CN110039841A - A kind of preparation method of the honeycomb sandwich structure Wave suction composite material of bowknot shape Co/C nano wave-absorbing material filling - Google Patents
A kind of preparation method of the honeycomb sandwich structure Wave suction composite material of bowknot shape Co/C nano wave-absorbing material filling Download PDFInfo
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- CN110039841A CN110039841A CN201810034216.8A CN201810034216A CN110039841A CN 110039841 A CN110039841 A CN 110039841A CN 201810034216 A CN201810034216 A CN 201810034216A CN 110039841 A CN110039841 A CN 110039841A
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- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 239000011358 absorbing material Substances 0.000 title claims abstract description 39
- 238000011049 filling Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000159 gelatin Polymers 0.000 claims abstract description 39
- 239000008273 gelatin Substances 0.000 claims abstract description 39
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 32
- 108010010803 Gelatin Proteins 0.000 claims abstract description 31
- 235000019322 gelatine Nutrition 0.000 claims abstract description 31
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 31
- 230000001413 cellular effect Effects 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 13
- 239000010941 cobalt Substances 0.000 claims abstract description 11
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000805 composite resin Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims abstract description 9
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 7
- 239000004917 carbon fiber Substances 0.000 claims abstract description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 50
- 238000010438 heat treatment Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 28
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 22
- 239000004202 carbamide Substances 0.000 claims description 22
- 239000003292 glue Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000002023 wood Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910021645 metal ion Inorganic materials 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 238000013459 approach Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000011152 fibreglass Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 19
- 238000003760 magnetic stirring Methods 0.000 description 6
- 239000002114 nanocomposite Substances 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 239000004643 cyanate ester Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- GJCOSYZMQJWQCA-UHFFFAOYSA-N 9H-xanthene Chemical compound C1=CC=C2CC3=CC=CC=C3OC2=C1 GJCOSYZMQJWQCA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
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- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
- B32B3/08—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/10—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material
- B32B3/12—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material characterised by a layer of regularly- arranged cells, e.g. a honeycomb structure
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- 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
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- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- B32B7/00—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
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/212—Electromagnetic interference shielding
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Abstract
The invention discloses a kind of preparation methods of the honeycomb sandwich structure Wave suction composite material of bowknot shape Co/C nano wave-absorbing material filling, it is related to electromagnetism stealth technical field of composite materials, this method has cobalt ions-gelatin copolymer presoma of bow-tie shape by hydro-thermal method synthesis using cobalt nitrate and gelatin as raw material；It is subsequently heat-treated that a kind of nano combined absorbing material of the Co/C with bow-tie shape hierarchical structure is prepared.The Co/C nano wave-absorbing material being prepared is filled into the cellular honeycomb of periodical aramid fiber, and it is covered each by galss fiber reinforced resin based composites covering and carbon fiber enhancement resin base composite material covering in the upper and lower sides of filled honeycomb, obtain the cellular sandwich Wave suction composite material of the nano combined absorbing material filling of bowknot shape Co/C.Solving, the effective absorption band of traditional absorbing material is narrow, the technical problem of mechanics bearing capacity difference.
Description
Technical field
The present invention relates to electromagnetism stealth technical field of composite materials, more particularly to a kind of bowknot shape Co/C nano wave-absorption
The preparation method of the honeycomb sandwich structure Wave suction composite material of material filling.
Background technique
Military domain is the weaponry of representative by more using military fighter aircraft with the development of modern radar Detection Techniques
Come more frequent tracking and detecting；Meanwhile in civil field, the development of telecommunication technology is bringing the convenient life of people
Serious electromagnetic radiation pollution problem is also brought simultaneously.Thus, it is possible to by electromagnetic wave energy be converted into heat energy loss fall to
The electromagnetic wave absorbent material for significantly reducing reflection of electromagnetic wave receives increasingly as the most effective solution to solve the above problems
More concerns.Due to the limitation of practical service environment, ideal electromagnetic wave absorbent material performance characteristics include: effective absorption band
Width, density of material is light, material thickness is thin, mechanical strength is high.Magnetic cobalt and its oxide and carbon base body composite wave-suction material due to
There is dielectric loss and magnetic hystersis loss to electromagnetic wave simultaneously.As one of widest wave absorbing agent is studied at present, magnetic Co/C is received
The carbon base body of nano composite material to electromagnetic wave have excellent dielectric loss performance, and domain wall resonance and natural resonance be its cobalt and
The most important magnetic loss absorption mechanism of its oxide.Magnetic Co/C nanocomposite is high with magnetic coercive force, it is high to inhale intensity of wave,
The advantages that simple is prepared, and as double lossy mediums, has dielectric loss, but its relative density again to the existing magnetic loss of electromagnetic wave
Greatly, the disadvantages of absorption band is narrow is difficult to meet the requirement of outstanding wave absorbing agent " thin, light, wide, strong ", limits it and further answers
With.To be in powdered be traditional magnetic Co/C nanocomposite more to be mixed and made into antiradar coatings with coating using technique simultaneously
Main, use process is easy to wear to fall off, it is difficult to meet contemporary aircraft for radar absorbing structural bearing and electromagnetic wave absorption function
It can integrated requirement.
Summary of the invention
In order to overcome above-mentioned traditional magnetic Co/C nanocomposite be in more it is powdered using technique with coating mix make
Relatively denser, absorption band is narrow based on antiradar coatings, mechanics bearing capacity is poor, use process is easy to wear falls off, it is difficult to full
The prior arts such as requirement of the sufficient contemporary aircraft for radar absorbing structural bearing and electromagnetic wave absorption function integration are not
Foot, the present invention provides a kind of systems of the honeycomb sandwich structure Wave suction composite material of bowknot shape Co/C nano wave-absorbing material filling
Preparation Method.
The technical scheme adopted by the invention is that: it is made using cobalt nitrate, gelatin, urea by raw material three-step approach, first with nitre
Sour cobalt and gelatin are raw material, prepare long chain cobalt ions-gelatin molecule metal ion polymer organic frame by solution thermal method
Frame；Then using urea as aids precipitation agent, there is the metal of bow-tie shape by the synthesis of autoclave high temperature hydro-thermal method
Ion-polymer cooperates presoma；Then the method that high-temperature heat treatment is used after being dried, by Co metal ion and bright
Xanthan polymer cooperates presoma, is prepared into a kind of nano combined absorbing material of the Co/C with bow-tie shape hierarchical structure.
The nano combined absorbing material of bowknot shape Co/C being prepared is filled into the cellular honeycomb hole of periodical aramid fiber, and is being filled out
It fills cellular upper and lower sides and is covered each by galss fiber reinforced resin based composites covering and carbon fiber enhancement resin base composite wood
Expect covering, finally obtains the cellular sandwich Wave suction composite material of the nano combined absorbing material filling of bowknot shape Co/C.Using state
Army's mark GJB 2038A-2011 arch frame method tests composite panel 2-18GHz reflection of electromagnetic wave rate, under 3mm thickness
Reflection loss is lower than effective absorption band width 9.8GHz of -10dB, and absorption maximum intensity reaches -49.9dB.
Specifically:
(1) in deionized water by cobalt nitrate, urea dissolution, stirring and dissolving obtains liquid A；By gelatin heating, stirring and dissolving
In deionized water, liquid B is obtained；Then liquid A and liquid B are mixed, heating reaction obtains cobalt ions-gelatin molecule metal
Ionomer organic frame glue mixed solution.
(2) glue mixed solution obtained in (1) is taken to be added in poly- four volts of ethylene liner reaction kettle, high temperature hydro-thermal reaction obtains
To bowknot shape presoma, precipitating is collected by centrifugation, it is dry.
(3) the bowknot shape precursor samples after will be dry obtained in (2), are placed in tube furnace, under protective gas
High-temperature heat treatment 2h obtains the Co/C nano wave-absorbing material of bow-tie shape.
(4) the Co/C nano wave-absorbing material of the bow-tie shape prepared in (3) is filled into periodical aramid fiber cellular board,
1mm thick fiberglass reinforced resin based composites wave transparent covering is covered in cellular board using the method for glue film bonding respectively up and down
With carbon fiber enhancement resin base composite material covering, the cellular sandwich of bowknot shape Co/C nano wave-absorbing material filling is finally obtained
Structure Wave suction composite material.
Preferably, the mass ratio of cobalt nitrate and urea is 1:1 in step (1)；Cobalt nitrate, urea are dissolved in deionized water
In, the mass volume ratio (g/mL) of cobalt nitrate and deionized water is 1:16；Gelatin heating temperature is 50 DEG C；Gelatin go from
In sub- water, the mass volume ratio (g/mL) of gelatin and deionized water is 1:5-1:10；The liquid A is mixed with liquid B, liquid A
The mass ratio of gelatin is 1:0.5-1:2 in middle cobalt nitrate and liquid B；Heating stirring is reacted after liquid A is mixed with liquid B, temperature
It is 60 DEG C -80 DEG C, time 1h.
Preferably, step (2) the high temperature hydrothermal temperature is 100 DEG C -110 DEG C, reaction time 6-10h；Centrifugation
Time is 5-15min, centrifugal condition 7000-9000rpm；The drying, temperature must not exceed 80 DEG C.
Preferably, step (3) protective gas is nitrogen or argon gas；The high-temperature heat treatment, temperature are 400 DEG C -600
℃。
Preferably, step (4) the periodical aramid fiber cellular board, aperture 2mm-10mm；Table on filled cellular board
The resin matrix of the galss fiber reinforced resin based composites wave transparent covering of face covering is epoxy resin or cyanate ester resin.
Compared with prior art, the beneficial effects of the invention are as follows
(1) the cobalt ions gelatin metal organic frame presoma with special bow-tie shape has been synthesized using hydro-thermal method,
And Co/C magnetic Nano composite wave-suction material has been obtained by heat treatment, it may be implemented pair by the control to the hydro-thermal reaction time
The Effective Regulation of product bowknot shape pattern saturation degree.
(2) method compound using Co/C magnetic nanometer composite material wave absorbing agent and honeycomb sandwich structure, is prepared for having
The broadband absorbing composite material of mechanics bearing capacity, by adjusting the laying of fiber in fiber-reinforced resin matrix compound material covering
Scheme can effectively control the mechanical strength of composite material, realize Wave suction composite material structural bearing and inhale the integration of wave energy
Design.
(3) compound with other materials, improve structural bearing and absorbing property.By the nano combined absorbing material of Co/C and
Special construction it is compound, while realizing broadband absorbing effect, reduce material thickness, it is strong to improve material entirety mechanics
Degree.
Detailed description of the invention
Fig. 1 is bowknot shape Co- gelatin metal organic frame presoma SEM photograph prepared by embodiment 1；
Fig. 2 is bowknot shape magnetism Co/C nanocomposite SEM photograph prepared by embodiment 1；
Fig. 3 is the nanomaterial-filled honeycomb sandwich structure composite material signal of the bowknot shape Co/C of the preparation of embodiment 1
Figure；
Fig. 4 is the nanomaterial-filled honeycomb sandwich structure composite panel 2- of the bowknot shape Co/C of the preparation of embodiment 1
The reflection of electromagnetic wave rate of 18GHz.
Specific embodiment
The following further describes the present invention with reference to the drawings.
Embodiment 1
(1) cobalt nitrate, urea are dissolved in deionized water medium-speed magnetic stirring 30min to whole dissolutions, obtain liquid A；
It will be dissolved in deionized water under the conditions of 50 DEG C of gelatin heating, medium-speed magnetic stirrings, be kept stirring state 30min, obtain liquid
B；Then cobalt nitrate and urea mixed solution and gelatin solution (i.e. liquid A and liquid B) are added in 250mL single-necked flask and are mixed
It closes, magnetic agitation is reacted under heating condition, and it is mixed to obtain cobalt ions-gelatin molecule metal ion polymer organic frame violet gum
Close solution.
(2) violet gum mixed solution obtained in (1) is taken to be added in the poly- four volts of ethylene liner reaction kettle of 100mL, hydro-thermal
Reaction certain time obtains bowknot shape presoma (see attached drawing 1), and precipitating is collected by centrifugation, and drying is stand-by for 24 hours.
(3) the bowknot shape precursor samples after will be dry obtained in (2), are placed in tube furnace, under protective gas
Heat treatment obtains the Co/C nano wave-absorbing material of bow-tie shape (see attached drawing 2).
(4) the Co/C nano wave-absorbing material of the bow-tie shape prepared in 50g (3) is filled into outer dimension is 300mm
In the periodical aramid fiber cellular board of × 300mm × 3mm, 1mm thickness is covered in cellular board using the method for glue film bonding respectively up and down
Galss fiber reinforced resin based composites wave transparent covering and carbon fiber enhancement resin base composite material covering, finally obtain butterfly
Tie the honeycomb sandwich structure Wave suction composite material of shape Co/C nano wave-absorbing material filling (see attached drawing 3).
The mass ratio of cobalt nitrate and urea is 1:1 in step (1)；Cobalt nitrate, urea dissolve in deionized water, cobalt nitrate
Mass volume ratio (g/mL) with deionized water is 1:16；Gelatin heating temperature is 50 DEG C；Gelatin is in deionized water, bright
Glue and the mass volume ratio (g/mL) of deionized water are 1:8；The liquid A is mixed with liquid B, cobalt nitrate and liquid in liquid A
The mass ratio of gelatin is 1:2 in B；Heating stirring is reacted after liquid A is mixed with liquid B, and temperature is 70 DEG C, time 1h.Step
(2) the high temperature hydrothermal temperature is 100 DEG C, reaction time 6h；Centrifugation time is 10min, and centrifugal condition is
9000rpm；The drying, 80 DEG C of temperature.
Step (3) protective gas is nitrogen；The high-temperature heat treatment, temperature are 800 DEG C.
Step (4) the periodical aramid fiber cellular board, aperture 4mm；The glass of filled cellular board upper surface covering
The resin matrix of fiber-reinforced resin matrix compound material wave transparent covering is epoxy resin.
(5) national military standard GJB 2038A-2011 electromagnetic wave absorption material reflectivity arch frame method is used, to bowknot shape obtained
Co/C nanomaterial-filled honeycomb sandwich structure composite panel 2-18GHz reflection of electromagnetic wave rate is tested, 3mm thickness
Lower reflection loss is lower than effective absorption band width 9.8GHz of -10dB, and absorption maximum intensity reaches -49.9dB (see attached drawing 4).
Embodiment 2
(1) cobalt nitrate, urea are dissolved in deionized water medium-speed magnetic stirring 30min to whole dissolutions, obtain liquid A；
It will be dissolved in deionized water under the conditions of 50 DEG C of gelatin heating, medium-speed magnetic stirrings, be kept stirring state 30min, obtain liquid
B；Then cobalt nitrate and urea mixed solution and gelatin solution (i.e. liquid A and liquid B) are added in 250mL single-necked flask and are mixed
It closes, magnetic agitation is reacted under heating condition, and it is mixed to obtain cobalt ions-gelatin molecule metal ion polymer organic frame violet gum
Close solution.
(2) violet gum mixed solution obtained in (1) is taken to be added in the poly- four volts of ethylene liner reaction kettle of 100mL, hydro-thermal
Reaction certain time obtains bowknot shape presoma, and precipitating is collected by centrifugation, and drying is stand-by for 24 hours.
(3) the bowknot shape precursor samples after will be dry obtained in (2), are placed in tube furnace, under protective gas
Heat treatment obtains the Co/C nano wave-absorbing material of bow-tie shape.
(4) the Co/C nano wave-absorbing material of the bow-tie shape prepared in 50g (3) is filled into outer dimension is 300mm
In the periodical aramid fiber cellular board of × 300mm × 3mm, 1mm thickness is covered in cellular board using the method for glue film bonding respectively up and down
Galss fiber reinforced resin based composites wave transparent covering and carbon fiber enhancement resin base composite material covering, finally obtain butterfly
Tie the honeycomb sandwich structure Wave suction composite material of shape Co/C nano wave-absorbing material filling.
The mass ratio of cobalt nitrate and urea is 1:1 in step (1)；Cobalt nitrate, urea dissolve in deionized water, cobalt nitrate
Mass volume ratio (g/mL) with deionized water is 1:16；Gelatin heating temperature is 50 DEG C；Gelatin is in deionized water, bright
Glue and the mass volume ratio (g/mL) of deionized water are 1:5；The liquid A is mixed with liquid B, cobalt nitrate and liquid in liquid A
The mass ratio of gelatin is 1:0.5 in B；Heating stirring is reacted after liquid A is mixed with liquid B, and temperature is 60 DEG C, time 1h.Step
Suddenly (2) described high temperature hydrothermal temperature is 100 DEG C, reaction time 6h；Centrifugation time is 5min, and centrifugal condition is
7000rpm；The drying, 80 DEG C of temperature.
Step (3) protective gas is argon gas；The high-temperature heat treatment, temperature are 400 DEG C.
Step (4) the periodical aramid fiber cellular board, aperture 2mm；The glass of filled cellular board upper surface covering
The resin matrix of fiber-reinforced resin matrix compound material wave transparent covering is cyanate ester resin.
(5) national military standard GJB 2038A-2011 electromagnetic wave absorption material reflectivity arch frame method is used, to bowknot shape obtained
Co/C nanomaterial-filled honeycomb sandwich structure composite panel 2-18GHz reflection of electromagnetic wave rate is tested, 3mm thickness
Lower reflection loss is lower than effective absorption band width 8.5GHz of -10dB, and absorption maximum intensity reaches -38dB.
Embodiment 3
(1) cobalt nitrate, urea are dissolved in deionized water medium-speed magnetic stirring 30min to whole dissolutions, obtain liquid A；
It will be dissolved in deionized water under the conditions of 50 DEG C of gelatin heating, medium-speed magnetic stirrings, be kept stirring state 30min, obtain liquid
B；Then cobalt nitrate and urea mixed solution and gelatin solution (i.e. liquid A and liquid B) are added in 250mL single-necked flask and are mixed
It closes, magnetic agitation is reacted under heating condition, and it is mixed to obtain cobalt ions-gelatin molecule metal ion polymer organic frame violet gum
Close solution.
(2) violet gum mixed solution obtained in (1) is taken to be added in the poly- four volts of ethylene liner reaction kettle of 100mL, hydro-thermal
Reaction certain time obtains bowknot shape presoma, and precipitating is collected by centrifugation, and drying is stand-by for 24 hours.
(3) the bowknot shape precursor samples after will be dry obtained in (2), are placed in tube furnace, under protective gas
Heat treatment obtains the Co/C nano wave-absorbing material of bow-tie shape.
(4) the Co/C nano wave-absorbing material of the bow-tie shape prepared in 50g (3) is filled into outer dimension is 300mm
In the periodical aramid fiber cellular board of × 300mm × 3mm, 1mm thickness is covered in cellular board using the method for glue film bonding respectively up and down
Galss fiber reinforced resin based composites wave transparent covering and carbon fiber enhancement resin base composite material covering, finally obtain butterfly
Tie the honeycomb sandwich structure Wave suction composite material of shape Co/C nano wave-absorbing material filling.
The mass ratio of cobalt nitrate and urea is 1:1 in step (1)；Cobalt nitrate, urea dissolve in deionized water, cobalt nitrate
Mass volume ratio (g/mL) with deionized water is 1:16；Gelatin heating temperature is 50 DEG C；Gelatin is in deionized water, bright
Glue and the mass volume ratio (g/mL) of deionized water are 1:10；The liquid A is mixed with liquid B, cobalt nitrate and liquid in liquid A
The mass ratio of gelatin is 1:2 in B；Heating stirring is reacted after liquid A is mixed with liquid B, and temperature is 80 DEG C, time 1h.Step
(2) the high temperature hydrothermal temperature is 110 DEG C, reaction time 10h；Centrifugation time is 15min, and centrifugal condition is
9000rpm；The drying, temperature 70 C.
Step (3) protective gas is nitrogen；The high-temperature heat treatment, temperature are 800 DEG C.
Step (4) the periodical aramid fiber cellular board, aperture 10mm；The glass of filled cellular board upper surface covering
The resin matrix of fiber-reinforced resin matrix compound material wave transparent covering is cyanate ester resin.
(5) national military standard GJB 2038A-2011 electromagnetic wave absorption material reflectivity arch frame method is used, to bowknot shape obtained
Co/C nanomaterial-filled honeycomb sandwich structure composite panel 2-18GHz reflection of electromagnetic wave rate is tested, 3mm thickness
Lower reflection loss is lower than effective absorption band width 7.6GHz of -10dB, and absorption maximum intensity reaches -35dB.
Claims (9)
1. a kind of preparation method of the honeycomb sandwich structure Wave suction composite material of bowknot shape Co/C nano wave-absorbing material filling,
It is characterized in that: being made using cobalt nitrate, gelatin, urea by raw material three-step approach；First using cobalt nitrate and gelatin as raw material, pass through solution
Thermal method prepares long chain cobalt ions-gelatin molecule metal ion polymer organic frame；Then using urea as aids precipitation
Agent by the synthesis of high temperature hydro-thermal method there is the metal ion-polymer of bow-tie shape to cooperate presoma；Then pass through at dry
Co metal ion and gelatin copolymer are cooperated presoma by the method that high-temperature heat treatment is used after reason, and being prepared into one kind has
The nano combined absorbing material of bowknot shape Co/C；The nano combined absorbing material of bowknot shape Co/C being prepared is filled into week
In the cellular honeycomb hole of phase property aramid fiber, and galss fiber reinforced resin based composites are covered each by the upper and lower sides of filled honeycomb
Covering and carbon fiber enhancement resin base composite material covering finally obtain the nano combined absorbing material filling of bowknot shape Co/C
Cellular sandwich Wave suction composite material.
2. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 1 inhales wave composite wood
The preparation method of material, which is characterized in that the specific steps of this method are as follows:
(1) in deionized water by cobalt nitrate, urea dissolution, stirring and dissolving obtains liquid A；Gelatin heating, stirring and dissolving are being gone
In ionized water, liquid B is obtained；Then liquid A and liquid B are mixed, heating reaction obtains cobalt ions-gelatin molecule metal ion
Polymer organic frame glue mixed solution；
(2) it takes glue mixed solution obtained in (1) to carry out high temperature hydro-thermal reaction and obtains bowknot shape presoma, it is heavy to be collected by centrifugation
It forms sediment, it is dry；
(3) the bowknot shape precursor samples after will be dry obtained in (2), are placed in tube furnace, high temperature under protective gas
Heat treatment 2h obtains the Co/C nano wave-absorbing material of bow-tie shape；
(4) the Co/C nano wave-absorbing material of the bow-tie shape prepared in (3) is filled into periodical aramid fiber cellular board, is used
The method of glue film bonding covers 1mm thick fiberglass reinforced resin based composites wave transparent covering and carbon in cellular board respectively up and down
Fiber-reinforced resin matrix compound material covering finally obtains the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling
Wave suction composite material.
3. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
The preparation method of material, it is characterised in that: the mass ratio of cobalt nitrate and urea is 1:1 in step (1)；Cobalt nitrate, urea are dissolved in
In deionized water, the mass volume ratio (g/mL) of cobalt nitrate and deionized water is 1:16.
4. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
The preparation method of material, it is characterised in that: step (1) the gelatin heating temperature is 50 DEG C；Gelatin is in deionized water, bright
Glue and the mass volume ratio (g/mL) of deionized water are 1:5-1:10.
5. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
The preparation method of material, it is characterised in that: step (1) described liquid A is mixed with liquid B, in liquid A cobalt nitrate with it is bright in liquid B
The mass ratio of glue is 1:0.5-1:2；Heating stirring react after liquid A and liquid B mix, and temperature is 60 DEG C -80 DEG C, and the time is
1h。
6. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
Preparation method for material, it is characterised in that: step (2) the high temperature hydrothermal temperature is 100 DEG C -110 DEG C, reaction time 6-
10h。
7. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
Preparation method for material, it is characterised in that: step (2) centrifugation time is 5-15min, centrifugal condition 7000-9000rpm；Institute
Drying is stated, temperature must not exceed 80 DEG C.
8. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
Preparation method for material, it is characterised in that: step (3) protective gas is nitrogen or argon gas；The high-temperature heat treatment, temperature are
400℃-800℃。
9. the honeycomb sandwich structure of bowknot shape Co/C nano wave-absorbing material filling according to claim 2 inhales wave composite wood
Preparation method for material, it is characterised in that: step (4) the periodical aramid fiber cellular board, aperture 2mm-10mm；Filled honeycomb
The resin matrix of the galss fiber reinforced resin based composites wave transparent covering of plate upper surface covering is epoxy resin or cyanate
Resin.
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| CN113777679A (en) * | 2021-08-13 | 2021-12-10 | 中国航天空气动力技术研究院 | Topological stealth structure and preparation method thereof |
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