CN105255446A - Reduced graphene oxide and nano cerium oxide composite microwave absorbing material and preparation method thereof - Google Patents
Reduced graphene oxide and nano cerium oxide composite microwave absorbing material and preparation method thereof Download PDFInfo
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- CN105255446A CN105255446A CN201510751438.8A CN201510751438A CN105255446A CN 105255446 A CN105255446 A CN 105255446A CN 201510751438 A CN201510751438 A CN 201510751438A CN 105255446 A CN105255446 A CN 105255446A
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Abstract
The invention specifically relates to a reduced graphene oxide and nano cerium oxide composite microwave absorbing material and a preparation method thereof. The method comprises the following steps: preparing graphene oxide by using an improved Hummers method; mixing a graphene oxide aqueous solution with cerium nitrate in a mass ratio of 1:25, and adjusting the pH value to 10; and by using a one-step hydrothermal method, simultaneously generating nano cerium oxide and reducing the graphene oxide, so that a reduced graphene oxide and nano cerium oxide composite microwave absorbing material is obtained. The microwave absorption parameters of the composite material are tested by using a vector network analyzer, and the microwave reflection loss of the composite material is calculated by using a classical coaxial line theory. Results show that the reduced graphene oxide and nano cerium oxide composite microwave absorbing material has excellent microwave absorbing properties, high absorption strength and wide absorption band, and compared with nano cerium oxide, the microwave absorbing properties are greatly improved. Thus, the reduced graphene oxide and nano cerium oxide composite microwave absorbing material disclosed by the invention has broad application prospects, and is of great significance to the expansion of industrial application of rare earth oxides and the national defense construction.
Description
Technical field
The invention belongs to technical field of function materials, be specifically related to a kind of microwave absorbing material and preparation method.
Background technology
Along with the development of military stealthy technique and civilian electromagnetism interference technology, microwave absorbing material (abbreviation absorbing material) becomes study hotspot, and such material becomes an important branch of application function material gradually.Absorbing material refer to can absorb, the hertzian wave of attenuate incident, and convert its electromagnetic energy the energy of heat energy or other form to and dissipate, or the class material that hertzian wave is disappeared because of interference.
Tradition absorbing material, the such as main drawback of ferrite, graphite, ceramic-like materials be that density is large, absorption band is narrow and absorption intensity inadequate etc., thus can not meet the requirement of absorbing material " thin, light, wide, strong ".In recent years, the application of nano composite material in microwave absorbing becomes study hotspot, quantum size effect, macro quanta tunnel effect and interfacial effect specific to nano material change the physical properties such as electricity, magnetic of material, while there is good absorbing property, having had both the features such as broadband, compatibility is good, quality is light, thickness is thin, is a kind of extremely rising stealth material.
Carbonaceous material is widely used in electromagnetic shielding and absorbing material field always.As the representative of new carbon, Graphene is since appearance, and the mechanics of its uniqueness, electricity, optics and magnetic performance are the focuses that field of functional materials is paid close attention to always.The special two-dimensional sheet monolayer carbon atom honeycomb structure that Graphene has imparts the advantages such as its high-specific surface area, high electron mobility and high strength.Compared with traditional material, graphene composite material can meet the feature of impedance matching relatively easily, reaches the requirement of absorbing material to " thin, light, wide, strong ".
Cerium oxide (CeO
2) be rare-earth oxide the most widely in a kind of industrial application, its molecular formula is CeO
2, molecular weight is 172.12, exists with fluorite type structure at occurring in nature.CeO
2nano material has important industrial application in luminescent device, purifying vehicle exhaust catalysis, solid-oxide fuel battery electrolyte and novel uvioresistant absorption.
At CeO
2crystals, due to the existence of oxygen defect, there is middle valence state in Ce ion, i.e. Ce usually
4+with Ce
3+, under certain condition, Ce
4+with Ce
3+very easily there is conversion mutually, thus make CeO
2the Lacking oxygen that inner formation is a large amount of, therefore, fluorite type CeO
2have and extremely strong store oxygen ability.Numerous industrial application of cerium oxide all have benefited from its special Lacking oxygen effect all the time.
The Lacking oxygen defect that crystals is a large amount of, along with+3 valency cerium ions of high density, can improve CeO
2conductivity, can conduction loss be produced under extraneous electromagnetic wave influence, attenuates electromagnetic waves; Meanwhile, being formed in lattice of Lacking oxygen produces a large amount of unbound electron, can aggravate charge polarization, also can strengthen its microwave absorbing property.
Prepare graphene-based cerium oxide nano matrix material, play excellent carrier effect and the CeO of Graphene
2special Lacking oxygen effect, can improve CeO
2the microwave absorbing property of nano composite material.
Summary of the invention
In order to expand the application of nanometer rare earth oxide material in field of microwave absorption, the invention provides a kind of redox graphene (RGO) and nano-cerium oxide (CeO
2) microwave absorbing material of compound and preparation method.
The microwave absorbing material of a kind of redox graphene and nano-cerium oxide compound with the Hummers legal system improved for graphite oxide, by graphene oxide solution and six nitric hydrate ceriums in mass ratio 1:25 mix, adjust ph is 10, adopt one step hydro thermal method, while generation nano-cerium oxide, graphene oxide is reduced, the composite microwave absorbing material of obtained redox graphene and nano-cerium oxide;
The feature of the microwave absorbing material of described compound is: on the surface of reduction-oxidation graphite flakes, uniform loading ceria nanoparticles, is separated from each other between adjacent scale, in stratiform sandwich structure, contributes to the raising of microwave absorbing property;
Described nano-cerium oxide (CeO
2) nano particle mean sizes be 15nm, there is the Lacking oxygen effect of outstanding quantum size effect and excellence;
Redox graphene (RGO) and nano-cerium oxide (CeO in the microwave absorbing material of described compound
2) weight ratio be 1:10;
When the microwave absorbing material of compound is the coating of thickness 1.5 ~ 2.0mm, the reflection loss being 4.3 ~ 17GHz place in frequency is-32 ~-10dB; Absorption of electromagnetic wave reaches more than 90%.
The operation steps specifically preparing the microwave absorbing material of redox graphene and nano-cerium oxide compound is as follows:
(1) preparation of graphite oxide
Adopt the Hummers legal system improved for graphite oxide, get 3g Graphite Powder 99 and 2g SODIUMNITRATE (NaNO
3) join in the beaker of 250mL, slowly add 70mL concentration along wall of cup and be the vitriol oil of 95 ~ 98% and stir; Under condition of ice bath, divide and add 10g potassium permanganate (KMnO for 5 times
4), each add-on is 2g, stirs one hour; At 35 C stirred in water bath 2h, obtain mixing solutions; Slowly being joined by 140mL deionized water in mixing solutions and to stir 15min, now system is warming up to 88 ~ 92 C, drips the hydrogen peroxide (H that concentration is 30%
2o
2) until reaction solution becomes glassy yellow; Reacting liquor while hot is filtered, and washs with the dilute hydrochloric acid solution of 1:10, remove unnecessary metal ion; By high speed centrifugation and repeatedly washing until pH value is 7; Lyophilize 48h, obtains graphite oxide;
(2) preparation of the microwave absorbing material of redox graphene and nano-cerium oxide compound
Getting 20mg graphite oxide is dissolved in the deionized water of 60mL, ultrasonic disperse 1h, the graphene oxide solution of obtained 60mL brown color; Get 0.5g six nitric hydrate cerium (Ce (NO
3)
36H
2o) join in the graphene oxide solution of 60mL, magnetic agitation; Treat that six nitric hydrate ceriums dissolve completely, under ultrasonication, slowly in reaction solution, drip 3mL concentration is 25 ~ 28% ammonia solns, and 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; Centrifugal, washing, washing with alcohol purification process; Vacuum-drying 24h under 60 C, obtains redox graphene and nano-cerium oxide (RGO/CeO
2) microwave absorbing material of compound.
The microwave absorbing material of redox graphene of the present invention and nano-cerium oxide compound can as excellent microwave absorption, and its microwave absorbing property parameter is obtained by following detection means:
The microwave absorbing material of redox graphene and nano-cerium oxide compound is mixed with paraffin (volume fraction of composite microwave absorbing material accounts for 30%), be incubated half an hour under 80 C and make paraffin melting, stir, be put in mould, the coaxial annulus that internal diameter is 3.04mm, external diameter is 7.00mm is made under 2Mpa pressure, and its thickness is polished into 2mm, be placed in coaxial line fixture build-in test, obtain real part of permittivity, imaginary part of dielectric constant, by the reflection loss of the coaxial line Theoretical Calculation microwave absorbing material of the present invention of classics.
RGO and nano Ce O
2the microwave absorbing property of the microwave absorbing material of compound is tested by AV3629D (institute of group of China Electronics the 41st) vector network analyzer, and adopt the APC7 coaxial line fixture of length 99.898mm, calibrating device is AV31101.Test frequency range is 2-18GHz, and test sample is the coaxial annulus that composite microwave absorbing material mixes that with paraffin the thickness formed is 2mm, is drawn at thickness to be the reflection loss of microwave absorbing material of the present invention within the scope of 1-5mm by matching.
RGO and nano Ce O
2the crystal phase structure of the microwave absorbing material of compound confirms (see figure 1) by X-ray diffraction (XRD).XRD result shows that matrix material is typical cubic fluorite structure, its crystalline phase ownership and CeO
2unanimously, adopt Debye-Scherrer formula to calculate its (111) crystal face, show that nanocrystalline grain size is 15nm.Do not occur the characteristic peak of graphene oxide in the XRD figure spectrum of material, illustrate through hydrothermal treatment consists, graphene oxide is effectively reduced, and generates redox graphene (RGO).
RGO and nano Ce O
2the microtexture of the microwave absorbing material of compound observes (see figure 2) by transmission electron microscope (TEM).CeO
2nanoparticle is dispersed on monolithic redox graphene uniformly, in hexagonal pattern.Particle sizing result display CeO
2nanoparticle mean sizes is 15nm, and this result is consistent with XRD result.
RGO and nano Ce O
2the microwave absorbing material of compound has efficient microwave absorbing property (see figure 3).Sample coatings thickness (
d) for 1.5mm time, be that to obtain best reflection loss be-32dB at 17GHz place in frequency.When coat-thickness is 2.0mm, reflection loss reaches more than 90% lower than-10dB(absorption of electromagnetic wave) frequency span be 4.3GHz.Compared with nano-cerium oxide, this matrix material has high microwave absorbing intensity and wide absorption band (see figure 4).
RGO and nano Ce O
2the microwave absorbing material of compound adopts graphene oxide to be presoma, mainly because surface of graphene oxide is with a large amount of oxygen-containing functional groups, such as hydroxyl, carboxyl, epoxy group(ing) etc., these functional groups can regard as reactive behavior point, when adding cerium ion, electrostatic attraction effect can make cerium ion be adsorbed on graphene oxide sheet, contributes to crystal homogeneous nucleation.In water-heat process, graphene oxide can be reduced, and most of oxygen-containing functional group disappears, at this moment redox graphene and CeO
2between can there is Van der Waals force, make CeO
2immobilized on redox graphene sheet closely.
At RGO and nano Ce O
2in the preparation process of the microwave absorbing material of compound, when dripping precipitation agent ammoniacal liquor, be aided with ultrasonication, object improves CeO
2the dispersiveness of nanoparticle on graphene oxide sheet.At the crystal nucleation initial stage, ultrasonication can improve environment of crystal growth, improves the dispersity of nucleus, thus makes nano particle reach homodisperse degree, so also contributes to the microwave absorbing property improving material.
Advantageous Effects of the present invention embodies in the following areas:
1.the microwave absorbing material of redox graphene of the present invention and nano-cerium oxide compound, make full use of Graphene and there is high electron mobility, the feature of bigger serface, take into account the significant Lacking oxygen effect of nano-cerium oxide simultaneously, thus obtain the cerium oxide nano matrix material of absorbing property excellence, compared with nano-cerium oxide, the advantage of the microwave absorbing material of this compound is that microwave absorbing is strong, absorption band is wide, best microwave reflection loss is-32dB, when coat-thickness is 2.0mm, reflection loss reaches more than 90% lower than-10dB(absorption of electromagnetic wave) frequency span be 4.3GHz.
2. in hydro-thermal presoma process for preparation, adopt ultrasonic field assist, effectively improve nanocrystalline one-tenth nuclear environment through ultrasonic radiation, improve the dispersiveness of nanoparticle on Graphene carrier while also prevent the stacking of graphene sheet layer.
3. preparation technology of the present invention is simple, and cost is low, and security is good, without the need to adding reductive agent and tensio-active agent in building-up process, environmentally friendly.The present invention has wide development and application prospect, has and important meaning the microwave absorbing application of expanding cerium oxide nano matrix material.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of redox graphene of the present invention/cerium oxide nano matrix material.
Fig. 2 is the TEM photo of redox graphene of the present invention/cerium oxide nano matrix material.
Fig. 3 is the reflection of electromagnetic wave loss collection of illustrative plates of redox graphene of the present invention/cerium oxide nano matrix material.
Fig. 4 is that the reflection of electromagnetic wave loss of redox graphene of the present invention/cerium oxide nano matrix material and pure zirconia cerium nanoparticle contrasts collection of illustrative plates (sample coatings thickness is 2.0mm).
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Raw materials used and source as follows:
(1) natural graphite scale: 325 orders, purity >=99%, Qingdao Hua Tai permanent seal company limited
(2) potassium permanganate: purity AR, Chemical Reagent Co., Ltd., Sinopharm Group
(3) hydrogen peroxide: purity AR, Chemical Reagent Co., Ltd., Sinopharm Group
(4) vitriol oil: purity 95-98%, Tianjin Bo Di Chemical Co., Ltd.
(5) strong phosphoric acid: purity >=85%, Tianjin Bo Di Chemical Co., Ltd.
(6) hydrochloric acid: purity 36-38%, Tianjin Bo Di Chemical Co., Ltd.
(7) ammoniacal liquor: purity 25%, Chemical Reagent Co., Ltd., Sinopharm Group
(8) six nitric hydrate cerium: purity AR, Aladdin reagent
(9) ethanol: purity AR, Chemical Reagent Co., Ltd., Sinopharm Group.
The concrete operation step preparing the microwave absorbing material of redox graphene and nano-cerium oxide compound is as follows:
(1) preparation of graphite oxide
Adopt the Hummers legal system improved for graphite oxide, get 3g Graphite Powder 99 and 2g SODIUMNITRATE (NaNO
3) join in the beaker of 250mL, slowly add 70mL concentration along wall of cup and be the vitriol oil of 95 ~ 98% and stir.Under condition of ice bath, by 10g potassium permanganate (KMnO
4) be divided into 5 parts, divide and add for 5 times, interval adds once in 10 minutes, stirs one hour.Remove ice-water bath afterwards, at 35 C stirred in water bath 2h.After stirring terminates, slowly being joined by 140mL deionized water in mixing solutions and to stir 15min, now system is warming up to about 90 C, drips the hydrogen peroxide (H that concentration is 30% subsequently
2o
2) until reaction solution becomes glassy yellow.After reaction terminates, reacting liquor while hot is filtered, and wash with the dilute hydrochloric acid of 1:10 (concentrated hydrochloric acid being 36 ~ 38% by the deionized water of 500mL and 50mL concentration configures), remove unnecessary metal ion.Product is by high speed centrifugation and repeatedly wash until pH is 7.Finally by product lyophilize 48h, obtain graphite oxide.
(2) preparation of the microwave absorbing material of redox graphene and nano-cerium oxide compound
Getting 20mg graphite oxide is dissolved in the deionized water of 60mL, ultrasonic disperse 1h, and ultrasonic radiation power is 180W, the graphene oxide solution of obtained 60mL brown color.Take 0.5g six nitric hydrate cerium (Ce (NO
3)
36H
2o) join in the graphene oxide solution of 60mL, magnetic agitation.Treat that six nitric hydrate ceriums dissolve completely, under ultrasonication, slowly in reaction solution, drip 3mL concentration is 25 ~ 28% ammonia solns, and now the pH value of reaction solution is about 10, and ultrasonic radiation power is 180W, and sonication treatment time is 30min.Reaction solution is transferred in the hydrothermal reaction kettle of 100mL, 180
?hydro-thermal reaction 24h under C.After reaction terminates, product is through the purification process such as centrifugal, washing, washing with alcohol.Finally vacuum-drying 24h under 60 C, obtains the microwave absorbing material of redox graphene and nano-cerium oxide compound.
The microwave absorbing material of redox graphene and nano-cerium oxide compound can as excellent microwave absorption, and its microwave absorbing property parameter is obtained by following detection means:
The microwave absorbing material of redox graphene and nano-cerium oxide compound is mixed with paraffin (volume fraction of composite microwave absorbing material accounts for 30%), be incubated half an hour under 80 C and make paraffin melting, stir, be put in mould, under 2Mpa pressure, make internal diameter is 3.04mm, external diameter is the coaxial annulus of 7.00mm, and its thickness is polished into 2mm, be placed in coaxial line fixture build-in test, obtain real part of permittivity, imaginary part of dielectric constant, by the reflection loss of the coaxial line Theoretical Calculation matrix material of classics.
After tested, pure zirconia cerium nano particle does not almost have microwave absorbing property.And the microwave absorbing material of redox graphene of the present invention and nano-cerium oxide compound has excellent microwave absorbing property, when preparing coat-thickness and being 1.5 ~ 4.0mm, the microwave absorbing material of redox graphene and nano-cerium oxide compound is that-32 ~-10dB(absorption of electromagnetic wave reaches more than 90% at the reflection loss that frequency is 4.3 ~ 17GHz place); Microwave reflection loss reaches maximum at 17GHz place, is-32dB; When coat-thickness is 2.0mm, reflection loss reaches more than 90% lower than-10dB(absorption of electromagnetic wave) frequency span be 4.3GHz.
Claims (3)
1. the microwave absorbing material of a redox graphene and nano-cerium oxide compound, it is characterized in that: with the Hummers legal system improved for graphite oxide, by graphene oxide solution and six nitric hydrate ceriums in mass ratio 1:25 mix, adjust ph is 10, adopt one step hydro thermal method, while generation nano-cerium oxide, graphene oxide is reduced, the composite microwave absorbing material of obtained redox graphene and nano-cerium oxide;
The feature of described composite microwave absorbing material is: on the surface of reduction-oxidation graphite flakes, uniform loading ceria nanoparticles, is separated from each other between adjacent scale, in stratiform sandwich structure, contributes to the raising of microwave absorbing property;
The nano particle mean sizes of described nano-cerium oxide is 15nm, has the Lacking oxygen effect of outstanding quantum size effect and excellence;
In described composite microwave absorbing material, the weight ratio of redox graphene and nano-cerium oxide is 1:10;
When composite microwave absorbing material is the coating of thickness 1.5 ~ 4.0mm, the reflection loss being 4.3 ~ 17GHz place in frequency is-32 ~-10dB; Absorption of electromagnetic wave reaches more than 90%.
2. prepare the method for the microwave absorbing material of a kind of redox graphene and nano-cerium oxide compound described in claim 1, it is characterized in that concrete operation step is as follows:
(1) adopt the Hummers legal system improved for graphite oxide
Get 3g Graphite Powder 99 and 2g SODIUMNITRATE joins in the beaker of 250mL, slowly add 70mL concentration along wall of cup and be the vitriol oil of 95 ~ 98% and stir; Under condition of ice bath, divide and add 10g potassium permanganate 5 times, each add-on is 2g, stirs one hour; At 35 C stirred in water bath 2h, obtain mixing solutions; Slowly being joined by 140mL deionized water in mixing solutions and to stir 15min, now system is warming up to 88 ~ 92 C, and dripping concentration is that the hydrogen peroxide of 30% is until reaction solution becomes glassy yellow; Reacting liquor while hot is filtered, and washs with the dilute hydrochloric acid solution of 1:10, remove unnecessary metal ion; By high speed centrifugation and repeatedly washing until pH value is 7; Lyophilize 48h, obtains graphite oxide;
(2) preparation of the microwave absorbing material of redox graphene and nano-cerium oxide compound
Getting 20mg graphite oxide is dissolved in the deionized water of 60mL, ultrasonic disperse 1h, the graphene oxide solution of obtained 60mL brown color; Getting 0.5g six nitric hydrate cerium joins in the graphene oxide solution of 60mL, magnetic agitation; Treat that six nitric hydrate ceriums dissolve completely, under ultrasonication, in reaction solution, slowly drip the ammonia soln of 3mL concentration 25 ~ 28%, 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; Centrifugal, washing, washing with alcohol purification process; Vacuum-drying 24h under 60 C, obtains the microwave absorbing material of redox graphene and nano-cerium oxide compound.
3. the preparation method of the microwave absorbing material of redox graphene and nano-cerium oxide compound according to claim 2, is characterized in that: in step (2) in hydro-thermal presoma process for preparation, ultrasonic radiation power is 180W, and sonication treatment time is 30min.
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