CN106520071A - Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof - Google Patents
Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a rice husk based C/magnetic Co particle composite wave absorber and a preparation method thereof and belongs to the technical field of wave absorbing materials. Magnetic Co particles of the rice husk based C/magnetic Co particle composite wave absorber are 1.3 mu m in size, and rice husk based C also has a porous structure. The preparation method of the composite wave absorber comprises three steps: pretreatment: rice husk is washed with purified water and treated with HF (hydrofluoric acid), Si compounds in the rice husk are removed through etching, and the rice husk treated with the HF is obtained after drying; modification: the rice husk treated with the HF is soaked in a CoCl2 aqueous solution, water is removed through reduced-pressure distillation, and CoCl2 modified rice husk is obtained; carbonization: the CoCl2 modified rice husk is placed in a tube furnace and carbonized at a high temperature in an inert gas atmosphere, the carbonized material is further ground, and the rice husk based C/magnetic Co particle composite wave absorber is obtained. The prepared wave absorber has excellent wave absorbing performance and shows stronger absorbing characteristic on electromagnetic waves.
Description
Technical field
The invention belongs to absorbing material technical field, more particularly to a kind of rice husk base carbon/magnetic Co particle composite wave-absorbing
Agent and preparation method thereof.
Background technology
The fast development of electronics industry so that electromagnetic pollution in recent years becomes to be on the rise, and absorbing material is dirty in electromagnetism
Dye protection and electromagnetic attenuation field serve vital effect.Simultaneously in the stealthy field of military target, absorbing material
Also vital effect has been played, can have effectively ensured the safety of the military targets such as target aircraft.Absorbing material, also known as
Make microwave absorbing material or electromagnetic wave attenuation material, can more efficiently reduce reflection of the incident electromagnetic wave in body surface,
Electromagnetic wave is enabled effectively to enter to inject the inside of material, so as to pass through the dielectric loss and magnetic loss of absorbing material itself
Characteristic is quickly decayed, and reaches the purpose of electromagnetic wave absorption.Absorbing material can be divided into two parts according to its composition：A part
It is the matrix for playing cementation, is usually the resin material that some have good wave transparent and thermal stability；Another portion
It is wave absorbing agent to divide, and as the main body of absorbing material, primarily serves the effect of electromagnetic consumable.Therefore, the excellent suction ripple of processability
Agent is the premise for preparing absorbing material.Outstanding wave absorbing agent material should have that lightweight, absorption intensity are big, loss ability is strong, system concurrently
Standby simple process and the characteristic such as cheap.
According to transmission line theory (Qin, the F. in electromagnetic wave field；Brosseau,C.,J.Appl.Phys.2012,111,
061301), the wave absorbing agent material of one-component, such as single dielectric loss material or magnetic loss consumption material, due to being often difficult to
The characteristic of preferable electromagnetic matching is realized, so the inside that electromagnetic wave is difficult to effectively enter material is depleted, absorbing property is past
Toward relatively limited, it has been difficult to meet the characteristics such as efficient, lightweight and wideband.Therefore, prepare and have electricity, magnetic loss one concurrently and answer
Mould assembly wave absorbing agent is the study hotspot in absorbing material field.Dielectric loss component is effectively combined with magnetic loss component, a side
Face can solve the problems, such as electromagnetic matching so that electromagnetic wave can be efficiently entering inside absorbing material, and on the other hand various losses are special
Property combination, enable to quickly be lost into the electromagnetic wave for injecting material internal, so as to reaching low reflection, strong absorbing
Characteristic.Material with carbon element, with good chemical stability, high mechanical strength and outstanding electric conductivity, while heat stability is excellent
Different, density of material is less.Therefore, material with carbon element has larger potentiality preparing outstanding wave absorbing agent field.Meanwhile, using certain
Means, the magnetic particle with magnetic loss ability is combined with material with carbon element, carbon/magnetic particle composite wave-absorbing agent is prepared, is expected to
The rapid deterioration to electromagnetic wave is realized, excellent absorbing property is obtained.
Rice husk contains abundant carbon, at the same as agricultural industry a kind of garbage often by direct burning disposal,
Price is more cheap, is a kind of cheap carbon source material.But, the modification of the further magnetic component of rice husk Carbon Materials often compared with
For complexity, so the research of rice husk base carbon wave absorbing agent is more short of.Therefore, design certain method of modifying, by magnetic particle with
Rice husk base carbon is effectively combined, and is expected to obtain a kind of rice husk base wave absorbing agent material of excellent performance.
The content of the invention
The invention mainly solves the technical problem of there is provided a kind of excellent rice husk base carbon/magnetic Co particle of absorbing property
Composite wave-absorbing agent and preparation method thereof.The present invention makes full use of the construction featuress of rice husk composition, devises a kind of pretreatment modification
The method of magnetic particle, prepares rice husk base carbon/magnetic Co particle composite wave-absorbing agent material.The preparation technology letter of the composite wave-absorbing agent
Just, it is easy to practical operation, it is easy to industrialized production.Meanwhile, the Absorbing Materials of preparation are stronger, have wider suction wave frequency concurrently
The characteristics such as band, less matching thickness, future have larger application potential in absorbing material field.
In the present invention, with rice husk as raw material, successively the process such as experience etching, modification, carbonization and grinding, obtains
Rice husk base carbon/magnetic particle composite wave-absorbing agent.The wave absorbing agent absorbing property of preparation is excellent, shows the suction stronger to electromagnetic wave
Receive characteristic.When the thickness of absorbing material is 1.8mm, its maximum reflection loss has reached -40.1dB (more than 99.99%
Absorb).Simultaneously by adjusting the thickness of absorbing material, it is possible to achieve to electromagnetic wave 3.9-18GHz frequency ranges (C-band, X-band and
KuWave band) more than the absorption of -10dB.
Rice husk base carbon provided by the present invention/magnetic Co particle composite wave-absorbing agent material, magnetic Co particle size are 1.3 μ
M, while rice husk base carbon has loose structure concurrently.The preparation process of composite wave-absorbing agent material is divided into three below step：Pretreatment, will
Rice husk is cleaned using pure water, and then using Fluohydric acid. (HF) process, etching removes the silicon-containing compound in rice husk, after being dried
To the rice husk of HF process；The rice husk of HF process is placed in CoCl by modification2Aqueous solution in, immersion, and by vacuum distillation removing
Water, obtains CoCl2The rice husk of modification；Carbonization, by CoCl2The rice husk of modification is placed in tube furnace, in atmosphere of inert gases, high
Temperature carbonization, the material after carbonization are further ground and obtain rice husk base/magnetic Co particle composite wave-absorbing agent material.
The preparation method of rice husk base carbon of the present invention/magnetic Co particle composite wave-absorbing agent material, its specific synthesis
Step is as follows：
(1) rice husk is removed into the impurity such as the dust on rice husk surface using distilled water wash 3～5 times；After drying, by rice husk
It is placed in the hydrofluoric acid aqueous solution of mass fraction 20～40%, stirring 8～12h of etching, in centrifugation (1000～3000rpm) removing
Clear liquid；Then centrifugation product is washed into 2～4 times with the hydrofluoric acid aqueous solution of mass fraction 20～40%, centrifugation；Again will be from
Heart product distilled water wash 2～4 times, centrifugation；Centrifugation product is dried into 8～12h at 60～100 DEG C finally, is obtained
The rice husk of hydrofluoric acid treatment；
(2) six chloride hydrate of the rice husk of the hydrofluoric acid treatment that 2.5～3.5g steps (1) are obtained and 12.5～17.5mmol
Cobalt CoCl2·6H2O is added in 40～80mL distilled water, is stirred and is standing and soak for 8～12h again after cobalt chloride hexahydrate dissolving,
Then vacuum distillation removes distilled water, is finally dried 8～12h at 100～140 DEG C, obtains the rice husk of cobaltous chloride modification；
(3) rice husk of the cobaltous chloride modification for obtaining step (2) be carbonized under the conditions of 900～1100 DEG C 1～3h, finally general
Carbonized product grinds, so as to obtain rice husk base carbon of the present invention/magnetic Co particle composite wave-absorbing agent material.
The rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared using the present invention, further based on paraffin,
The absorbing material of different wave absorbing agent loadings can be prepared, the method which is prepared is as follows：
(1) by paraffin and rice husk base carbon/magnetic Co particle composite wave-absorbing agent mixing, wherein composite wave-absorbing agent/(composite wave-absorbing
Agent+paraffin) mass percent be 15%～35%；
(2) by the mixture of the wave absorbing agent of upper step and paraffin by mould using hydraulic press be suppressed into external diameter be 7mm,
Test annulus of the internal diameter for 3mm；
(3) electromagnetic parameter of the above-mentioned prepared sample in the range of 2～18GHz is tested using Agilent N5244A PNA-X
(ε ', ε ", μ ', μ ") calculate reflection loss RL (Lu Shaowei, Li Qian, Xiong Xuhai, the horse of the composite wave-absorbing agent using following formula
Gram bright, Xu Weikai, Jia Caixia, Journal of Inorganic Materials, 2015,30,23-28).
In formula：Z0It is free space impedance；μ0、ε0It is permeability of vacuum and dielectric constant, ε0=8.854187817 × 10-12F/m, μ0=4 π × 10-7H/m；ZinIt is the input impedance (", μ ', μ " is obtained by data calculation using ε ', ε) of absorbing material；F is
The frequency (scope is 2～18GHz) of electromagnetic wave；D is the thickness of absorbing material；C is spread speed of the electromagnetic wave in free space,
Equal to the light velocity 3 × 108m/s；εr(εr=ε '-j ε ") and μr(μr=μ '-j μ ") is that the equivalent relative complex dielectric of absorbing material is normal
Number and complex permeability, j are the imaginary part unit of complex dielectric constant and complex permeability, without practical significance.Experiment can be measured
ε ', ε of the material under different wave frequency f ", μ ', μ ".
Description of the drawings
Fig. 1：The schematic arrangement of rice husk main component lignin and cellulose；
Fig. 2：The XRD spectra of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared by embodiment 1.
Fig. 3：The stereoscan photograph of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared by embodiment 1.
Fig. 4：The stereoscan photograph of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared by embodiment 2.
Fig. 5：The stereoscan photograph of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared by embodiment 3.
Fig. 6：The rice husk base carbon prepared in the embodiment 1/later scanning of magnetic Co particle composite wave-absorbing agent experience grinding
Electromicroscopic photograph.
Fig. 7：The transmission electron microscope photo of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared by embodiment 1.
Fig. 8：The electromagnetic parameter curve of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared by embodiment 1.
Fig. 9：The electromagnetic parameters of the rice husk base carbon/magnetic Co particle composite wave-absorbing agent material tested using embodiment 2
The reflection loss RL datagrams for obtaining.
Fig. 1 gives the schematic arrangement of main component lignin and cellulose in rice husk.As can be seen from the figure
In the structure of lignin and cellulose, with substantial amounts of oh group, the presence of these oh groups so that rice husk with compared with
Strong water absorption character.The present invention exactly utilizes this characteristic, rice husk is removed silicon-containing compound using hf etching first, then
Further processed using the aqueous solution of cobaltous chloride.Due to the water absorption character of rice husk, the aqueous solution of cobaltous chloride can be entered into
The inside of rice husk, in subsequent carbonisation, cobaltous chloride is reduced to metallic cobalt simple substance, is filled in the inside of rice husk base carbon,
So as to obtain rice husk base carbon/magnetic Co particle composite wave-absorbing agent material.
Fig. 2 gives the XRD spectra of the rice husk base carbon/magnetic Co particle composite wave-absorbing agent material of the preparation of embodiment 1.By
XRD is characterized and is understood, after experience high temperature cabonization is processed, cobaltous chloride is reduced to cobalt simple substance, is that rice husk base carbon brings magnetic loss
Component.
Fig. 3 gives the scanning electron microscope of the rice husk base carbon/magnetic Co particle composite wave-absorbing agent material of the preparation of embodiment 1 and shines
Piece.Knowable in stereoscan photograph, magnetic cobalt particle is more uniformly dispersed in rice hull carbon.Also, magnetic cobalt particle
Size at 1.3 μm or so, be embedded in the inside of rice husk carbon.Additionally, rice husk carbon has certain loose structure, this loose structure
It is capable of the quality of effective lightening material, while loose structure can strengthen reflection of the electromagnetic wave inside absorbing material so as to increase
The contact probability of power-up magnetic wave and wave absorbing agent so that electromagnetic wave quickly can be lost.
The scanning electron microscope of the rice husk base carbon that Fig. 4 is prepared in giving embodiment 2/magnetic Co particle composite wave-absorbing agent material shines
Piece.
The scanning electron microscope of the rice husk base carbon that Fig. 5 is prepared in giving embodiment 3/magnetic Co particle composite wave-absorbing agent material shines
Piece.
The rice husk base carbon that Fig. 6 is prepared in giving embodiment 1/magnetic Co particle composite wave-absorbing agent experience grinding is later
Stereoscan photograph.As seen from the figure, after the wave absorbing agent experience grinding of preparation, the size of granule is below 150 μm.
The transmission electron microscope of the rice husk base carbon that Fig. 7 is prepared in giving embodiment 1/magnetic Co particle composite wave-absorbing agent material shines
Piece.The sign of transmission electron microscope further demonstrates the size and dispersing characteristic of magnetic cobalt particle.
Fig. 8 gives the survey that the rice husk base carbon/magnetic Co particle composite wave-absorbing agent of the preparation of embodiment 1 is mixed with paraffin
The electromagnetic parameter of test agent.As the real part and imaginary part of electromagnetic parameter medium dielectric constant microwave medium and pcrmeability represent material pair respectively
The storage capacity of the energy of electromagnetic field and loss ability, so the rice husk base carbon/magnetic Co particle composite wave-absorbing agent material for preparing
With relatively strong dielectric loss ability and magnetic loss ability.For the electromagnetic wave of low frequency has stronger dielectric loss energy
Power, and for the electromagnetic wave of high frequency also shows stronger magnetic loss ability.
The reflection loss number of the rice husk base carbon that Fig. 9 is prepared in giving embodiment 1/magnetic Co particle composite wave-absorbing agent material
According to.Rice husk base carbon/magnetic Co particle composite wave-absorbing agent material shows excellent loss characteristic to electromagnetic wave, works as absorbing material
Thickness (thickness here is not a concept with the thickness in embodiment 4 when being 1.8mm.Thickness in embodiment 4 is to survey
The thickness of the sample prepared when the electromagnetic parameter of examination material, this thickness are to combine formula using electromagnetic parameter to calculate material
The assignment of d when reflection loss), the loss of the maximum for electromagnetic wave is realized, reflection loss has reached -40.1dB.Simultaneously
By the thickness for adjusting absorbing material, when thickness changes between 1.1～4.0mm, material can show to 3.9～
The stronger absorbability (reflection loss RL≤- 10dB) of the electromagnetic wave of 18GHz.Therefore the rice husk base carbon/magnetic Co particle for preparing
Composite wave-absorbing agent material has stronger electromagnetic consumable ability.In the present invention using the construction featuress of rice husk composition, employing
Pretreatment modification prepares the method for rice husk base carbon/magnetic Co particle composite wave-absorbing agent material can improve the suction of rice husk base material with carbon element
Ripple performance, provides certain technological means to prepare high-performance wave-absorbing material, with potential using value.
Specific embodiment
Embodiment 1
The synthetic method of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material that the present invention is provided, can be by following anti-
Step is answered to realize：
(1) rice husk (10.0g) is removed into the impurity such as the dust on rice husk surface using distilled water wash 3 times.After drying, will
Rice husk is placed in the plastic containers containing hydrofluoric acid aqueous solution (mass fraction 30%), stirring etching 10h, is centrifuged (2000rpm)
Supernatant is removed, then centrifugation product is washed 3 times using hydrofluoric acid aqueous solution (mass fraction 20%), centrifugation；Then from
Heart product is using distilled water wash 3 times, centrifugation；Finally centrifugation product is placed in baking oven, 80 DEG C are dried 10h, obtain hydrogen fluorine
The rice husk 7.6g of acid treatment.
(2) rice husk of 3.0g hydrofluoric acid treatment is added in the single necked round bottom flask of 250mL, six hydrations of 15mmol are added
Cobaltous chloride CoCl2·6H2O, adds 50mL distilled water, stirs after cobalt chloride hexahydrate dissolving, is standing and soak for 10h, and decompression is steamed
Distilled water is removed in distillation.The rice husk that cobaltous chloride is modified is placed in baking oven, 120 DEG C of dried 10h obtain product 4.6g.
(3) rice husk of cobaltous chloride process is placed in porcelain crucible, is transferred in high temperature process furnances, 1000 DEG C of process 2h (journeys
Sequence heats up：20～1000 DEG C, 5 DEG C/min, 196min；1000 DEG C, 120min；1000～100 DEG C, 5 DEG C/min, 180min).Carbon
Product after change, further mechanical lapping (this did not test specific mesh number, but the size of granule 150 μm with
Under), rice husk base carbon/magnetic Co particle composite wave-absorbing agent material is obtained, product 2.4g is obtained.
Embodiment 2
The synthetic method of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material that the present invention is provided, can be by following anti-
Step is answered to realize：
(1) the rice husk 2.5g of hydrofluoric acid treatment in 1 step of embodiment (1) is added in the single necked round bottom flask of 250mL, plus
Enter the cobalt chloride hexahydrate CoCl of 15mmol2·6H2O, adds 50mL distilled water, stirs after cobalt chloride hexahydrate dissolving, quiet
Immersion 10h is put, vacuum distillation removes distilled water.The rice husk that cobaltous chloride is modified is placed in baking oven, 120 DEG C of dried 10h are obtained
Product 4.0g.
(2) rice husk of cobaltous chloride process is placed in porcelain crucible, is transferred in high temperature process furnances, 1000 DEG C of process 2h (journeys
Sequence heats up：20～1000 DEG C, 5 DEG C/min, 196min；1000 DEG C, 120min；1000～100 DEG C, 5 DEG C/min, 180min).Carbon
Product after change, further mechanical lapping obtain rice husk base carbon/magnetic Co particle composite wave-absorbing agent material, obtain product 1.8g.
Embodiment 3
The synthetic method of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material that the present invention is provided, can be by following anti-
Step is answered to realize：
(1) the rice husk 3.2g of hydrofluoric acid treatment in 1 step of embodiment (1) is added in the single necked round bottom flask of 250mL, plus
Enter the cobalt chloride hexahydrate CoCl of 17mmol2·6H2O, adds 50mL distilled water, stirs after cobalt chloride hexahydrate dissolving, quiet
Immersion 10h is put, vacuum distillation removes distilled water.The rice husk that cobaltous chloride is modified is placed in baking oven, 120 DEG C of dried 10h are obtained
Product 5.1g.
(2) rice husk of cobaltous chloride process is placed in porcelain crucible, is transferred in high temperature process furnances, 1000 DEG C of process 2h (journeys
Sequence heats up：20～1000 DEG C, 5 DEG C/min, 196min；1000 DEG C, 120min；1000～100 DEG C, 5 DEG C/min, 180min).Carbon
Product after change, further mechanical lapping obtain rice husk base carbon/magnetic Co particle composite wave-absorbing agent material, obtain product 2.6g.
Embodiment 4：
The application of the rice husk base carbon/magnetic Co particle composite wave-absorbing agent material prepared as the present invention, based on paraffin,
Rice husk base carbon/magnetic Co particle composite material is prepared using in embodiment 1 as wave absorbing agent, wave absorbing agent loading is prepared for for 25%
Test sample, can be realized by following steps：
(1) paraffin and rice husk base carbon/magnetic Co particle composite wave-absorbing agent material are mixed according to certain mass ratio；Its
The mass percent of middle wave absorbing agent/(wave absorbing agent+paraffin) is 25%；
(2) by the mixture of the wave absorbing agent of upper step and paraffin by mould using hydraulic press be suppressed into external diameter be 7mm,
The test annulus that internal diameter is 3.04mm, thickness is 2mm；
(3) electromagnetic parameter of the above-mentioned prepared sample in the range of 2～18GHz is tested using Agilent N5244A PNA-X
(ε ', ε ", μ ', μ ") calculate the reflection loss RL of the composite wave-absorbing agent using formula.
Claims (3)
1. the preparation method of a kind of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material, its step are as follows：
(1) rice husk is removed into the impurity on rice husk surface using distilled water wash 3～5 times；After drying, rice husk is placed in into quality point
In the hydrofluoric acid aqueous solution of number 20～40%, stirring 8～12h of etching is centrifuged off supernatant；Then by centrifugation product quality
The hydrofluoric acid aqueous solution of fraction 20～40% is washed 2～4 times, centrifugation；Again will centrifugation product distilled water wash 2～4 times,
Centrifugation；Centrifugation product is dried into 8～12h at 60～100 DEG C finally, the rice husk of hydrofluoric acid treatment is obtained；
(2) rice husk and 12.5～17.5mmol cobalt chloride hexahydrates of the hydrofluoric acid treatment that 2.5～3.5g steps (1) are obtained
CoCl2·6H2O is added in 40～80mL distilled water, is stirred and is standing and soak for 8～12h again after cobalt chloride hexahydrate dissolving, so
Vacuum distillation afterwards removes distilled water, is finally dried 8～12h at 100～140 DEG C, obtains the rice husk of cobaltous chloride modification；
(3) rice husk of the cobaltous chloride modification for obtaining step (2) be carbonized under the conditions of 900～1100 DEG C 1～3h, will finally be carbonized
Product grinds, so as to obtain rice husk base carbon/magnetic Co particle composite wave-absorbing agent material.
2. a kind of rice husk base carbon/magnetic Co particle composite wave-absorbing agent material, it is characterised in that：It is by the side described in claim 1
Method is prepared.
3. a kind of absorbing material of different wave absorbing agent loadings, it is characterised in that：It is by the rice husk described in paraffin and claim 2
Base carbon/magnetic Co particle composite wave-absorbing agent mixes, and the mass percent of wherein composite wave-absorbing agent/(composite wave-absorbing agent+paraffin) is
15%～35%.
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| CN113453524A (en) * | 2021-04-23 | 2021-09-28 | 中南林业科技大学 | Magnetic metal composite material based on bamboo-wood three-dimensional hole frame and preparation method and application thereof |
| CN113423254A (en) * | 2021-05-26 | 2021-09-21 | 西安理工大学 | Composite wave absorbing agent with electromagnetic wave absorbing performance and preparation method thereof |
| CN113891647A (en) * | 2021-11-22 | 2022-01-04 | 江苏科技大学 | Porous rice hull carbon/double transition metal sulfide nanoparticle composite wave-absorbing material and preparation method thereof |
| CN114806255A (en) * | 2022-04-08 | 2022-07-29 | 江苏科技大学 | Magnetic composite wave-absorbing material based on industrial waste rice hull carbon and preparation method thereof |
| CN115305055A (en) * | 2022-08-03 | 2022-11-08 | 浙江大学 | Biomass-derived electromagnetic functional material and preparation method thereof |
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