CN105219345B - Preparation method of ferroferric oxide @ iron core shell structure-graphene composite absorbing material - Google Patents
Preparation method of ferroferric oxide @ iron core shell structure-graphene composite absorbing material Download PDFInfo
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Abstract
The invention relates to a preparation method of a ferroferric oxide @ iron core shell structure-graphene composite absorbing material. The preparation method is characterized in that K3[Fe(CN)6] and graphene oxide are taken as the raw materials, and further comprises three steps: firstly, on the basis of taking K3[Fe(CN)6] as the raw material, carrying out hydrothermal reaction to prepare tree-leaf-shaped alpha-Fe2O3; secondly, mixing alpha-Fe2O3 with graphene oxide, and on the basis of taking absolute ethyl alcohol as a solvent, carrying out hydrothermal reduction to produce alpha-Fe2O3-reduced graphene oxide composite material; finally, performing reduction on the alpha-Fe2O3-reduced graphene oxide composite material under a mixed atmosphere of hydrogen and argon, so as to obtain the ferroferric oxide @ iron core shell structure-graphene composite absorbing material. The preparation method is simple, controllable, can effectively broaden the absorbing range of a single material, and can further strengthen the absorbing property.
Description
Technical field
The present invention relates to field of microwave absorption, specifically a kind of ferroso-ferric oxide@iron core shell structure-Graphene composite wave-absorbing
The preparation method of material.
Background technology
With the fast development of radar and microwave electron technology, stealth technology as improve armament systems existence, it is prominent anti-and
The effective means of deep strike, becomes one of study hotspot of military power of various countries.Meanwhile, using for electronic equipment is produced in life
The a large amount of electromagnetic waves of life, cause Electromagnetic Interference, radio frequency or radio interference problem.With the development of epoch and technology, ripple material is inhaled
Material will have excellent electro-magnetic wave absorption performance in the range of wave frequency as wide as possible, it is also desirable to have light weight, resistance to
The performance such as temperature, moisture-proof, anticorrosive.Therefore, the R and D to meeting the novel wave-absorbing material of above-mentioned requirements seem particularly heavy
Will.
Ferrite starts from phase early 1940s as microwave absorbing material, is more and comparative maturity the suction ripple of research
Material.Used as conventional absorbents, ferrite has excellent absorbing property.It has, and Curie temperature is high, temperature stability is good, magnetic
The features such as conductance and larger dielectric constant, so being widely applied in absorbing material field.However, ferrite wave-absorbing material
It is disadvantageous in that high band is reduced due to absorbing property, frequency bandwidth is narrower, it is difficult to meet the new period to absorbing material wideband
Requirement with absorbing, needing to be combined with other materials just can cover the shortage.
Graphene be carbon atom periodic arrangement formed a kind of bi-dimensional cellular shape material, with high mechanical strength,
Excellent heat conductivility and great specific surface area, and the special nature such as room-temperature quantum Hall effect and room-temperature ferromagnetic.Cause
For its unique excellent properties, Graphene is used widely.Containing a large amount of residual in Graphene prepared by graphite oxide-reducing process
Complementary basis group and defect, are conducive to the absorption to microwave.Because higher specific surface area, aspect ratio and preferable microwave absorption are special
Property, can prepare that density is little, the more superior good novel wave-absorbing material of absorbing property by Graphene and other materials are compound.
Preferably absorbing material requires the characteristics of having thickness of thin, light weight, strong suction ripple, frequency range width, and single material leads to
Often it is difficult to meet simultaneously to require, it is therefore desirable to be optimized the material with different qualities compound to obtain optimum efficiency.Also
The features such as former graphene oxide has light weight, high mechanical properties, reduces the density of composite；Ferroso-ferric oxide is conventional
Magnetic material, the addition of ferroso-ferric oxide can strengthen the ferromagnetism of Graphene, make composite have magnetic loss and electrical loss concurrently,
Electromagnetic matching is advantageously implemented, strengthens absorbing property；Meanwhile, the reflectance loss of ferroso-ferric oxide generally occurs in low-frequency range,
The reflectance loss of Graphene is usually located at high frequency region, and being compounded with for the two is beneficial to absorb widening for frequency range.
The content of the invention
Technical barrier to be solved by this invention is to overcome the deficiencies in the prior art, there is provided a kind of ferroso-ferric oxide@iron
The preparation method of core shell structure-Graphene composite wave-suction material, widens the absorption region of absorbing material, strengthens absorbing property, and
The problem for effectively overcoming composite wave-suction material density big.
A kind of preparation method of ferroso-ferric oxide@iron core shell structure-Graphene composite wave-suction material, it is characterised in that：With
Potassium ferricyanide K3[Fe(CN)6], graphene oxide be made up of raw material three-step approach, first with K3[Fe(CN)6] it is raw material, by water
Thermal response makes leaf shape α-Fe2O3；Secondly by α-Fe2O3Mix with graphene oxide, with absolute ethyl alcohol as solvent, hydro-thermal is anti-
α-Fe should be generated2O3- redox graphene composite；Finally, by α-Fe2O3- redox graphene composite Jing hydrogen
The mixed atmosphere reduction of gas, argon gas, obtains ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material.
The method is concretely comprised the following steps：
（1）Take K3[Fe(CN)6] deionized water is dissolved in, controlled concentration is 0.01-1.0 mol/L, is put into polytetrafluoroethylene (PTFE)
Middle hydro-thermal reaction, temperature 130-160 DEG C, generates bolarious leaf shape α-Fe at 1-3 days time2O3。
（2）Graphene oxide is dispersed in absolute ethyl alcohol, ultrasonic disperse 30-60 min；By step（1）The tree of middle generation
Lobate α-Fe2O3In adding to the alcohol dispersion liquid of graphene oxide, and add a small amount of glycerine, magnetic agitation 1-5h；Again will mixing
Solution is placed in hydrothermal reaction kettle carries out hydrothermal reduction, temperature 160-200 DEG C, reaction time 10-24 h；After reaction terminates, lead to
Centrifuge precipitation is crossed, control rotating speed is in 8000-10000 r/min, time 10-30 min, centrifugal process absolute ethyl alcohol
Cleaning 3-5 time；The precipitation that centrifugation is obtained is placed in into vacuum drying chamber, 60-90 DEG C of drying obtains α-Fe russet2O3- reduction
Graphene oxide composite material；
（3）By the α-Fe for obtaining2O3- redox graphene composite is placed in the mixed atmosphere of hydrogen, argon gas and anneals
Reduction, controls temperature 300-400 DEG C, and hydrogen, argon flow amount compare H2: (H2+Ar)=（5-10）:100, annealing time 2-8 h；
To the leaf shape ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material of black.
Leaf shape α-Fe2O3Beam length be 3-5 μm, leaf length be 0.5-1.5 μm.
Dispersion liquid concentration of the graphene oxide in absolute ethyl alcohol is the volume of 1-6 mg/mL, absolute ethyl alcohol and glycerine
Than for（1-5）:1, α-Fe2O3It is with the mass ratio of graphene oxide（1-9）: 3.
Compared with prior art, the advantage for possessing is the present invention：
（1）Overall process is simply controllable, is mainly completed by hydro-thermal reaction；
（2）Set in the leaf shape ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material of the present invention
Lobate ferroso-ferric oxide@iron core shell structure is loaded in graphenic surface, effectively suppresses the reunion of Graphene；
（3）The absorption region of absorbing material is widened in the addition of Graphene, strengthens absorbing property, and effectively overcomes composite wave-absorbing
The big problem of density of material.
Description of the drawings
Fig. 1 is leaf shape α-Fe2O3SEM figure.
Specific embodiment
Embodiment 1：
（1）Take a certain amount of K3[Fe(CN)6] deionized water is dissolved in, controlled concentration is 0.1 mol/L, is put into polytetrafluoro
Hydro-thermal reaction in ethene, 140 DEG C of temperature, obtains bolarious leaf shape α-Fe at 2 days time2O3；
（2）The graphene oxide of certain mass is dispersed in 150 ml absolute ethyl alcohols, the min of ultrasonic disperse 30 is divided
Scattered concentration is 5 mg/mL graphene oxide dispersions；Will（1）α-the Fe of middle generation2O3By with the mass ratio of graphene oxide be 1:
In 3 alcohol dispersion liquids for adding to graphene oxide, and 50 ml glycerine are added, the h of magnetic agitation 4.Mixed solution is placed in again
Hydrothermal reduction, 200 DEG C of temperature, the h of reaction time 12 are carried out in hydrothermal reaction kettle.It is heavy by centrifuge after reaction terminates
Form sediment, control rotating speed in 10000 r/min, the min of time 10, centrifugal process washes of absolute alcohol 3 times.By sinking that centrifugation is obtained
Shallow lake is placed in vacuum drying chamber, and 70 DEG C of dryings obtain α-Fe russet2O3- redox graphene composite.
（3）By the α-Fe for obtaining2O3- redox graphene composite is placed in the mixed atmosphere of hydrogen, argon gas and anneals
Reduction, controls 350 DEG C of temperature, and hydrogen, argon flow amount compare H2/（H2+Ar）=8/100, the h of annealing time 4.Obtain the leaf of black
Shape ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material.
（4）By obtained leaf shape ferroso-ferric oxide@iron core shell structure-redox graphene composite wave-suction material with it is solid
Body paraffin presses mass fraction 10:90 uniform mixing, are pressed into the mm of external diameter 7.00, the mm of internal diameter 3.04, thickness on particular manufacturing craft
The coaxial sample of 2.0 mm, with model HP722ES vector network analyzer its suction in 2-18 gigahertz frequency ranges is tested
Ripple performance.When the matching thickness of sample is 3.6 mm, the dB of minimum reflectance -31.58, correspondence RL are reached at 10.69 GHz
<The frequency range of -10 dB is 8.3 ~ 14.9 GHz, and bin width reaches 6.6 GHz.
Embodiment 2：
（1）Take a certain amount of K3[Fe(CN)6] deionized water is dissolved in, controlled concentration is 0.1 mol/L, is put into polytetrafluoro
Hydro-thermal reaction in ethene, 140 DEG C of temperature, obtains bolarious leaf shape α-Fe at 2 days time2O3；
（2）The graphene oxide of certain mass is dispersed in 150 ml absolute ethyl alcohols, the min of ultrasonic disperse 30 is divided
Scattered concentration is 3 mg/mL graphene oxide dispersions；Will（1）α-the Fe of middle generation2O3By with the mass ratio of graphene oxide be 1:
In 1 alcohol dispersion liquid for adding to graphene oxide, and 50 ml glycerine are added, the h of magnetic agitation 4.Mixed solution is placed in again
Hydrothermal reduction, 180 DEG C of temperature, the h of reaction time 12 are carried out in hydrothermal reaction kettle.It is heavy by centrifuge after reaction terminates
Form sediment, control rotating speed in 10000 r/min, the min of time 10, centrifugal process washes of absolute alcohol 3 times.By sinking that centrifugation is obtained
Shallow lake is placed in vacuum drying chamber, and 70 DEG C of dryings obtain α-Fe russet2O3- redox graphene composite.
（3）By the α-Fe for obtaining2O3- redox graphene composite is placed in the mixed atmosphere of hydrogen, argon gas and anneals
Reduction, controls 380 DEG C of temperature, and hydrogen, argon flow amount compare H2/（H2+Ar）=8/100, the h of annealing time 3.Obtain the leaf of black
Shape ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material.
（4）By obtained leaf shape ferroso-ferric oxide@iron core shell structure-redox graphene composite wave-suction material with it is solid
Body paraffin presses mass fraction 15:85 uniform mixing, are pressed into the mm of external diameter 7.00, the mm of internal diameter 3.04, thickness on particular manufacturing craft
The coaxial sample of 2.0 mm, with model HP722ES vector network analyzer its suction in 2-18 gigahertz frequency ranges is tested
Ripple performance.When the matching thickness of sample is 4.0 mm, the dB of minimum reflectance -23.09, correspondence RL are reached at 9.16 GHz<
The frequency range of -10 dB is 7.4 ~ 11.3 GHz, and bin width reaches 3.9 GHz.
Embodiment 3：
（1）Take a certain amount of K3[Fe(CN)6] deionized water is dissolved in, controlled concentration is 0.1 mol/L, is put into polytetrafluoro
Hydro-thermal reaction in ethene, 140 DEG C of temperature, obtains bolarious leaf shape α-Fe at 2 days time2O3；
（2）The graphene oxide of certain mass is dispersed in 150 ml absolute ethyl alcohols, the min of ultrasonic disperse 30 is divided
Scattered concentration is 3 mg/mL graphene oxide dispersions；Will（1）α-the Fe of middle generation2O3By with the mass ratio of graphene oxide be 1:
In 1 alcohol dispersion liquid for adding to graphene oxide, and 50 ml glycerine are added, the h of magnetic agitation 3.Mixed solution is placed in again
Hydrothermal reduction, 160 DEG C of temperature, the h of reaction time 12 are carried out in hydrothermal reaction kettle.It is heavy by centrifuge after reaction terminates
Form sediment, control rotating speed in 10000 r/min, the min of time 10, centrifugal process washes of absolute alcohol 3 times.By sinking that centrifugation is obtained
Shallow lake is placed in vacuum drying chamber, and 70 DEG C of dryings obtain α-Fe russet2O3- redox graphene composite.
（3）By the α-Fe for obtaining2O3- redox graphene composite is placed in the mixed atmosphere of hydrogen, argon gas and anneals
Reduction, controls 330 DEG C of temperature, and hydrogen, argon flow amount compare H2/（H2+Ar）=8/100, the h of annealing time 3.Obtain the leaf of black
Shape ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material.
（4）By obtained leaf shape ferroso-ferric oxide@iron core shell structure-redox graphene composite wave-suction material with it is solid
Body paraffin presses mass fraction 15:85 uniform mixing, are pressed into the mm of external diameter 7.00, the mm of internal diameter 3.04, thickness on particular manufacturing craft
The coaxial sample of 2.0 mm, with model HP722ES vector network analyzer its suction in 2-18 gigahertz frequency ranges is tested
Ripple performance.When the matching thickness of sample is 2.8 mm, the dB of minimum reflectance -20.09, correspondence RL are reached at 13.82 GHz
<The frequency range of -10 dB is 11.5 ~ 17.3 GHz, and bin width reaches 5.8 GHz.
Claims (2)
1. a kind of preparation method of ferroso-ferric oxide@iron core shell structure-Graphene composite wave-suction material, it is characterised in that：With iron
Potassium cyanide K3[Fe(CN)6], graphene oxide be made up of raw material three-step approach, first with K3[Fe(CN)6] it is raw material, by hydro-thermal
Leaf shape α-Fe are made in reaction2O3；Secondly by α-Fe2O3Mix with graphene oxide, with absolute ethyl alcohol as solvent, hydro-thermal reaction
Generate α-Fe2O3- redox graphene composite；Finally, by α-Fe2O3- redox graphene composite Jing hydrogen
The mixed atmosphere reduction of gas, argon gas, obtains ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material, should
Method is concretely comprised the following steps：
（1）Take K3[Fe(CN)6] deionized water is dissolved in, controlled concentration is 0.01-1.0 mol/L, is put into water in polytetrafluoroethylene (PTFE)
Thermal response, temperature 130-160 DEG C, generates bolarious leaf shape α-Fe at 1-3 days time2O3；
（2）Graphene oxide is dispersed in absolute ethyl alcohol, ultrasonic disperse 30-60 min；By step（1）The leaf shape of middle generation
α-Fe2O3In adding to the alcohol dispersion liquid of graphene oxide, and add a small amount of glycerine, magnetic agitation 1-5h；Again by mixed solution
Being placed in hydrothermal reaction kettle carries out hydrothermal reduction, temperature 160-200 DEG C, reaction time 10-24 h；Reaction terminate after, by from
Scheming centrifugation, control rotating speed is in 8000-10000 r/min, time 10-30 min, centrifugal process washes of absolute alcohol
3-5 time；The precipitation that centrifugation is obtained is placed in into vacuum drying chamber, 60-90 DEG C of drying obtains α-Fe russet2O3- reduction-oxidation
Graphene composite material；
（3）By the α-Fe for obtaining2O3- redox graphene composite is placed in annealing in the mixed atmosphere of hydrogen, argon gas and goes back
Original, controls temperature 300-400 DEG C, and hydrogen, argon flow amount compare H2: (H2+Ar)=（5-10）:100, annealing time 2-8 h；Obtain
The leaf shape ferroso-ferric oxide@iron core shell structures-redox graphene composite wave-suction material of black；
Dispersion liquid concentration of the graphene oxide in absolute ethyl alcohol is 1-6 mg/mL, and absolute ethyl alcohol is with the volume ratio of glycerine
（1-5）:1, α-Fe2O3It is with the mass ratio of graphene oxide（1-9）: 3.
2. a kind of preparation side of ferroso-ferric oxide@iron core shell structure-Graphene composite wave-suction material according to claim 1
Method, it is characterised in that leaf shape α-Fe2O3Beam length be 3-5 μm, leaf length be 0.5-1.5 μm.
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| CN110041884B (en) * | 2018-01-15 | 2022-05-17 | 深圳烯创先进材料研究院有限公司 | Leaf-shaped nano Fe3O4Preparation method of filled wave-absorbing composite material with honeycomb sandwich structure |
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| CN114085649A (en) * | 2020-08-25 | 2022-02-25 | 安徽璜峪电磁技术有限公司 | Non-metal graphene-based composite wave-absorbing material and preparation method thereof |
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| CN102544457B (en) * | 2012-02-17 | 2014-12-03 | 合肥工业大学 | Method for preparing graphene oxide-iron sesquioxide nanotube composite material by using in-situ method |
| CN104037405A (en) * | 2013-03-06 | 2014-09-10 | 佛山市顺德宇红纳米科技有限公司 | Method for preparation of ferric oxide/graphene/carbon fiber composite material |
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