersion is then moved in air dry oven and dried at a temperature of 50-170 DEG C, nanofiber is made and inhales to remove remaining solvent Ripple film.
The beneficial effect that is reached of the present invention is：This method has given full play to the programmable unique texture of composite lay Advantage, on the premise of composite conventional molding process is not changed substantially, wave energy layer will be inhaled and be integrated in laminated composite In the preparation process of plate, significantly and the at low cost overall suction wave energy of Synchronous lifting composite and mechanical property.System Product have excellent carrying and stealthy dual-use function concurrently, are had broad application prospects in Aerospace Engineering field.
Brief description of the drawings
Fig. 1：The structural representation of nano wave-absorption film functional modification composite material laminated board；
Fig. 2：The reflectance curve figure of nano wave-absorption film functional modification composite material laminated board.
Embodiment
With reference to embodiment, the present invention is further illustrated.
In embodiment
Epoxy resin is commercial products, from any of E51, E44, E54, E20；
Bimaleimide resin is commercial products, from any of QY8911- I, II, III and 5405；
Described glass fibre, carbon fiber, pbo fiber, aramid fiber and its plain or twill are commercial products；
Described CNT, carbonyl iron dust, ferrite, iron, cobalt, nickel and its alloy is commercial products；
Described PAEK, polyether sulphone, PPESK are commercial products；
Described DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE, chloroform, dichloromethane are commercial products.
Embodiment 1
Nano-particle is selected：Carbonyl iron dust and ferritic blend, particle diameter are 20 nm；
Polyarylether resin is selected：PAEK；
The solvent used in resin solution is configured to select：DMAC N,N' dimethyl acetamide；
Continuous fiber is selected：Carbon fiber；
Resin matrix is selected：Bimaleimide resin；
Moulding process is selected：Die press technology for forming；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) nanometer carbonyl iron dust and ferritic blend are configured to the resin solution of stable homogeneous with PAEK
Specially：Using DMA as solvent, the nanometer carbonyl iron that mass percent concentration is 10% is added Powder and ferritic blend, the ultrasonic disperse for carrying out 2h are handled, sonification power 1000W, frequency 40KHz, then Ketone-grouped resin is added, resin demand is the 30% of solvent load, at 40 DEG C after mechanical agitation 3h, then carries out the super of 40min Sound decentralized processing, stand, continue after temperature is down to room temperature after stirring 1h, utilize rotating speed of the homogenous disperse instrument at 18000 revs/min Lower processing 30min, carbonyl iron dust and the finely dispersed resin solution of ferrite blend is made；
(2) resin solution prepared is prepared into by nano wave-absorption film using the tape casting technique
Specially：Nanometer carbonyl iron dust and the finely dispersed resin solution of ferrite blend are poured on smooth metallic plate Upper plastic film mulch, then film is placed in appropriate solvent bath after immersion removing residual solvent, then moved in air dry oven 170 Dried at a temperature of DEG C, nano wave-absorption film is made；
(3) continuous carbon fibre and bismaleimide resin solution are sufficiently impregnated preparing material prepreg
Specially：Continuous carbon fibre is abundant for 50% bimaleimide resin/acetone soln with weight/mass percentage composition After dipping, removing solvent obtains material prepreg at a temperature of 50 DEG C；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, camouflage composite material laminate is prepared using die press technology for forming, the temperature of compression molding is 230 DEG C, pressure 5MPa.
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 5-8GHz band radars Below ripple absorption value -5dB, below 8-18GHz band radar ripple absorption values -10dB, -18dB is reached as high as, as shown in Figure 2. Product has excellent carrying and stealthy dual-use function concurrently, is had broad application prospects in Aerospace Engineering field.
Embodiment 2
In the present embodiment
Nano-particle is selected：CNT, particle diameter 5nm；
Polyarylether resin is selected：PAEK；
The solvent used in resin solution is configured to select：Dichloromethane；
Continuous fiber is selected：Glass fibre；
Resin matrix is selected：Epoxy-resin systems；
Moulding process is selected：Die press technology for forming；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) CNT and PAEK are configured to the resin solution of stable homogeneous
Specially：Using dichloromethane as solvent, the CNT that mass percent is 5% is added, carries out 0.5h ultrasound point Processing is dissipated, then sonification power 300W, frequency 20KHz add ketone-grouped resin, resin demand is solvent load 15%, at 40 DEG C after mechanical agitation 1h, then carry out 10min ultrasonic disperse processing, stand, it is follow-up to treat that temperature is down to room temperature After continuous stirring 1h, 10min is handled under 10000 revs/min of rotating speed using homogenous disperse instrument, it is finely dispersed that CNT is made Resin solution；
(2) resin solution prepared is prepared into by nano wave-absorption film using the tape casting technique
Specially：The finely dispersed resin solution of CNT is poured on plastic film mulch on smooth metallic plate, then by film It is placed in appropriate solvent bath after immersion removing residual solvent, then moves in air dry oven and dried at a temperature of 50 DEG C, made Obtain nano wave-absorption film.
(3) continuous glass fibre and epoxy-resin systems are sufficiently impregnated preparing material prepreg
Specially：By continuous glass fibre and epoxy-resin systems（Epoxy resin, curing agent diaminodiphenyl-methane and Diluent polyethyleneglycol diglycidylether blend, mass ratio 1: 0.2: 0.2）After being sufficiently impregnated, glass fibre is prepared Reinforced epoxy prepreg；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, camouflage composite material laminate is prepared using die press technology for forming, the temperature of compression molding is 80 DEG C, and pressure is 0.5MPa。
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 6-10GHz band radars Below ripple absorption value -5dB, reaches as high as -8dB.Product has excellent carrying and stealthy dual-use function concurrently, in Aerospace Engineering Field has broad application prospects.
Embodiment 3
Nano-particle is selected：Carbonyl iron dust, particle diameter are 60 nm；
Polyarylether resin is selected：Polyether sulphone；
The solvent used in resin solution is configured to select：1-METHYLPYRROLIDONE；
Continuous fiber is selected：Carbon fiber；
Resin matrix is selected：Bimaleimide resin；
Moulding process is selected：Autoclave forming process；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) nanometer carbonyl iron dust and polyether sulphone are made to the resin solution of stable homogeneous
Specially：1-METHYLPYRROLIDONE is solvent, the nanometer carbonyl iron dust that addition mass percent is 10%, carries out 2h Ultrasonic disperse processing, then sonification power 1000W, frequency 40KHz add polyether sulphone, resin demand is molten The 30% of agent dosage, at 80 DEG C after mechanical agitation 3h, then carry out 40min ultrasonic disperse processing, stand, treat that temperature is down to room Continue after temperature after stirring 2h, 30min is handled under 18000 revs/min of rotating speed using homogenous disperse instrument, obtained carbonyl iron dust disperses Uniform resin solution；
(2) resin solution prepared is prepared into by nano wave-absorption film using electrostatic spinning process
Specially：By the syringe of the finely dispersed resin solution injection electrostatic spinning apparatus of the carbonyl iron dust prepared In, syringe spinning head internal diameter is 1.6mm, uses stainless steel plate or aluminium foil as receiver, and spinning head to receiver distance is 30cm, 30KV DC voltage is added between spinning head and collector, you can nanofiber is continuously produced, will be from connecing Receive to be collected into nano fiber non-woven fabric on device and be placed in appropriate solvent bath and soak to remove remaining solvent, then move to air blast and do Dried in dry case at a temperature of 140 DEG C, nanofiber wave absorbing thin film is made.
(3) continuous carbon fibre and bimaleimide resin solution are sufficiently impregnated preparing material prepreg
Specially：Continuous carbon fibre is sufficiently impregnated with weight/mass percentage composition for 50% bimaleimide resin solution Afterwards, solvent is removed at a temperature of 50 DEG C and obtains material prepreg；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, and it is sealed in vacuum bag and is then placed in autoclave, forming temperature is 200 DEG C, pressure 3MPa.
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 8-15GHz band radars Below ripple absorption value -8dB, reaches as high as -11dB.Product has excellent carrying and stealthy dual-use function concurrently, in Aero-Space work Journey field has broad application prospects.
Embodiment 4
Nano-particle is selected：Ferrite, particle diameter 40nm；
Polyarylether resin is selected：Poly (aryl ether sulfone ketone)；
The solvent used in resin solution is configured to select：DMAC N,N' dimethyl acetamide；
Continuous fiber is selected：Aramid fiber；
Resin matrix is selected：Epoxy-resin systems；
Moulding process is selected：Die press technology for forming；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) nanometer ferrite and poly (aryl ether sulfone ketone) are configured to the resin solution of stable homogeneous
Specially：Using DMA as solvent, addition mass percent is 8% nanometer ferrite, is carried out 1.5h ultrasonic disperse processing, sonification power 700W, frequency 30KHz, then adds poly (aryl ether sulfone ketone), resin demand For the 20% of solvent load, at 60 DEG C after mechanical agitation 2h, then carry out 30min ultrasonic disperse processing, stand, treat that temperature drops Continue after to room temperature after stirring 1.5h, 20min is handled under 15000 revs/min of rotating speed using homogenous disperse instrument, ferrite is made Finely dispersed resin solution；
(2) resin solution prepared is prepared into by nano wave-absorption film using the tape casting technique
Specially：The finely dispersed resin solution of ferrite is poured on plastic film mulch on smooth metallic plate, then put film In appropriate solvent bath after immersion removing residual solvent, then move in air dry oven and dried at a temperature of 100 DEG C, is made Nano wave-absorption film.
(3) continuous aramid fiber and epoxy-resin systems are sufficiently impregnated preparing material prepreg
Specially：By continuous aramid fiber and epoxy-resin systems（Epoxy resin, curing agent diaminodiphenyl-methane and Diluent polyethyleneglycol diglycidylether blend, mass ratio 1: 0.2: 0.2）After being sufficiently impregnated, fiber reinforcement is prepared Epoxy prepreg；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, camouflage composite material laminate is prepared using die press technology for forming, the temperature of compression molding is 90 DEG C, pressure 3MPa.
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 14-18GHz wave band thunders Up to below ripple absorption value -10dB, -13dB is reached as high as.Product has excellent carrying and stealthy dual-use function concurrently, in Aero-Space Engineering field has broad application prospects.
Embodiment 5
Nano-particle is selected：Iron particle, particle diameter 20nm；
Polyarylether resin is selected：PAEK；
The solvent used in resin solution is configured to select：Chloroform；
Continuous fiber is selected：Pbo fiber；
Resin matrix is selected：Bimaleimide resin；
Moulding process is selected：Die press technology for forming；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) nano-iron particle and PAEK are configured to the resin solution of stable homogeneous
Specially：Using chloroform as solvent, mass percent is added as 6% nano-iron particle, at the ultrasonic disperse for carrying out 1h Reason, sonification power 500W, frequency 25KHz, PAEK then being added, resin demand is the 18% of solvent load, At 50 DEG C after mechanical agitation 1.5h, then carry out 20min ultrasonic disperse processing, stand, continue to stir after temperature is down to room temperature After 1.8h, 15min is handled under 12000 revs/min of rotating speed using homogenous disperse instrument, it is molten that the finely dispersed resin of iron particle is made Liquid；
(2) resin solution prepared is prepared into by nano wave-absorption film using electrostatic spinning process
Specially：The finely dispersed resin solution of the iron particle prepared is injected in the syringe of electrostatic spinning apparatus, Syringe spinning head internal diameter is 1.6mm, uses stainless steel plate or aluminium foil as receiver, and spinning head to receiver distance is 30cm, 30KV DC voltage is added between spinning head and collector, you can nanofiber is continuously produced, will be from receiver On be collected into nano fiber non-woven fabric and be placed in appropriate solvent bath and soak to remove remaining solvent, then move to air dry oven In dried at a temperature of 80 DEG C, nanofiber wave absorbing thin film is made.
(3) continuous P BO fibers and bimaleimide resin solution are sufficiently impregnated preparing material prepreg
Specially：Continuous P BO fibers are sufficiently impregnated with weight/mass percentage composition for 50% bimaleimide resin solution Afterwards, solvent is removed at a temperature of 35 DEG C and obtains material prepreg；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, camouflage composite material laminate is prepared using die press technology for forming, the temperature of compression molding is 230 DEG C, pressure 4MPa.
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 12-14GHz wave band thunders Up to below ripple absorption value -10dB, -12dB is reached as high as.Product has excellent carrying and stealthy dual-use function concurrently, in Aero-Space Engineering field has broad application prospects.
Embodiment 6
Nano-particle is selected：Cobalt particle, particle diameter 50nm；
Polyarylether resin is selected：PAEK；
The solvent used in resin solution is configured to select：1-METHYLPYRROLIDONE；
Fabric is selected：Aramid fiber plain；
Resin matrix is selected：Epoxy-resin systems；
Moulding process is selected：Die press technology for forming；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) nanometer cobalt particle and PAEK are configured to the resin solution of stable homogeneous
Specially：Using 1-METHYLPYRROLIDONE as solvent, addition mass percent is 8% nanometer cobalt particle, carries out 0.8h Ultrasonic disperse processing, then sonification power 900W, frequency 35KHz add PAEK, resin demand is solvent The 28% of dosage, at 70 DEG C after mechanical agitation 2.5h, then carry out 15min ultrasonic disperse processing, stand, treat that temperature is down to room Continue after temperature after stirring 1.1h, 12min is handled under 11000 revs/min of rotating speed using homogenous disperse instrument, obtained cobalt particle disperses Uniform resin solution；
(2) resin solution prepared is prepared into by nano wave-absorption film using the tape casting technique
Specially：The finely dispersed resin solution of nanometer cobalt is poured on plastic film mulch on smooth metallic plate, then put film In appropriate solvent bath after immersion removing residual solvent, then move in air dry oven and dried at a temperature of 140 DEG C, is made Nano wave-absorption film.
(3) aramid fiber plain and epoxy-resin systems are sufficiently impregnated preparing material prepreg
Specially：By aramid fiber plain and epoxy-resin systems（Epoxy resin, curing agent diaminodiphenyl-methane And diluent polyethyleneglycol diglycidylether blend, mass ratio 1: 0.2: 0.2）After being sufficiently impregnated, fiber increasing is prepared Strong epoxy prepreg；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, camouflage composite material laminate is prepared using die press technology for forming, the temperature of compression molding is 100 DEG C, and pressure is 4.5MPa。
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 6-15GHz band radars Below ripple absorption value -5dB, reaches as high as -10dB.Product has excellent carrying and stealthy dual-use function concurrently, in Aero-Space work Journey field has broad application prospects.
Embodiment 7
Nano-particle is selected：Nickel particles, particle diameter are 50 nm；
Polyarylether resin is selected：PAEK；
The solvent used in resin solution is configured to select：DMAC N,N' dimethyl acetamide；
Fabric is selected：Glass fibre twill；
Resin matrix is selected：Bimaleimide resin；
Moulding process is selected：Autoclave forming process；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) nanometer nickel particles and PAEK are configured to the resin solution of stable homogeneous；、
Specially：Using DMA as solvent, addition mass percent is 9% nanometer nickel particles, is carried out Then 1.6h ultrasonic disperse processing, sonification power 400W, frequency 25KHz add ketone-grouped resin, resin is used Measure as the 28% of solvent load, at 70 DEG C after mechanical agitation 2.2h, then carry out 35min ultrasonic disperse processing, stand, treat temperature Degree continues after stirring 1.8h after being down to room temperature, handles 20min under 17000 revs/min of rotating speed using homogenous disperse instrument, nickel is made The finely dispersed resin solution of particle；
(2) resin solution prepared is prepared into by nano wave-absorption film using electrostatic spinning process
Specially：The finely dispersed resin solution of the nickel particles prepared is injected in the syringe of electrostatic spinning apparatus, Syringe spinning head internal diameter is 1.2mm, uses stainless steel plate or aluminium foil as receiver, and spinning head to receiver distance is 25cm, 27KV DC voltage is added between spinning head and collector, you can nanofiber is continuously produced, will be from receiver On be collected into nano fiber non-woven fabric and be placed in appropriate solvent bath and soak to remove remaining solvent, then move to air dry oven In dried at a temperature of 170 DEG C, nanofiber wave absorbing thin film is made.
(3) glass fibre twill and bimaleimide resin solution are sufficiently impregnated preparing material prepreg
Specially：Glass fibre twill is abundant for 30% bimaleimide resin solution with weight/mass percentage composition After dipping, removing solvent obtains material prepreg at a temperature of 35 DEG C；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, and it is sealed in vacuum bag and is then placed in autoclave, forming temperature is 180 DEG C, pressure 3MPa.
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 7-14GHz band radars Below ripple absorption value -5dB, reaches as high as -10dB.Product has excellent carrying and stealthy dual-use function concurrently, in Aero-Space work Journey field has broad application prospects.
Embodiment 8
Nano-particle is selected：Iron-nickel alloy particle and CNT blend, particle diameter are 20 nm；
Polyarylether resin is selected：Poly (aryl ether sulfone ketone)；
The solvent used in resin solution is configured to select：Chloroform；
Continuous fiber is selected：Carbon fiber；
Resin matrix is selected：Epoxy-resin systems；
Moulding process is selected：Die press technology for forming；
As shown in Figure 1, a kind of method of nano wave-absorption film functional modification composite material laminated board, including following step Suddenly：
(1) Nanoscale Iron nickel alloy particles and CNT blend are configured to the tree of stable homogeneous with poly (aryl ether sulfone ketone) Lipoprotein solution
Specially：Using chloroform as solvent, addition mass percent is that 8% Nanoscale Iron nickel alloy particles and CNT are total to Mixed thing, 0.6h ultrasonic disperse processing is carried out, sonification power 600W, frequency 39KHz, then adds poly (aryl ether sulfone ketone) Resin, resin demand is the 22% of solvent load, at 77 DEG C after mechanical agitation 2.8h, then is carried out at 30min ultrasonic disperse Reason, stand, continue after temperature is down to room temperature after stirring 1.6h, handled using homogenous disperse instrument under 16000 revs/min of rotating speed 29min, iron-nickel alloy particle and the finely dispersed resin solution of CNT particle blend is made；
(2) resin solution prepared is prepared into by nano wave-absorption film using electrostatic spinning process
Specially：By the Nanoscale Iron nickel alloy particles prepared and the finely dispersed resin solution note of CNT blend In the syringe for entering electrostatic spinning apparatus, syringe spinning head internal diameter is 1.5mm, uses stainless steel plate or aluminium foil as receiver, Spinning head to receiver distance is 26cm, 15KV DC voltage is added between spinning head and collector, you can successively Ground produce nanofiber, will be collected into from receiver nano fiber non-woven fabric be placed in appropriate solvent bath soak it is surplus to remove Remaining solvent, then move in air dry oven and dried at a temperature of 80 DEG C, nanofiber wave absorbing thin film is made.
(3) continuous carbon fibre and epoxy-resin systems are sufficiently impregnated preparing material prepreg
Specially：By continuous carbon fibre and epoxy-resin systems（Epoxy resin, curing agent diaminodiphenyl-methane and dilute Release agent polyethyleneglycol diglycidylether blend, mass ratio 1: 0.2: 0.2）After being sufficiently impregnated, fiber reinforcement ring is prepared Oxygen resin prepreg material；
(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite material process planning system Standby structure/function integration camouflage composite material laminate
Specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, alternating is layed in mill In tool, camouflage composite material laminate is prepared using die press technology for forming, the temperature of compression molding is 100 DEG C, pressure 3MPa.
Obtained structure/function integration camouflage composite material laminate absorbing property is excellent, in 6-14GHz band radars Below ripple absorption value -8dB, reaches as high as -12dB.Product has excellent carrying and stealthy dual-use function concurrently, in Aero-Space work Journey field has broad application prospects.

Claims (6)

  1. A kind of 1. method of nano wave-absorption film functional modification composite material laminated board, it is characterised in that:Including following step Suddenly：(1) nano-particle and polyarylether resin are configured to the resin solution of stable homogeneous；(2) use thin film preparation process will The resin solution prepared is prepared into nano wave-absorption film；(3) continuous fiber or fabric are sufficiently impregnated with resin matrix Prepare material prepreg；(4) nano wave-absorption film is coated between the laying of material prepreg, according to composite wood Expect moulding process preparation structure/function integration camouflage composite material laminate；
    Described (1) step is specially：The nano-particle that mass percent is 5-10% is added in a solvent, carries out 0.5-2h's Then ultrasonic disperse processing, sonification power 300-1000W, frequency 20-40KHz add polyarylether resin, resin is used Measure the 15-30% for solvent load, at 40-80 DEG C after mechanical agitation 1-3h, then carry out 10-40min ultrasonic disperse processing, Stand, continue after temperature is down to room temperature after stirring 1-2h, using homogenous disperse instrument under 10000-18000 revs/min of rotating speed 10-30min is handled, the dispersed resin solution of nano-particle is made；
    Described (3) step is specially：Resin matrix solution by continuous fiber or its fabric with weight/mass percentage composition for 5-50% After being sufficiently impregnated, removing solvent obtains material prepreg at a temperature of 30-50 DEG C；
    Described (4) step is specially：After nano wave-absorption film and material prepreg are cut according to grinding tool size, by setting Fixed ply sequence is inserted in grinding tool, prepares camouflage composite material laminate using moulding process, the temperature of shaping is 80-230 DEG C, pressure 0.5-5MPa；
    In described (2) step, thin film preparation process refers to the tape casting technique or electrostatic spinning process；Under the tape casting technique includes Row step：The dispersed resin solution of nano-particle is poured on plastic film mulch on smooth metallic plate, is then placed in film suitably Solvent bath in immersion removing residual solvent after, then move in air dry oven and dried at a temperature of 50-170 DEG C, be made receive Rice wave absorbing thin film；
    Electrostatic spinning process comprises the following steps：The resin solution of the stable homogeneous prepared is injected to the note of electrostatic spinning apparatus In emitter, syringe spinning head internal diameter is 0.5-1.6mm, uses stainless steel plate or aluminium foil as receiver, spinning head to receiver Distance is 5-30cm, 10-30KV DC voltage is added between spinning head and collector, you can continuously produce nanometer Fiber, nano fiber non-woven fabric will be collected into from receiver and is placed in appropriate solvent bath and is soaked to remove remaining solvent, Then move in air dry oven and dried at a temperature of 50-170 DEG C, nanofiber wave absorbing thin film is made.
  2. 2. the method for nano wave-absorption film functional modification composite material laminated board according to claim 1, its feature exist In:In described (1) step, polyarylether resin is PAEK, polyether sulphone or poly (aryl ether sulfone ketone).
  3. 3. the method for nano wave-absorption film functional modification composite material laminated board according to claim 1, its feature exist In:In described (1) step, the solvent configured used in resin solution is DMA, N- crassitudes Ketone, chloroform or dichloromethane.
  4. 4. the method for nano wave-absorption film functional modification composite material laminated board according to claim 1, its feature exist In:In described (1) step, nano-particle is in CNT, carbonyl iron dust, ferrite, iron, cobalt, nickel and its alloy One or more, particle diameter are 5-60 nm.
  5. 5. the method for nano wave-absorption film functional modification composite material laminated board according to claim 1, its feature exist In:In described (3) step, described continuous fiber refers to glass fibre, carbon fiber, aramid fiber or pbo fiber, fiber Fabric is the plain or twill that above-mentioned fibrage forms；Described resin matrix is epoxy resin or BMI Resin.
  6. 6. the method for nano wave-absorption film functional modification composite material laminated board according to claim 1, its feature exist In:In described (4) step, described moulding process refers to die press technology for forming or autoclave forming process.
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