CN109294519A - A kind of preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design - Google Patents
A kind of preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design Download PDFInfo
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- CN109294519A CN109294519A CN201811370065.XA CN201811370065A CN109294519A CN 109294519 A CN109294519 A CN 109294519A CN 201811370065 A CN201811370065 A CN 201811370065A CN 109294519 A CN109294519 A CN 109294519A
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Abstract
The invention discloses a kind of preparation methods of the wideband graphene absorbing material of multilayered structure concentration gradient design, the method comprises the following steps: Step 1: obtaining redox graphene hydrogel using the method for hydro-thermal method Chemical self-assembly；Step 2: preparing porous graphene sponge；Step 3: preparing the graphene sponge of different densities；Step 4: graphene sponge is filled into the cellular honeycomb hole of periodical aramid fiber, according to the sequence of graphene sponge concentration from small to large stacked arrangement from top to bottom；Step 5: honeycomb interlayer is using single layer quartz fibre reinforced resin based composites as articulamentum, it is covered each by quartz fibre reinforced resin based composites covering and carbon fiber enhancement resin base composite material covering splicing cellular upper and lower sides, obtains the wideband graphene absorbing material of multilayered structure concentration gradient design.Wideband graphene absorbing material prepared by the present invention has excellent low frequency and broadband absorbing performance, is provided simultaneously with good structural-load-carrying capacity.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of preparation method more particularly to one of electromagnetism stealth composite material
The preparation method of the wideband graphene absorbing material of kind multilayered structure concentration gradient design.
Background technique
Military domain is the weaponry of representative by more using military fighter aircraft with the development of modern radar Detection Techniques
The electromagnetism stealth problem for coming more frequent tracking and detecting, especially low frequency and wideband has become limitation a new generation of China opportunity of combat
In the important technology bottleneck of future battlefield existence and penetration ability.Meanwhile in civil field, the development of telecommunication technology exists
Serious electromagnetic radiation pollution problem is also brought while bringing people's convenient life.Thus, it is possible to which electromagnetic wave energy is turned
Heat energy loss is turned to fall so that the electromagnetic wave absorbent material for significantly reducing reflection of electromagnetic wave is most effective as what is solved the above problems
Solution receives more and more attention.Due to the limitation of practical service environment, ideal electromagnetic wave absorbent material performance is special
Point includes: that effective absorption band is wide, density of material is light, material thickness is thin, mechanical strength is high.Graphene possesses strong dielectric loss,
It is easily modified to adjust electromagnetic parameter, it is easily assembled as a series of feature performance benefits such as three-dimensional structure, becomes the research hotspot of absorbing material.It is existing
There is graphene absorbing material based on modified by magnetic nanoparticles graphene powder and graphene three-dimensional sponge, there are low frequencies to inhale wave
Effect is poor, effectively inhale wave frequency band is narrow, mechanical strength is very poor, without bearing capacity the defects of, it is difficult to meet contemporary aircraft for thunder
Up to the requirement of absorbing material low frequency broadband absorbing and structural bearing and electromagnetic wave absorption function integration.
Summary of the invention
In order to overcome, above-mentioned conventional graphite alkene absorbing material low frequency wave-absorbing effect is poor, effective suction wave frequency band is narrow, mechanical strength
The defects of very poor, without bearing capacity, and it is difficult to meet contemporary aircraft for radar absorbing low frequency broadband absorbing and knot
The deficiencies in the prior art such as structure carrying and the requirement of electromagnetic wave absorption function integration, the present invention provides a kind of multilayered structure concentration
The preparation method of the wideband graphene absorbing material of gradient design.The wideband of multilayered structure concentration gradient design prepared by the present invention
Graphene absorbing material has excellent low frequency and broadband absorbing performance, is provided simultaneously with good structural-load-carrying capacity.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design, includes the following steps:
Step 1: sodium ascorbate is crosslinking agent using graphene oxide aqueous dispersion liquid as raw material, pass through aqueous environment water
Thermal method Chemical self-assembly obtains redox graphene hydrogel, the specific steps are as follows:
Deionized water is added to dilute graphene oxide aqueous dispersion liquid, ultrasonic wave added stirs to obtain dispersion liquid；
Sodium ascorbate powder is added, the dissolution of ultrasonic wave added sodium ascorbate is added in hydrothermal reaction kettle and carries out hydro-thermal, natural cooling obtains
To graphene oxide hydrogel, in which: the concentration of graphene oxide aqueous dispersion liquid is 5~15mg/mL, sodium ascorbate crosslinking
Agent addition metering is 4~8mg/mL, and hydrothermal temperature is 90~120 DEG C, and the reaction time is 8~12h.
Step 2: graphene oxide hydrogel is freeze-dried and the steam reduction of heating environment hydrazine hydrate, porous stone is obtained
Black alkene sponge, in which: condenser temperature is -70 DEG C, -40 DEG C of holding 2h of sample initial temperature in freezing dry process, heating rate 1
℃/h；Hydrazine hydrate usage amount be 5mL/g, heating temperature be 80~100 DEG C, soaking time be 12~for 24 hours.
Step 3: changing the step the concentration of graphene oxide dispersion in one, step 2 is repeated, the stone of different densities is obtained
Black alkene sponge.
Step 4: the graphene sponge of different densities is filled into respectively in the cellular honeycomb hole of periodical aramid fiber, graphite
Alkene filled honeycomb according to graphene sponge concentration sequence from small to large from top to bottom stacked arrangement to the specified number of plies, in which: virtue
The cellular honeycomb hole cell shape of synthetic fibre is regular hexagon, and cell radius is 2~5mm, and monolayer honeycomb is with a thickness of 10mm, honeycomb plane
Having a size of two kinds of specifications of 300mm × 300mm and 600mm × 600mm.
Step 5: honeycomb interlayer uses single layer quartz fibre reinforced resin based composites as articulamentum, in splicing bee
The upper and lower sides of nest are covered each by quartz fibre reinforced resin based composites covering and carbon fiber enhancement resin base composite material covers
Skin finally obtains the wideband graphene absorbing material of multilayered structure concentration gradient design, in which: single layer quartz fibre reinforced resin
Based composites with a thickness of 0.1mm, quartz fibre reinforced resin based composites covering with a thickness of 1mm, fibre reinforced
Polymer matrix composites covering with a thickness of 2mm, the resin matrix of quartz fibre reinforced resin based composites covering is epoxy
Resin or cyanate ester resin, the resin matrix of carbon fiber enhancement resin base composite material covering are epoxy resin.
Compared with the prior art, the present invention has the advantage that
1, three-dimensional grapheme sponge structure has been obtained using the method for hydro-thermal method Chemical self-assembly, by graphene oxide
The Effective Regulation to final graphene sponge density may be implemented in the control of aqueous dispersion liquid material concentration.
2, the method compound using graphene sponge and honeycomb sandwich structure, is prepared for the low frequency with mechanics bearing capacity
The composite material of broadband absorbing ability, can be with by adjusting the laying scheme of fiber in fiber-reinforced resin matrix compound material covering
The effectively mechanical strength of control composite material realizes Wave suction composite material structural bearing and inhales the integrated design of wave energy.
3, compound with other materials, improve low frequency broadband absorbing performance and mechanics bearing capacity.
4, the aramid fiber paper honeycomb filled by various concentration graphene sponge, is passed from top to bottom according to graphene sponge concentration
Increase arrangement, forms multilayer concentration gradient graphene Wave suction composite material, realize low frequency and broadband absorbing effect.
Detailed description of the invention
Fig. 1 is the SEM photograph of graphene sponge prepared by embodiment 1；
Fig. 2 is the wideband graphene Wave suction composite material schematic diagram of three-decker concentration gradient design prepared by embodiment 1；
The wideband graphene Wave suction composite material 0.5 for the three-decker concentration gradient design that Fig. 3 is prepared for embodiment 1~
40GHz reflection of electromagnetic wave rate curve；
Fig. 4 is the wideband graphene Wave suction composite material schematic diagram of four-layer structure concentration gradient design prepared by embodiment 2；
The wideband graphene Wave suction composite material 0.5 for the four-layer structure concentration gradient design that Fig. 5 is prepared for embodiment 2~
40GHz reflection of electromagnetic wave rate curve.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the range of technical solution of the present invention, should all be covered at this
In the protection scope of invention.
Embodiment 1
The wideband graphene absorbing material of multilayered structure concentration gradient design is prepared according to the following steps in the present embodiment:
(1) deionized water is added to be diluted to 5mg/mL graphene oxide aqueous dispersion liquid, ultrasonic wave added stirs
Obtain dispersion liquid；The sodium ascorbate powder of certain mass is added, controls the addition metering of sodium ascorbate powder in dispersion liquid
For 4mg/mL, ultrasonic 5min auxiliary sodium ascorbate dissolution is added in hydrothermal reaction kettle, is heated to 90 DEG C of hydro-thermal reaction 12h, from
So cooling obtains graphene oxide hydrogel.
(2) it takes graphene oxide hydrogel obtained in (1) to be freeze-dried to obtain graphite oxide aerogel sponge, controls
- 70 DEG C of condenser temperature in freezing dry process, sample initial temperature -40 DEG C of holding 2h, 1 DEG C/h of heating rate.
(3) the graphite oxide aerogel sponge sample for arriving (2) is placed in the special stainless steel sealing container of vacuum,
Add a certain amount of 80% hydrazine hydrate solution, control graphene oxide sponge reduction process hydrazine hydrate usage amount is 5mL/g, is heated to 90
DEG C heat preservation 12h, natural cooling obtains graphene sponge (see Fig. 1).
(4) change (1) in graphene oxide aqueous dispersion liquid concentration be 10mg/mL and 15mg/mL, repeat above-mentioned (2) and
(3) process, obtaining three kinds of density is respectively 0.004g/cm3、0.008g/cm3、0.012g/cm3Graphene sponge.
(5) graphene sponge of three kinds of concentration is filled into respectively in aramid fiber paper honeycomb, the aramid paper honeycomb hole trellis
The hexagonal honeycomb that is positive of shape, cell radius are 5mm, and monolayer honeycomb thickness 10mm, honeycomb planar dimension is 600mm × 600mm,
Being subsequently filled honeycomb, lamination is arranged from top to bottom according to the sequence that graphene sponge concentration is 5mg/mL, 10mg/mL and 15mg/mL
Column.
(6) honeycomb interlayer, which uses, enhances cyanate resin base composite material conduct with a thickness of the single layer quartz fibre of 0.1mm
Articulamentum enhances cyanate resin base composite material wave transparent covering splicing cellular upper surface covering 1mm thick fiberglass,
The carbon fiber reinforced epoxy resin-based composite covering for splicing cellular lower surface covering 2mm thickness, finally obtains three-decker
The wideband graphene Wave suction composite material of concentration gradient design (see Fig. 2).
(7) national military standard GJB 2038A-2011 electromagnetic wave absorption material reflectivity arch frame method is used, to three-decker obtained
Wideband graphene Wave suction composite material plate 0.5~40GHz reflection of electromagnetic wave rate of concentration gradient design is tested, 0.5~
40GHz frequency range internal reflection loss lower than -10dB effective absorption band width reach 37.65GHz (0.85~1.5GHz, 3-~
40GHz).Wherein 0.5~3GHz full frequency band reflection loss is lower than -5dB, and reflection loss reaches -21dB, 14.6GHz at 1.16GHz
Place's absorption maximum intensity reaches -42dB (see Fig. 3).In conclusion the wideband graphene of three-decker concentration gradient design inhales wave
Composite material flat plate has excellent low frequency and broadband absorbing performance.
Embodiment 2
The wideband graphene absorbing material of multilayered structure concentration gradient design is prepared according to the following steps in the present embodiment:
(1) deionized water is added to be diluted to 5mg/mL graphene oxide aqueous dispersion liquid, ultrasonic wave added stirs
Obtain dispersion liquid；The sodium ascorbate powder of certain mass is added, controls the addition metering of sodium ascorbate powder in dispersion liquid
For 8mg/mL, ultrasonic 5min auxiliary sodium ascorbate dissolution is added in hydrothermal reaction kettle, is heated to 120 DEG C of hydro-thermal reaction 8h, from
So cooling obtains graphene oxide hydrogel.
(2) it takes graphene oxide hydrogel obtained in (1) to be freeze-dried to obtain graphite oxide aerogel sponge, controls
- 70 DEG C of condenser temperature in freezing dry process, sample initial temperature -40 DEG C of holding 2h, 1 DEG C/h of heating rate.
(3) the graphite oxide aerogel sponge sample for arriving (2) is placed in the special stainless steel sealing container of vacuum,
Add a certain amount of 80% hydrazine hydrate solution, control graphene oxide sponge reduction process hydrazine hydrate usage amount is 5mL/g, is heated to 95
DEG C heat preservation for 24 hours, natural cooling obtains graphene sponge.
(4) change (1) in graphene oxide aqueous dispersion liquid concentration be 10mg/mL and 15mg/mL, repeat above-mentioned (2) and
(3) process, obtaining three kinds of density is respectively 0.004g/cm3、0.008g/cm3、0.012g/cm3Graphene sponge.
(5) graphene sponge of three kinds of concentration is filled into respectively in aramid fiber paper honeycomb, the aramid paper honeycomb hole trellis
The hexagonal honeycomb that is positive of shape, cell radius are 2mm, and monolayer honeycomb thickness 10mm, honeycomb planar dimension is 600mm × 600mm,
Be subsequently filled honeycomb according to graphene sponge concentration be 5mg/mL, 5mg/mL, 10mg/mL and 15mg/mL sequence from top to bottom
Stacked arrangement.
(6) honeycomb interlayer, which uses, enhances cyanate resin base composite material conduct with a thickness of the single layer quartz fibre of 0.1mm
Articulamentum is splicing cellular upper surface covering 1mm thick fiberglass reinforced epoxy or cyanate resin base composite material
Wave transparent covering, it is final to obtain in the carbon fiber reinforced epoxy resin-based composite covering for splicing cellular lower surface covering 2mm thickness
The wideband graphene Wave suction composite material designed to four-layer structure concentration gradient (see Fig. 4).
(7) national military standard GJB 2038A-2011 electromagnetic wave absorption material reflectivity arch frame method is used, to four-layer structure obtained
Wideband graphene Wave suction composite material plate 0.5~40GHz reflection of electromagnetic wave rate of concentration gradient design is tested, 0.5~
40GHz frequency range internal reflection loss lower than -10dB effective absorption band width reach 37.5GHz (0.5~1GHz, 3~
40GHz)；Effective absorption band width of the reflection loss lower than -20dB reaches 36.3GHz (3.7~40GHz).Wherein 0.5~
3GHz full frequency band reflection loss is lower than -5dB, and reflection loss reaches -27dB at 0.69GHz, and absorption maximum intensity reaches at 23GHz
To -62dB (see Fig. 5).In conclusion the wideband graphene Wave suction composite material plate of four-layer structure concentration gradient design has
Excellent low frequency and broadband absorbing performance.
Claims (9)
1. a kind of preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design, it is characterised in that the side
Method includes the following steps:
Step 1: sodium ascorbate is crosslinking agent using graphene oxide aqueous dispersion liquid as raw material, pass through aqueous environment hydro-thermal method
Chemical self-assembly obtains redox graphene hydrogel；
Step 2: graphene oxide hydrogel is freeze-dried and the steam reduction of heating environment hydrazine hydrate, porous graphene is obtained
Sponge；
Step 3: changing the step the concentration of graphene oxide dispersion in one, step 2 is repeated, the graphene of different densities is obtained
Sponge；
Step 4: the graphene sponge of different densities is filled into respectively in the cellular honeycomb hole of periodical aramid fiber, graphene is filled out
Fill honeycomb according to graphene sponge concentration sequence from small to large from top to bottom stacked arrangement to the specified number of plies；
Step 5: honeycomb interlayer uses single layer quartz fibre reinforced resin based composites as articulamentum, it is cellular splicing
Upper and lower sides are covered each by quartz fibre reinforced resin based composites covering and carbon fiber enhancement resin base composite material covering, most
The wideband graphene absorbing material of multilayered structure concentration gradient design is obtained eventually.
2. the preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1,
It is characterized in that specific step is as follows for the step 1: adding deionized water to dilute graphene oxide aqueous dispersion liquid, ultrasound
Auxiliary stirs to obtain dispersion liquid；Sodium ascorbate powder is added, hydro-thermal is added in the dissolution of ultrasonic wave added sodium ascorbate
Hydro-thermal is carried out in reaction kettle, natural cooling obtains graphene oxide hydrogel.
3. the preparation side of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1 or 2
Method, it is characterised in that the concentration of the graphene oxide aqueous dispersion liquid is 5~15mg/mL, the addition of sodium ascorbate crosslinking agent
Metering is 4~8mg/mL, and hydrothermal temperature is 90~120 DEG C, and the reaction time is 8~12h.
4. the preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1,
It is characterized in that condenser temperature is -70 DEG C, -40 DEG C of holding 2h of sample initial temperature in freezing dry process in the step 2,
1 DEG C/h of heating rate.
5. the preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1,
It is characterized in that in the step 2, hydrazine hydrate usage amount is 5mL/g, and heating temperature is 80~100 DEG C, soaking time is 12~
24h。
6. the preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1,
It is characterized in that the cellular honeycomb hole cell shape of aramid fiber is regular hexagon, and cell radius is 2~5mm, single in the step 4
Layer honeycomb is with a thickness of 10mm.
7. the preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1,
It is characterized in that honeycomb planar dimension is 300mm × 300mm or 600mm × 600mm in the step 4.
8. the preparation method of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1,
It is characterized in that in the step 5, single layer quartz fibre reinforced resin based composites with a thickness of 0.1mm, quartz fibre increases
Strong polymer matrix composites covering with a thickness of 1mm, carbon fiber enhancement resin base composite material covering with a thickness of 2mm.
9. the preparation side of the wideband graphene absorbing material of multilayered structure concentration gradient design according to claim 1 or 8
Method, it is characterised in that the resin matrix of the quartz fibre reinforced resin based composites covering is epoxy resin or cyanate resin
Rouge, the resin matrix of carbon fiber enhancement resin base composite material covering are epoxy resin.
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