CN109233741A - A kind of preparation method of three-dimensional carbon network load cobalt ferrite nano-particles reinforcement wave absorbing agent - Google Patents
A kind of preparation method of three-dimensional carbon network load cobalt ferrite nano-particles reinforcement wave absorbing agent Download PDFInfo
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- CN109233741A CN109233741A CN201811066644.5A CN201811066644A CN109233741A CN 109233741 A CN109233741 A CN 109233741A CN 201811066644 A CN201811066644 A CN 201811066644A CN 109233741 A CN109233741 A CN 109233741A
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Abstract
The present invention relates to a kind of preparation methods of three-dimensional carbon network load cobalt ferrite nano-particles reinforcement wave absorbing agent, it include: that (1) desivac prepares composite material precursor powder: using cabaltous nitrate hexahydrate as cobalt source, Fe(NO3)39H2O is source of iron, DEXTROSE ANHYDROUS is carbon source, sodium chloride is as template, wherein the molar ratio of Co:Fe:C:NaCl is 0.5:1:20:150, by cobalt source, source of iron, carbon source and sodium chloride dissolution are in deionized water, uniform mixed solution is obtained by magnetic agitation, uniformly mixed solution is placed in refrigerator and is freezed, precursor powder is obtained using frozen dried.(2) calcining of composite material precursor powder.(3) removal of NaCl template.The three-dimensional carbon network load cobalt ferrite nano particle composite material can be applied to electro-magnetic wave absorption.
Description
Technical field
The present invention relates to a kind of three-dimensional carbon network load cobalt ferrite nano particle composite materials for electro-magnetic wave absorption
Preparation method belongs to absorbing material field.
Background technique
Due to electronics being widely used in people's daily life, a large amount of electromagnetic wave has been full of our life
Space living, the health for not only endangering the mankind also disturb the normal work of other electronic equipments.Currently, electromagnetic pollution is asked
Topic just gradually gets more and more people's extensive concerning.Brought harm to solve electromagnetic radiation, a kind of most effective approach be utilize it is electric
Electro-magnetic wave absorption material.Absorbing material can be divided into structural absorbing mater ials and coating-type absorbing materials, and wherein application type inhales wave material
Material has obtained a large amount of research due to the feature that its structure is simple, thickness is thin, absorbent properties are good, adaptable to target shape.
Coating-type absorbing materials mainly consist of two parts: wave absorbing agent and binder.Wherein wave absorbing agent is the key point of absorbing material,
Directly decide the absorbing property of material.
Ferrite Material, since it is with very strong absorbent properties, has obtained extensive as a kind of traditional wave absorbing agent
Using.But the electromagnetic environment to become increasingly complex is to absorbing material that more stringent requirements are proposed: not only having stronger absorption
Ability should also meet the wide needs of thin thickness, light weight, absorption band.And ferrite is since its density is big, absorption band
Narrow, the big disadvantage of additive amount in the base, is no longer satisfied the requirement of " thin, light, wide, strong " feature.Therefore, researcher just causes
Power is in the research and development of New Radar Absorbing agent.
Carbon material is shown due to having the advantages that low density, stable structure, electrical and thermal conductivity are good in absorbing material field
Good application prospect.But single carbon material, without magnetism, loss mechanisms are single, and impedance matching property is poor, lead to it
Show lower absorbing property.Recently, researcher has found, carbon material is carried out the compound each group that can play with ferrite and is become a useful person
The synergistic effect of material improves impedance matching property, inhales to obtain the high-performance that light weight, absorption band are wide, absorbent properties are strong
Wave agent.Currently, carbon-based ferrite wave absorbing agent mainly include carbon fiber/ferrite wave absorbing agent, carbon nanotube/ferrite wave absorbing agent,
Graphene/ferrite wave absorbing agent and porous carbon/ferrite wave absorbing agent.Although the research about carbon-based ferrite composite wave-absorbing agent
There are many reports, but the cost of great number, complicated preparation process, low production restriction its development and application.
In addition to this, the existing addition of most of carbon-based ferrite wave absorbing agent in the base effectively absorbs still in 30wt% or more
Frequency band is still in 6GHz hereinafter, lightweight and the performance of wideband need further to improve.Therefore, using the raw material of low cost, lead to
Simple synthesis technology is crossed, is prepared on a large scale out lightweight, the carbon-based ferrite wave absorbing agent of wideband just becomes exploitation New Radar Absorbing
Material important directions.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of three-dimensional carbon network load cobalt ferrite nano particle composite material
Method, the composite material are supported on three-dimensional carbon network by ferrous acid cobalt nano-particle and are constituted, and preparation method is simple and easy, can measure
It produces, and has the characteristics that light weight, absorption band are wide, good absorption can be played to electromagnetic wave, be expected to further reality
Now industrial application.Technical scheme is as follows:
A kind of preparation method of three-dimensional carbon network load cobalt ferrite nano-particles reinforcement wave absorbing agent, steps are as follows:
(1) desivac prepares composite material precursor powder
Using cabaltous nitrate hexahydrate as cobalt source, Fe(NO3)39H2O is source of iron, and DEXTROSE ANHYDROUS is carbon source, and sodium chloride is as mould
Plate, wherein the molar ratio of Co:Fe:C:NaCl be 0.5:1:20:150, by cobalt source, source of iron, carbon source and sodium chloride be dissolved in from
In sub- water, uniform mixed solution is obtained by magnetic agitation, uniformly mixed solution is placed in refrigerator and is freezed, using jelly
Dry-cure obtains precursor powder.
(2) calcining of composite material precursor powder
Precursor powder prepared in step (1) is laid in Noah's ark, tube furnace flat-temperature zone is placed in and is calcined: with argon
Gas rises to 600~650 DEG C as protective atmosphere, with the heating rate of 10 DEG C/min, keep the temperature 2 hours carry out glucose carbonization with
And the decomposition of cobalt nitrate and ferric nitrate, cooled down after reaction with the rate of 5 DEG C/min, after being cooled to room temperature, obtains calcining and produce
Object.
(3) removal of NaCl template
Calcined product obtained in collection step (2), is washed to until not having NaCl in product, finally in 80 DEG C of baking ovens
Drying obtains three-dimensional carbon network load cobalt ferrite nano particle composite material.
The three-dimensional carbon network load cobalt ferrite nano particle composite material is applied to electro-magnetic wave absorption.
The features of the present invention: the present invention has been prepared in situ three-dimensional carbon network load cobalt ferrite using raw material cheap and easy to get and has received
Rice grain composite material, preparation process is simple, and material can mass production.Cobalt ferrite is on three-dimensional carbon network in composite material
It is evenly distributed, and has good interface cohesion with carbon base body.As wave absorbing agent, loading of the composite material in paraffin matrix is only
For 20wt%.When inhaling wave layer with a thickness of 2.5mm, composite material achieves effective absorption band of 6.63GHz (11.37-18GHz)
Width covers entire Ku wave band, is expected to realize popularization and use industrially.
Detailed description of the invention
Fig. 1 is the XRD diagram of the resulting three-dimensional carbon network load cobalt ferrite nano particle composite material of the embodiment of the present invention 1.
Fig. 2 is that the SEM of the resulting three-dimensional carbon network load cobalt ferrite nano particle composite material of the embodiment of the present invention 1 shines
Piece.
Fig. 3 is the TEM photo of the resulting three-dimensional carbon network load cobalt ferrite nano particle composite material of the embodiment of the present invention 1
And constituent analysis.
Fig. 4 is that the electromagnetism of the resulting three-dimensional carbon network load cobalt ferrite nano particle composite material of the embodiment of the present invention 1 is joined
Several and absorbing property figure.
Specific embodiment:
The present invention will be described with attached drawing combined with specific embodiments below, these embodiments are only intended to illustrate this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1
0.647g cabaltous nitrate hexahydrate, 1.796g Fe(NO3)39H2O, 2.667g DEXTROSE ANHYDROUS, 39g sodium chloride are weighed,
Mixture is dissolved in 130ml deionized water simultaneously magnetic agitation 4 hours, uniform mixed solution is obtained.Acquired solution is poured into
In the culture dish that two diameters are 18cm, it is subsequently placed in refrigerator, is freezed for 24 hours at a temperature of -20 DEG C.The two disk solution frozen are put
Enter in freeze drier, is dried in vacuo at a temperature of -50 DEG C for 24 hours, obtains presoma.Presoma is ground into powder, 15g is taken to be placed in
In Noah's ark, Noah's ark is put into tube furnace flat-temperature zone, 400ml/min Ar 15min is passed through and empties air, then with 80ml/min Ar
630 DEG C are warming up to as protective atmosphere, and with the heating rate of 10 DEG C/min, heat preservation 2h carries out carbonization and the nitric acid of glucose
The decomposition of cobalt and ferric nitrate is cooled to room temperature under Ar atmosphere protection after reaction, obtains calcined product.Calcining is collected to produce
Object, being washed in product does not have NaCl, finally dries in 80 DEG C of baking ovens, and three-dimensional carbon network load ferrous acid cobalt nano-particle is made
Composite material.
Precursor powder is as shown in Figure 1 by the XRD for calcining and removing the product after NaCl in embodiment 1, it is known that system
The main component of standby composite material is CoFe2O4;In addition there are also a small amount of FeO to exist.SEM observation shows that material has and mutually interconnects
Logical three-dimensional network-like structure, and CoFe is evenly distributed on carbon network2O4Nano particle.TEM picture further illustrates
The tridimensional network and CoFe of composite material2O4Nano particle is uniformly distributed carbon base body, is consistent with SEM figure;Except this it
Outside, it is swept by first vegetarian noodles, power spectrum and high power TEM have further determined that the particle on three-dimensional carbon network is mainly CoFe2O4Nanometer
Particle, and particle and carbon base body have good interface cohesion.
By in embodiment 1 three-dimensional carbon network load cobalt ferrite nano particle composite material and solid paraffin according to mass ratio
20%:80% is uniformly mixed, and the coaxial circles of outer diameter 7.00mm, internal diameter 3.00mm, thickness 2.00mm are pressed into particular manufacturing craft
Ring sample tests its electromagnetic parameter in 1-18GHz frequency range with model HP-8722ES vector network analyzer, and according to
Transmission line theory equation, by MATLAB software calculated the dielectric loss tangent value of composite sample, magnetic loss tangent value and
Reflection loss curve, as shown in Figure 4.When inhaling wave layer with a thickness of 2.5mm, reflection loss (RL) value of the composite material is-
19.6dB, effective Absorber Bandwidth (RL < -10dB) have reached 6.63GHz (11.37-18GHz), have covered entire Ku wave band.Except this
Except, composite material, which inhales effective Absorber Bandwidth (RL < -10dB) in wave layer thickness range in 1.5~5.0mm, to be reached
12.75GHz(5.25-18GHz).To sum up, three-dimensional carbon network load cobalt ferrite nano particle composite material is shown good
Electromagnetic wave absorption performance.
Embodiment 2
0.647g cabaltous nitrate hexahydrate, 1.796g Fe(NO3)39H2O, 2.667g DEXTROSE ANHYDROUS, 39g sodium chloride are weighed,
Mixture is dissolved in 130ml deionized water simultaneously magnetic agitation 4 hours, uniform mixed solution is obtained.Acquired solution is poured into
In the culture dish that two diameters are 18cm, it is subsequently placed in refrigerator, is freezed for 24 hours at a temperature of -20 DEG C.The two disk solution frozen are put
Enter in freeze drier, is dried in vacuo at a temperature of -50 DEG C for 24 hours, obtains presoma.Presoma is ground into powder, 15g is taken to be placed in
In Noah's ark, Noah's ark is put into tube furnace flat-temperature zone, 400ml/min Ar 15min is passed through and empties air, then with 80ml/min Ar
600 DEG C are warming up to as protective atmosphere, and with the heating rate of 10 DEG C/min, heat preservation 2h carries out carbonization and the nitric acid of glucose
The decomposition of cobalt and ferric nitrate is cooled to room temperature under Ar atmosphere protection after reaction, obtains calcined product.Calcining is collected to produce
Object, being washed in product does not have NaCl, finally dries in 80 DEG C of baking ovens, and three-dimensional carbon network load ferrous acid cobalt nano-particle is made
Composite material.
Embodiment 3
0.647g cabaltous nitrate hexahydrate, 1.796g Fe(NO3)39H2O, 2.667g DEXTROSE ANHYDROUS, 39g sodium chloride are weighed,
Mixture is dissolved in 130ml deionized water simultaneously magnetic agitation 4 hours, uniform mixed solution is obtained.Acquired solution is poured into
In the culture dish that two diameters are 18cm, it is subsequently placed in refrigerator, is freezed for 24 hours at a temperature of -20 DEG C.The two disk solution frozen are put
Enter in freeze drier, is dried in vacuo at a temperature of -50 DEG C for 24 hours, obtains presoma.Presoma is ground into powder, 15g is taken to be placed in
In Noah's ark, Noah's ark is put into tube furnace flat-temperature zone, 400ml/min Ar 15min is passed through and empties air, then with 80ml/min Ar
620 DEG C are warming up to as protective atmosphere, and with the heating rate of 10 DEG C/min, heat preservation 2h carries out carbonization and the nitric acid of glucose
The decomposition of cobalt and ferric nitrate is cooled to room temperature under Ar atmosphere protection after reaction, obtains calcined product.Calcining is collected to produce
Object, being washed in product does not have NaCl, finally dries in 80 DEG C of baking ovens, and three-dimensional carbon network load ferrous acid cobalt nano-particle is made
Composite material.
Embodiment 4
0.647g cabaltous nitrate hexahydrate, 1.796g Fe(NO3)39H2O, 2.667g DEXTROSE ANHYDROUS, 39g sodium chloride are weighed,
Mixture is dissolved in 130ml deionized water simultaneously magnetic agitation 4 hours, uniform mixed solution is obtained.Acquired solution is poured into
In the culture dish that two diameters are 18cm, it is subsequently placed in refrigerator, is freezed for 24 hours at a temperature of -20 DEG C.The two disk solution frozen are put
Enter in freeze drier, is dried in vacuo at a temperature of -50 DEG C for 24 hours, obtains presoma.Presoma is ground into powder, 15g is taken to be placed in
In Noah's ark, Noah's ark is put into tube furnace flat-temperature zone, 400ml/min Ar 15min is passed through and empties air, then with 80ml/min Ar
650 DEG C are warming up to as protective atmosphere, and with the heating rate of 10 DEG C/min, heat preservation 2h carries out carbonization and the nitric acid of glucose
The decomposition of cobalt and ferric nitrate is cooled to room temperature under Ar atmosphere protection after reaction, obtains calcined product.Calcining is collected to produce
Object, being washed in product does not have NaCl, finally dries in 80 DEG C of baking ovens, and three-dimensional carbon network load ferrous acid cobalt nano-particle is made
Composite material.
Claims (2)
1. a kind of preparation method of three-dimensional carbon network load cobalt ferrite nano-particles reinforcement wave absorbing agent, steps are as follows:
(1) desivac prepares composite material precursor powder
Using cabaltous nitrate hexahydrate as cobalt source, Fe(NO3)39H2O is source of iron, and DEXTROSE ANHYDROUS is carbon source, sodium chloride as template,
Wherein the molar ratio of Co:Fe:C:NaCl is 0.5:1:20:150, and cobalt source, source of iron, carbon source and sodium chloride are dissolved in deionized water
In, uniform mixed solution is obtained by magnetic agitation, uniformly mixed solution is placed in refrigerator and is freezed, at freeze-drying
Reason obtains precursor powder.
(2) calcining of composite material precursor powder
Precursor powder prepared in step (1) is laid in Noah's ark, tube furnace flat-temperature zone is placed in and is calcined: being made with argon gas
For protective atmosphere, 600~650 DEG C are risen to the heating rate of 10 DEG C/min, keeps the temperature the carbonization for carrying out glucose for 2 hours and nitre
The decomposition of sour cobalt and ferric nitrate is cooled down with the rate of 5 DEG C/min after reaction, after being cooled to room temperature, obtains calcined product.
(3) removal of NaCl template
Calcined product obtained in collection step (2), is washed to until not having NaCl in product, finally dries in 80 DEG C of baking ovens
It is dry, obtain three-dimensional carbon network load cobalt ferrite nano particle composite material.
2. the three-dimensional carbon network load cobalt ferrite nano particle composite material is applied to electro-magnetic wave absorption.
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