CN105255446B - The compound microwave absorbing material of a kind of redox graphene and nano-cerium oxide and preparation method - Google Patents
The compound microwave absorbing material of a kind of redox graphene and nano-cerium oxide and preparation method Download PDFInfo
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Abstract
Present invention relates particularly to the compound microwave absorbing material of a kind of redox graphene and nano-cerium oxide and preparation method, and graphene oxide is prepared with improved Hummers methods, by graphene oxide water solution and cerous nitrate in mass ratio 1:25 mixing, while it is 10 to adjust pH, using one step hydro thermal method, is reduced graphene oxide while nano-cerium oxide is generated, the compound microwave absorbing material of obtained redox graphene and nano-cerium oxide.Using the microwave absorption parameter of vector network analyzer test compound material, it is lost by the microwave reflection of the coaxial line theoretical calculation composite of classics.As a result show, the compound microwave absorbing material of redox graphene/nano-cerium oxide has excellent microwave absorbing property, and absorption intensity is high, and absorption band is wide, and compared with nano-cerium oxide, absorbing property increases substantially.Therefore, the present invention is had broad application prospects, and the commercial Application and national defense construction for expanding rare earth oxide are extremely important.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of microwave absorbing material and preparation method.
Background technology
With the development of military stealth technology and civilian electromagnetism interference technology, microwave absorbing material（Referred to as inhale ripple material
Material）Turn into study hotspot, such material is increasingly becoming an important branch of application function material.Absorbing material refers to energy
Absorb, the electromagnetic wave that decay is incident, and its electromagnetic energy is converted into the energy of heat energy or other forms and dissipated, or make electromagnetism
A kind of material that ripple disappears by interference.
Traditional absorbing material, such as the major defect of ferrite, graphite, ceramic-like materials is that density is big, absorption band is narrow
And absorption intensity is not enough etc., thus can not meet the requirement of absorbing material " thin, light, wide, strong ".In recent years, nano combined material
Expect that the application in terms of microwave absorption turns into study hotspot, quantum size effect, macroscopic quantum tunnel specific to nano material
Channel effect and interfacial effect change the physical properties such as the electricity of material, magnetic, while with good absorbing property, have both
The features such as broadband, compatibility are good, light weight, thickness of thin, is a kind of extremely promising stealth material.
Carbon-based material is widely used in electromagnetic shielding and absorbing material field always.As the representative of new carbon, stone
For black alkene since appearance, its unique mechanics, electricity, optics and magnetic performance are always the focus of field of functional materials concern.
The special two-dimensional sheet single layer of carbon atom honeycomb that graphene has impart its high-specific surface area, high electron mobility and
The advantages that high strength.Compared with traditional material, graphene composite material can relatively easily meet the characteristics of impedance matching,
Reach requirement of the absorbing material to " thin, light, wide, strong ".
Cerium oxide（CeO2）It is widest rare-earth oxide in a kind of commercial Application, its molecular formula is CeO2, point
Son amount is 172.12, is existed in nature with fluorite type structure.CeO2 Nano material is in luminescent device, purifying vehicle exhaust
Catalysis, solid-oxide fuel battery electrolyte and new uvioresistant absorption aspects have important commercial Application.
In CeO2Crystals, due to the presence of oxygen defect, generally there is middle valence state, i.e. Ce in Ce ions4+With Ce3+,
Under certain condition, Ce4+With Ce3+Mutually conversion easily occurs, so that CeO2Substantial amounts of Lacking oxygen is internally formed, therefore,
Fluorite type CeO2Oxygen ability is stored with extremely strong.It is special that numerous commercial Applications of cerium oxide benefit from its all the time
Lacking oxygen effect.
The substantial amounts of Lacking oxygen defect of crystals, along with high concentration+trivalent cerium ion, CeO can be improved2Electrical conductance
Can, conduction loss can be produced under extraneous electromagnetic wave influence, electromagnetic wave of decaying；Meanwhile the formation of Lacking oxygen produces in lattice
A large amount of free electrons, charge polarization can be aggravated, can also strengthen its microwave absorbing property.
Graphene-based cerium oxide nano composite is prepared, plays excellent carrier effect and the CeO of graphene2It is special
Lacking oxygen effect, CeO can be improved2The microwave absorbing property of nano composite material.
The content of the invention
In order to expand application of the nanometer rare earth oxide material in field of microwave absorption, the present invention provides a kind of reduction-oxidation
Graphene（RGO）And nano-cerium oxide（CeO2）Compound microwave absorbing material and preparation method.
The compound microwave absorbing material of a kind of redox graphene and nano-cerium oxide is prepared with improved Hummers methods
Graphite oxide, by graphene oxide solution and six nitric hydrate ceriums in mass ratio 1:25 mixing, regulation pH value is 10, using a step
Hydro-thermal method, graphene oxide is reduced while nano-cerium oxide is generated, redox graphene and nano-cerium oxide is made
Composite microwave absorbing material；
The characteristics of compound microwave absorbing material is：Uniform load nanometer on the surface of reduction-oxidation graphite flakes
Cerium oxide particle, it is separated from each other between adjacent scale, in stratiform sandwich structure, contributes to the raising of microwave absorbing property；
The nano-cerium oxide（CeO2）Nano particle average-size be 15 nm, there is prominent quantum size effect
And excellent Lacking oxygen effect；
Redox graphene in the compound microwave absorbing material（RGO）And nano-cerium oxide（CeO2）Weight ratio
For 1:10；
It is at 4.3~17 GHz in frequency when compound microwave absorbing material is 1.5~2.0mm of thickness coating
Reflection loss is -32~-10dB；Electro-magnetic wave absorption is up to more than 90%.
It is specific to prepare redox graphene and the operating procedure of the compound microwave absorbing material of nano-cerium oxide is as follows：
（1）The preparation of graphite oxide
Graphite oxide is prepared using improved Hummers methods, takes 3g graphite powders and 2g sodium nitrate（NaNO3）It is added to
In 250mL beaker, along wall of cup be slowly added to 70 mL concentration be 95 ~ 98% the concentrated sulfuric acid and stir；In condition of ice bath
Under, point 5 10 g potassium permanganate of addition（KMnO4）, each addition is 2g, stirs a hour；Stirred in 35 C water-baths
2h is mixed, obtains mixed solution；140 mL deionized waters are slowly added into mixed solution and stir 15 min, now system liter
The hydrogen peroxide that concentration is 30% is added dropwise to 88~92 C in temperature（H2O2）Until reaction solution is changed into glassy yellow；By reaction solution mistake while hot
Filter, and with 1:10 dilute hydrochloric acid solution washing, removes unnecessary metal ion；Washing is until pH by high speed centrifugation and repeatedly
It is worth for 7；48h is freeze-dried, obtains graphite oxide；
（2）The preparation of redox graphene and the compound microwave absorbing material of nano-cerium oxide
Take 20 mg graphite oxides to be dissolved in 60 mL deionized water, ultrasonic disperse 1h, the oxidation of 60mL brown colors is made
Graphene solution；Take the nitric hydrate ceriums of 0.5g six（Ce(NO3)3·6H2O）It is added in 60mL graphene oxide solution, magnetic force
Stirring；Treat that six nitric hydrate ceriums are completely dissolved, it is 25 ~ 28% ammonia that 3 mL concentration slowly, which are added dropwise, into reaction solution under ultrasonication
The aqueous solution, now the pH value of reaction solution is 9~11；Reaction solution is transferred in hydrothermal reaction kettle, 180˚Hydro-thermal reaction 24h under C；
Centrifugation, washing, ethanol washing purification process；24 h are dried in vacuo under 60 C, obtain redox graphene and nano oxidized
Cerium（RGO/CeO2）Compound microwave absorbing material.
The microwave absorbing material that the redox graphene and nano-cerium oxide of the present invention are compound can be used as excellent microwave
Absorbent, its microwave absorbing property parameter are obtained by following detection means：
The compound microwave absorbing material of redox graphene and nano-cerium oxide is mixed with paraffin（Composite microwave absorbs
The volume fraction of material accounts for 30%）, under 80 C insulation half an hour make paraffin melting, stir, be put into mould, pressed in 2 Mpa
The coaxial annulus that internal diameter is 3.04 mm, external diameter is 7.00 mm is made under power, and its thickness is polished into 2 mm, is placed in coaxial line
Tested in fixture, obtain real part of permittivity, imaginary part of dielectric constant, pass through the microwave of the coaxial line theoretical calculation present invention of classics
The reflection loss of absorbing material.
RGO and nano Ce O2The microwave absorbing property of compound microwave absorbing material is by AV3629D (groups of China Electronics
41st research institute) vector network analyzer test, using the mm of the length 99.898 coaxial wire holders of APC7, calibrating device is
AV31101.Test frequency range is 2-18 GHz, and test sample is that the thickness that composite microwave absorbing material mixes composition with paraffin is 2
Mm coaxial annulus, drawn by fitting in the reflection loss that thickness is microwave absorbing material of the invention in the range of 1-5 mm.
RGO and nano Ce O2The crystal phase structure of compound microwave absorbing material is by X-ray diffraction（XRD）Confirm（See Fig. 1）.
XRD results show that composite is typical cubic fluorite structure, its crystalline phase ownership and CeO2Unanimously, using Debye-
Scherrer formula are to it（111）Crystal face is calculated, and it is 15 nm to draw nanocrystalline grain size.In the XRD spectrum of material simultaneously
There is not the characteristic peak of graphene oxide, illustrate to pass through hydro-thermal process, graphene oxide is effectively reduced, generation reduction
Graphene oxide（RGO）.
RGO and nano Ce O2The microstructure of compound microwave absorbing material is by transmission electron microscope（TEM）Observation（See
Fig. 2）.CeO2Nano-particle is uniformly dispersed on monolithic redox graphene, in hexagonal pattern.Particle sizing result is shown
CeO2Nano-particle average-size is 15nm, and this result is consistent with XRD results.
RGO and nano Ce O2Compound microwave absorbing material has efficient microwave absorbing property（See Fig. 3）.Sample coatings
Thickness（d）For 1.5 mm when, be that optimal reflection loss is obtained at 17GHz is -32 dB in frequency.When coating layer thickness is 2.0 mm
When, reflection loss is less than -10 dB（Electro-magnetic wave absorption is up to more than 90%）Frequency bandwidth be 4.3 GHz.With nano-cerium oxide phase
Than this composite has high microwave absorption intensity and wide absorption band（See Fig. 4）.
RGO and nano Ce O2Compound microwave absorbing material uses graphene oxide to be primarily due to aoxidize for presoma
Graphenic surface carries substantial amounts of oxygen-containing functional group, such as hydroxyl, carboxyl, epoxy radicals etc., these functional groups can be regarded as reacting
Active site, when adding cerium ion, electrostatic attraction effect can make cerium ion absorption contribute to crystal equal on graphene oxide sheet
Even nucleation.Graphene oxide can be reduced in water-heat process, and most of oxygen-containing functional group disappears, at this moment redox graphene with
CeO2Between can have Van der Waals force, make CeO2Closely it is immobilized on redox graphene piece.
In RGO and nano Ce O2In the preparation process of compound microwave absorbing material, when precipitating reagent ammoniacal liquor is added dropwise, it is aided with super
Sound acts on, it is therefore an objective to improves CeO2Dispersiveness of the nano-particle on graphene oxide sheet.At crystal nucleation initial stage, ultrasonication
Environment of crystal growth can be improved, improve the decentralization of nucleus, so that nano particle reaches dispersed degree, so
It is favorably improved the microwave absorbing property of material.
The advantageous effects of the present invention embody in the following areas：
1. the compound microwave absorbing material of the redox graphene and nano-cerium oxide of the present invention, makes full use of graphene
With high electron mobility, the characteristics of bigger serface, while the significant Lacking oxygen effect of nano-cerium oxide is taken into account, so as to obtain
Absorbing property excellent cerium oxide nano composite, compared with nano-cerium oxide, this compound microwave absorbing material it is excellent
Gesture is that microwave absorption is strong, absorption band is wide, and optimal microwave reflection loss is -32dB, when coating layer thickness is 2.0mm, reflection
Loss is less than -10dB（Electro-magnetic wave absorption is up to more than 90%）Frequency bandwidth be 4.3GHz.
2. in hydro-thermal presoma process for preparation, aided in using ultrasonic field, by ultrasonic radiation be effectively improved it is nanocrystalline into
Nuclear environment, the heap that graphene sheet layer is also prevented while improving nano-particle in the dispersiveness on graphene carrier
It is folded.
3. the preparation technology of the present invention is simple, cost is low, and security is good, and reducing agent and surface need not be added in building-up process
Activating agent, it is environmentally friendly.The present invention has wide development and application prospect, to expanding the micro- of cerium oxide nano composite
Ripple absorption application has and its important meaning.
Brief description of the drawings
Fig. 1 is the XRD spectrum of redox graphene/cerium oxide nano composite of the present invention.
Fig. 2 is the TEM photos of redox graphene/cerium oxide nano composite of the present invention.
Fig. 3 is that collection of illustrative plates is lost in the reflection of electromagnetic wave of redox graphene/cerium oxide nano composite of the present invention.
Fig. 4 is electricity of the redox graphene/cerium oxide nano composite with pure zirconia cerium nano-particle of the present invention
Magnetic wave reflection loss contrasts collection of illustrative plates（Sample coatings thickness is 2.0 mm）.
Embodiment
With reference to embodiment, the present invention is further described.
Raw materials used and source is as follows：
（1）Natural graphite scale：325 mesh, purity >=99%, Qingdao Hua Tai permanent seals Co., Ltd
（2）Potassium permanganate：Purity AR, Chemical Reagent Co., Ltd., Sinopharm Group
（3）Hydrogen peroxide：Purity AR, Chemical Reagent Co., Ltd., Sinopharm Group
（4）The concentrated sulfuric acid：Purity 95-98%, Tianjin Bo Di Chemical Co., Ltd.s
（5）Concentrated phosphoric acid：Purity >=85%, Tianjin Bo Di Chemical Co., Ltd.s
（6）Hydrochloric acid：Purity 36-38%, Tianjin Bo Di Chemical Co., Ltd.s
（7）Ammoniacal liquor：Purity 25%, Chemical Reagent Co., Ltd., Sinopharm Group
（8）Six nitric hydrate ceriums：Purity AR, Aladdin reagent
（9）Ethanol：Purity AR, Chemical Reagent Co., Ltd., Sinopharm Group.
The concrete operation step for preparing redox graphene and the compound microwave absorbing material of nano-cerium oxide is as follows：
（1）The preparation of graphite oxide
Graphite oxide is prepared using improved Hummers methods, takes 3g graphite powders and 2g sodium nitrate（NaNO3）It is added to
In 250mL beaker, along wall of cup be slowly added to 70mL concentration be 95 ~ 98% the concentrated sulfuric acid and stir.In condition of ice bath
Under, by 10 g potassium permanganate（KMnO4）5 parts are divided into, point 5 additions, is spaced 10 minutes and adds once, stir a hour.
Ice-water bath is removed afterwards, in 35 C stirred in water bath 2h.After stirring terminates, it is molten that 140 mL deionized waters are slowly added into mixing
In liquid and 15min is stirred, now system is warming up to 90 C or so, and the hydrogen peroxide that concentration is 30% is then added dropwise（H2O2）It is until anti-
Liquid is answered to be changed into glassy yellow.After reaction terminates, reaction solution is filtered while hot, and with 1:10 watery hydrochloric acid（By 500 mL deionization
Water configures with the concentrated hydrochloric acid that 50mL concentration is 36 ~ 38%）Washing, removes unnecessary metal ion.Product is by high speed centrifugation and instead
Rehydration is washed until pH is 7.Product is finally freeze-dried 48 h, obtains graphite oxide.
（2）The preparation of redox graphene and the compound microwave absorbing material of nano-cerium oxide
20 mg graphite oxides are taken to be dissolved in 60mL deionized water, ultrasonic disperse 1h, ultrasonic radiation power is 180 W, system
Obtain the graphene oxide solution of 60mL brown colors.Weigh the nitric hydrate ceriums of 0.5g six（Ce(NO3)3·6H2O）It is added to 60mL's
In graphene oxide solution, magnetic agitation.Treat that six nitric hydrate ceriums are completely dissolved, slowly dripped under ultrasonication into reaction solution
It is 25 ~ 28% ammonia spirits to add 3mL concentration, and now the pH value of reaction solution is 10 or so, and ultrasonic radiation power is 180W, at ultrasound
The reason time is 30min.Reaction solution is transferred in 100mL hydrothermal reaction kettle, 180˚Hydro-thermal reaction 24h under C.Reaction terminates
Afterwards, product through centrifuging, washing, the purification process such as ethanol washing.24h finally is dried in vacuo under 60 C, obtains oxygen reduction fossil
The compound microwave absorbing material of black alkene and nano-cerium oxide.
Redox graphene and the compound microwave absorbing material of nano-cerium oxide can be used as excellent microwave absorption, its
Microwave absorbing property parameter is obtained by following detection means：
The compound microwave absorbing material of redox graphene and nano-cerium oxide is mixed with paraffin（Composite microwave absorbs
The volume fraction of material accounts for 30%）, under 80 C insulation half an hour make paraffin melting, stir, be put into mould, pressed in 2 Mpa
It is 3.04 mm that internal diameter is made under power, and external diameter is 7.00 mm coaxial annulus, and its thickness is polished into 2 mm, is placed in coaxial line
Tested in fixture, obtain real part of permittivity, imaginary part of dielectric constant, pass through the anti-of classical coaxial line theoretical calculation composite
Penetrate loss.
After tested, pure zirconia cerium nano particle does not almost have microwave absorbing property.And the redox graphene of the present invention
But there is excellent microwave absorbing property with the compound microwave absorbing material of nano-cerium oxide, when prepares coating thickness be 1.5~
During 4.0mm, redox graphene and the compound microwave absorbing material of nano-cerium oxide are anti-at 4.3~17GHz in frequency
It is -32~-10dB to penetrate loss（Electro-magnetic wave absorption is up to more than 90%）；Microwave reflection loss reaches maximum at 17GHz, for-
32dB；When coating layer thickness is 2.0mm, reflection loss is less than -10dB（Electro-magnetic wave absorption is up to more than 90%）Frequency bandwidth be
4.3 GHz。
Claims (1)
1. a kind of redox graphene and the compound microwave absorbing material of nano-cerium oxide, it is characterised in that：With improved
Hummers methods prepare graphite oxide, by graphene oxide solution and six nitric hydrate ceriums in mass ratio 1:25 mixing, adjust pH value
For 10, using one step hydro thermal method, graphene oxide is reduced while nano-cerium oxide is generated, redox graphene is made
With the composite microwave absorbing material of nano-cerium oxide；Concrete operation step is as follows：
（1）Graphite oxide is prepared using improved Hummers methods
3g graphite powders and 2g sodium nitrate is taken to be added in 250mL beaker, it is 95 ~ 98% to be slowly added to 70mL concentration along wall of cup
The concentrated sulfuric acid simultaneously stirs；Under condition of ice bath, point 5 addition 10g potassium permanganate, each addition is 2g, stirs one
Hour；In 35 C stirred in water bath 2h, mixed solution is obtained；140mL deionized waters are slowly added into mixed solution and stirred
15min is mixed, now system is warming up to 88~92 C, and the hydrogen peroxide that dropwise addition concentration is 30% is until reaction solution is changed into glassy yellow；Will
Reaction solution filters while hot, and with 1:10 dilute hydrochloric acid solution washing, removes unnecessary metal ion；By high speed centrifugation and repeatedly
Washing is until pH value is 7；48h is freeze-dried, obtains graphite oxide；
（2）The preparation of redox graphene and the compound microwave absorbing material of nano-cerium oxide
20mg graphite oxides are taken to be dissolved in 60mL deionized water, ultrasonic disperse 1h, the graphene oxide of obtained 60mL brown colors
Solution；The nitric hydrate ceriums of 0.5g six are taken to be added in 60mL graphene oxide solution, magnetic agitation；Treat that six nitric hydrate ceriums are complete
Fully dissolved, the pH value of the ammonia spirit, now reaction solution of 3mL concentration 25 ~ 28% is slowly added dropwise into reaction solution under ultrasonication
For 9~11；In hydro-thermal presoma process for preparation, ultrasonic radiation power is 180 W；Reaction solution is transferred in hydrothermal reaction kettle,
180˚Hydro-thermal reaction 24h under C；Centrifugation, washing, ethanol washing purification process；24h is dried in vacuo under 60 C, obtains oxygen reduction
Graphite alkene and the compound microwave absorbing material of nano-cerium oxide；
The characteristics of composite microwave absorbing material is：Uniform load nano-cerium oxide on the surface of reduction-oxidation graphite flakes
Particle, it is separated from each other between adjacent scale, in stratiform sandwich structure, contributes to the raising of microwave absorbing property；
The nano particle average-size of the nano-cerium oxide is 15nm, has prominent quantum size effect and excellent oxygen
Room effect；
The weight of redox graphene and nano-cerium oxide ratio is 1 in the composite microwave absorbing material:10；
It is the reflection loss at 4.3~17GHz in frequency when composite microwave absorbing material is 1.5~4.0mm of thickness coating
For -32~-10dB；Electro-magnetic wave absorption is up to more than 90%.
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| CN102199341B (en) * | 2011-04-07 | 2012-09-19 | 上海交通大学 | Preparation method of microwave absorbing material |
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| CN104209531B (en) * | 2013-05-31 | 2016-08-17 | 北京化工大学 | A kind of cobalt/Graphene composite nano wave-absorbing material and preparation method thereof |
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