CN105219345A - A kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material - Google Patents
A kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material Download PDFInfo
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- CN105219345A CN105219345A CN201510671580.1A CN201510671580A CN105219345A CN 105219345 A CN105219345 A CN 105219345A CN 201510671580 A CN201510671580 A CN 201510671580A CN 105219345 A CN105219345 A CN 105219345A
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Abstract
The present invention relates to a kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material.With K
3[Fe (CN)
6], graphene oxide is that raw material three-step approach is made, first with K
3[Fe (CN)
6] be raw material, make leaf shape α-Fe by hydro-thermal reaction
2o
3; Secondly by α-Fe
2o
3mixing with graphene oxide, take dehydrated alcohol as solvent, and hydrothermal reduction generates α-Fe
2o
3-redox graphene matrix material; Finally, by α-Fe
2o
3-redox graphene matrix material reduces through the mixed atmosphere of hydrogen, argon gas, obtains Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material.The inventive method is simple, controlled, effectively widens the suction ripple scope of single-material, strengthens absorbing property.
Description
Technical field
The present invention relates to field of microwave absorption, specifically a kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material.
Background technology
Along with the fast development of radar and microwave electron technology, stealthy technique, as the effective means improving weapons system existence, prominent anti-and deep strike, becomes one of study hotspot of military power of various countries.Meanwhile, in life, the utilization of electronics produces a large amount of hertzian wave, causes Electromagnetic Interference, radio frequency or wireless interference problem.Along with the development of epoch and technology, absorbing material will have excellent absorption of electromagnetic wave performance within the scope of wave frequency wide as far as possible, also require to have that quality is light, heatproof, moisture-proof, the performance such as anticorrosive.Therefore, the R and D of the novel wave-absorbing material meeting above-mentioned requirements are seemed particularly important.
Ferrite starts from phase early 1940s as microwave absorbing material, is the more and absorbing material of comparative maturity of research.As conventional absorbents, ferrite has excellent absorbing property.It has that Curie temperature is high, temperature stability good, magnetic permeability and the feature such as specific inductivity is larger, so be widely applied in absorbing material field.But ferrite wave-absorbing material weak point is that high band reduces due to absorbing property, and frequency span is narrower, is difficult to meet the requirement that the new period absorbs absorbing material broadband, needs just can cover the shortage with other materials compound.
Graphene is a kind of bi-dimensional cellular shape material that carbon atom periodic arrangement is formed, and has high physical strength, excellent heat conductivility and great specific surface area, and the special property such as room-temperature quantum Hall effect and room-temperature ferromagnetic.Because the excellent properties of its uniqueness, Graphene is used widely.Containing abundant residues group and defect in Graphene prepared by graphite oxide-reduction method, be conducive to the absorption to microwave.Because higher specific surface area, aspect ratio and desirable Microwave Absorption Properties, Graphene and other materials compound can be prepared density is little, the more superior good novel wave-absorbing material of absorbing property.
Desirable absorbing material requires to have the advantages that thickness is thin, quality light, suction ripple is strong, frequency range is wide, and single material is difficult to meet the demands usually simultaneously, therefore needs the material with different qualities to be optimized compound to obtain best effect.Redox graphene has that quality is light, mechanical property high, reduces the density of matrix material; Z 250 is conventional magneticsubstance, Z 250 add the ferromegnetism that can strengthen Graphene, make matrix material have magnetic loss and electrical loss concurrently, be conducive to realizing electromagnetic matching, strengthen absorbing property; Meanwhile, the reflectance loss of Z 250 usually occurs in low-frequency range, and the reflectance loss of Graphene is usually located at high frequency region, and being compounded with of the two is beneficial to widening of absorption frequency range.
Summary of the invention
Technical barrier to be solved by this invention overcomes the deficiencies in the prior art, provide a kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material, widen the absorption region of absorbing material, strengthen absorbing property, and effectively overcome the large problem of composite wave-suction material density.
A preparation method for Z 250 iron nucleocapsid structure-Graphene composite wave-suction material, is characterized in that: with Tripotassium iron hexacyanide K
3[Fe (CN)
6], graphene oxide is that raw material three-step approach is made, first with K
3[Fe (CN)
6] be raw material, make leaf shape α-Fe by hydro-thermal reaction
2o
3; Secondly by α-Fe
2o
3mixing with graphene oxide, take dehydrated alcohol as solvent, and hydro-thermal reaction generates α-Fe
2o
3-redox graphene matrix material; Finally, by α-Fe
2o
3-redox graphene matrix material reduces through the mixed atmosphere of hydrogen, argon gas, obtains Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material.
The concrete steps of the method are:
(1) K is got
3[Fe (CN)
6] be dissolved in deionized water, controlled concentration is 0.01-1.0mol/L, puts into tetrafluoroethylene hydro-thermal reaction, temperature 130-160 DEG C, time 1-3 days, generates bolarious leaf shape α-Fe
2o
3.
(2) graphene oxide is dispersed in dehydrated alcohol, ultrasonic disperse 30-60min; By the leaf shape α-Fe generated in step (1)
2o
3add in the alcohol dispersion liquid of graphene oxide, and add a small amount of glycerol, magnetic agitation 1-5h; Again mixing solutions is placed in hydrothermal reaction kettle and carries out hydrothermal reduction, temperature 160-200 DEG C, reaction times 10-24h; After reaction terminates, precipitated by centrifuge, control rotating speed at 8000-10000r/min, time 10-30min, centrifugal process washes of absolute alcohol 3-5 time; The centrifugal precipitation obtained is placed in vacuum drying oven, 60-90 DEG C of drying, obtains α-Fe russet
2o
3-redox graphene matrix material;
(3) α-Fe will obtained
2o
3-redox graphene matrix material is placed in the mixed atmosphere annealing reduction of hydrogen, argon gas, and control temperature 300-400 DEG C, hydrogen, argon flow amount compare H
2: (H
2+ Ar)=(5-10): 100, annealing time 2-8h; Obtain the leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material of black.
Leaf shape α-Fe
2o
3beam length be 3-5 μm, leaf length is 0.5-1.5 μm.
The dispersion liquid concentration of graphene oxide in dehydrated alcohol is 1-6mg/mL, and the volume ratio of dehydrated alcohol and glycerol is (1-5): 1, α-Fe
2o
3be (1-9) with the mass ratio of graphene oxide: 3.
Compared with prior art, the advantage possessed is in the present invention:
(1) overall process is simply controlled, completes mainly through hydro-thermal reaction;
(2) in leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material of the present invention, leaf shape Z 250 iron nucleocapsid structure, in graphenic surface load, effectively suppresses the reunion of Graphene;
(3) Graphene add the absorption region widening absorbing material, strengthen absorbing property, and effectively overcome the large problem of composite wave-suction material density.
Accompanying drawing explanation
Fig. 1 is leaf shape α-Fe
2o
3sEM figure.
Embodiment
Embodiment 1:
(1) a certain amount of K is got
3[Fe (CN)
6] be dissolved in deionized water, controlled concentration is 0.1mol/L, puts into tetrafluoroethylene hydro-thermal reaction, temperature 140 DEG C, 2 days time, obtains bolarious leaf shape α-Fe
2o
3;
(2) be dispersed in 150ml dehydrated alcohol by the graphene oxide of certain mass, ultrasonic disperse 30min, obtaining dispersion concentration is 5mg/mL graphene oxide dispersion; By the α-Fe generated in (1)
2o
3be that 1:3 adds in the alcohol dispersion liquid of graphene oxide by the mass ratio with graphene oxide, and add 50ml glycerol, magnetic agitation 4h.Again mixing solutions is placed in hydrothermal reaction kettle and carries out hydrothermal reduction, temperature 200 DEG C, reaction times 12h.After reaction terminates, precipitated by centrifuge, control rotating speed at 10000r/min, time 10min, centrifugal process washes of absolute alcohol 3 times.The centrifugal precipitation obtained is placed in vacuum drying oven, 70 DEG C of dryings, obtains α-Fe russet
2o
3-redox graphene matrix material.
(3) α-Fe will obtained
2o
3-redox graphene matrix material is placed in the mixed atmosphere annealing reduction of hydrogen, argon gas, and control temperature 350 DEG C, hydrogen, argon flow amount compare H
2/ (H
2+ Ar)=8/100, annealing time 4h.Obtain the leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material of black.
(4) obtained leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material and solid paraffin are pressed massfraction 10:90 Homogeneous phase mixing, particular manufacturing craft is pressed into the coaxial sample of external diameter 7.00mm, internal diameter 3.04mm, thickness 2.0mm, is that HP722ES vector network analyzer tests its absorbing property in 2-18GHz range of frequency by model.When the matching thickness of sample is 3.6mm, reach minimum reflectance-31.58dB at 10.69GHz place, the frequency range of corresponding RL<-10dB is 8.3 ~ 14.9GHz, and bin width reaches 6.6GHz.
Embodiment 2:
(1) a certain amount of K is got
3[Fe (CN)
6] be dissolved in deionized water, controlled concentration is 0.1mol/L, puts into tetrafluoroethylene hydro-thermal reaction, temperature 140 DEG C, 2 days time, obtains bolarious leaf shape α-Fe
2o
3;
(2) be dispersed in 150ml dehydrated alcohol by the graphene oxide of certain mass, ultrasonic disperse 30min, obtaining dispersion concentration is 3mg/mL graphene oxide dispersion; By the α-Fe generated in (1)
2o
3be that 1:1 adds in the alcohol dispersion liquid of graphene oxide by the mass ratio with graphene oxide, and add 50ml glycerol, magnetic agitation 4h.Again mixing solutions is placed in hydrothermal reaction kettle and carries out hydrothermal reduction, temperature 180 DEG C, reaction times 12h.After reaction terminates, precipitated by centrifuge, control rotating speed at 10000r/min, time 10min, centrifugal process washes of absolute alcohol 3 times.The centrifugal precipitation obtained is placed in vacuum drying oven, 70 DEG C of dryings, obtains α-Fe russet
2o
3-redox graphene matrix material.
(3) α-Fe will obtained
2o
3-redox graphene matrix material is placed in the mixed atmosphere annealing reduction of hydrogen, argon gas, and control temperature 380 DEG C, hydrogen, argon flow amount compare H
2/ (H
2+ Ar)=8/100, annealing time 3h.Obtain the leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material of black.
(4) obtained leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material and solid paraffin are pressed massfraction 15:85 Homogeneous phase mixing, particular manufacturing craft is pressed into the coaxial sample of external diameter 7.00mm, internal diameter 3.04mm, thickness 2.0mm, is that HP722ES vector network analyzer tests its absorbing property in 2-18GHz range of frequency by model.When the matching thickness of sample is 4.0mm, reach minimum reflectance-23.09dB at 9.16GHz place, the frequency range of corresponding RL<-10dB is 7.4 ~ 11.3GHz, and bin width reaches 3.9GHz.
Embodiment 3:
(1) a certain amount of K is got
3[Fe (CN)
6] be dissolved in deionized water, controlled concentration is 0.1mol/L, puts into tetrafluoroethylene hydro-thermal reaction, temperature 140 DEG C, 2 days time, obtains bolarious leaf shape α-Fe
2o
3;
(2) be dispersed in 150ml dehydrated alcohol by the graphene oxide of certain mass, ultrasonic disperse 30min, obtaining dispersion concentration is 3mg/mL graphene oxide dispersion; By the α-Fe generated in (1)
2o
3be that 1:1 adds in the alcohol dispersion liquid of graphene oxide by the mass ratio with graphene oxide, and add 50ml glycerol, magnetic agitation 3h.Again mixing solutions is placed in hydrothermal reaction kettle and carries out hydrothermal reduction, temperature 160 DEG C, reaction times 12h.After reaction terminates, precipitated by centrifuge, control rotating speed at 10000r/min, time 10min, centrifugal process washes of absolute alcohol 3 times.The centrifugal precipitation obtained is placed in vacuum drying oven, 70 DEG C of dryings, obtains α-Fe russet
2o
3-redox graphene matrix material.
(3) α-Fe will obtained
2o
3-redox graphene matrix material is placed in the mixed atmosphere annealing reduction of hydrogen, argon gas, and control temperature 330 DEG C, hydrogen, argon flow amount compare H
2/ (H
2+ Ar)=8/100, annealing time 3h.Obtain the leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material of black.
(4) obtained leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material and solid paraffin are pressed massfraction 15:85 Homogeneous phase mixing, particular manufacturing craft is pressed into the coaxial sample of external diameter 7.00mm, internal diameter 3.04mm, thickness 2.0mm, is that HP722ES vector network analyzer tests its absorbing property in 2-18GHz range of frequency by model.When the matching thickness of sample is 2.8mm, reach minimum reflectance-20.09dB at 13.82GHz place, the frequency range of corresponding RL<-10dB is 11.5 ~ 17.3GHz, and bin width reaches 5.8GHz.
Claims (4)
1. a preparation method for Z 250 iron nucleocapsid structure-Graphene composite wave-suction material, is characterized in that: with Tripotassium iron hexacyanide K
3[Fe (CN)
6], graphene oxide is that raw material three-step approach is made, first with K
3[Fe (CN)
6] be raw material, make leaf shape α-Fe by hydro-thermal reaction
2o
3; Secondly by α-Fe
2o
3mixing with graphene oxide, take dehydrated alcohol as solvent, and hydro-thermal reaction generates α-Fe
2o
3-redox graphene matrix material; Finally, by α-Fe
2o
3-redox graphene matrix material reduces through the mixed atmosphere of hydrogen, argon gas, obtains Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material.
2. the preparation method of a kind of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material according to claim 1, it is characterized in that, the concrete steps of the method are:
(1) K is got
3[Fe (CN)
6] be dissolved in deionized water, controlled concentration is 0.01-1.0mol/L, puts into tetrafluoroethylene hydro-thermal reaction, temperature 130-160 DEG C, time 1-3 days, generates bolarious leaf shape α-Fe
2o
3;
(2) graphene oxide is dispersed in dehydrated alcohol, ultrasonic disperse 30-60min; By the leaf shape α-Fe generated in step (1)
2o
3add in the alcohol dispersion liquid of graphene oxide, and add a small amount of glycerol, magnetic agitation 1-5h; Again mixing solutions is placed in hydrothermal reaction kettle and carries out hydrothermal reduction, temperature 160-200 DEG C, reaction times 10-24h; After reaction terminates, precipitated by centrifuge, control rotating speed at 8000-10000r/min, time 10-30min, centrifugal process washes of absolute alcohol 3-5 time; The centrifugal precipitation obtained is placed in vacuum drying oven, 60-90 DEG C of drying, obtains α-Fe russet
2o
3-redox graphene matrix material;
(3) α-Fe will obtained
2o
3-redox graphene matrix material is placed in the mixed atmosphere annealing reduction of hydrogen, argon gas, and control temperature 300-400 DEG C, hydrogen, argon flow amount compare H
2: (H
2+ Ar)=(5-10): 100, annealing time 2-8h; Obtain the leaf shape Z 250 iron nucleocapsid structure-redox graphene composite wave-suction material of black.
3. the preparation method of a kind of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material according to claim 1, is characterized in that, leaf shape α-Fe
2o
3beam length be 3-5 μm, leaf length is 0.5-1.5 μm.
4. the preparation method of a kind of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material according to claim 1, it is characterized in that, the dispersion liquid concentration of graphene oxide in dehydrated alcohol is 1-6mg/mL, and the volume ratio of dehydrated alcohol and glycerol is (1-5): 1, α-Fe
2o
3be (1-9) with the mass ratio of graphene oxide: 3.
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| CN106374233A (en) * | 2016-12-06 | 2017-02-01 | 周潇潇 | High-efficiency wave absorbing composite material |
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| CN106207137A (en) * | 2016-09-12 | 2016-12-07 | 华中科技大学 | A kind of composite negative electrode material of lithium ion battery and preparation method thereof |
| CN106374233A (en) * | 2016-12-06 | 2017-02-01 | 周潇潇 | High-efficiency wave absorbing composite material |
| CN107734948A (en) * | 2017-09-05 | 2018-02-23 | 西北工业大学 | Broadband absorbing material and preparation method based on frequency-selective surfaces and sandwich sandwich design |
| 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 |
| CN110041884A (en) * | 2018-01-15 | 2019-07-23 | 深圳烯创先进材料研究院有限公司 | A kind of leaf shape nanometer Fe3O4The preparation method of the honeycomb sandwich structure Wave suction composite material of filling |
| CN110964480A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Graphene oxide/ferroferric oxide/zinc oxide composite material, preparation method thereof and graphene-based magnetic heat-conducting wave-absorbing material |
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| CN110707319A (en) * | 2019-09-27 | 2020-01-17 | 上海应用技术大学 | Three-dimensional structured graphene-based iron oxide composite material and preparation and application thereof |
| CN111128560A (en) * | 2019-12-13 | 2020-05-08 | 蚌埠学院 | Preparation method and application of iron oxide/graphene composite nano material |
| 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 |
| CN113088251A (en) * | 2021-04-01 | 2021-07-09 | 安徽理工大学 | Bimetal MOFs derived Fe3O4Preparation method of/Fe/C composite wave-absorbing material |
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