CN108483508A - A kind of porous flake Fe3O4Electromagnetic wave absorption agent and preparation method thereof - Google Patents
A kind of porous flake Fe3O4Electromagnetic wave absorption agent and preparation method thereof Download PDFInfo
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- CN108483508A CN108483508A CN201810382761.6A CN201810382761A CN108483508A CN 108483508 A CN108483508 A CN 108483508A CN 201810382761 A CN201810382761 A CN 201810382761A CN 108483508 A CN108483508 A CN 108483508A
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- electromagnetic wave
- wave absorption
- absorption agent
- porous flake
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention discloses a kind of porous flake Fe3O4Electromagnetic wave absorption agent, the Fe3O4Electromagnetic wave absorption agent structure in the form of sheets has multiple pore structures in each laminated structure.The invention also discloses above-mentioned porous flake Fe3O4The preparation method of electromagnetic wave absorption agent.Porous flake Fe of the present invention3O4Electromagnetic wave absorption agent still has absorption intensity high under low thickness, the wide feature of effective absorption band, and excellent absorbing property is concentrated mainly on X and C-band；The preparation method of the present invention is simple for process, at low cost, without complicated synthesis device, it can be achieved that scale is produced in enormous quantities.
Description
Technical field
The present invention relates to a kind of porous flake Fe3O4Electromagnetic wave absorption agent further relates to above-mentioned porous flake Fe3O4Electromagnetic wave absorption
The preparation method of agent belongs to absorbing material technical field.
Background technology
In recent years, the high frequency wireless telecommunications system of fast development is brought greatly to daily life and Technological research
Facility.Meanwhile electromagenetic wave radiation causes huge do to the normal operation of living environment, human health and electronic equipment
It disturbs.In addition, in military field, stealth technology can improve the survival ability of target change system in practical operation, with country
Military capability of the country is closely linked.For this purpose, electromagnetic wave absorbent material is widely paid attention to and is ground in civil field and military field
Study carefully.Currently, absorbing material is broadly divided into dielectric loss and magnetic loss wave-absorber according to loss mechanism.Wherein magnetic loss wave-absorber with
Very important status is occupied in electro-magnetic wave absorption field by means of good impedance matching and magnetic loss ability.
Magnetic iron ore Fe3O4, as traditional ferromagnetic material because low cost, hypotoxicity and good bio-compatibility are being inhaled
Wave field has been widely used.For example, Beijing Institute of Technology Cao Maosheng professor seminar using the method for co-precipitation by Fe3O4
Nanoparticle deposition obtains Fe in carbon nanotube (MWCNTs)3O4/ MWCNTs composite materials, its effective electromagnetic wave at 3mm
Absorber Bandwidth is up to 11GHz (7-18GHz).(M.S.Cao,J.Yang,W.L.Song,D.Q.Zhang,B.Wen,H.B.Jin,
Z.L.Hou,J.Yuan,Ferroferric Oxide/Multiwalled Carbon Nanotube vs Polyaniline/
Ferroferric Oxide/Multiwalled Carbon Nanotube Multiheterostructures for
Highly Effective Microwave Absorption.ACS Appl.Mater.Interfaces 2012,4,6949-
6956).Harbin Institute of Technology Du Yunchen professors seminar passes through in N2Fe is calcined in atmosphere3O4It is obtained with phenolic resin compound
To Fe3O4@C microballoons, effective Absorber Bandwidth is up to 4.0 (12.9~17.8) GHz under 1.5mm thickness.(Y.C.Du,W.W.Liu,
R.Qiang,Y.Wang,X.J.Han,J.Ma,P.Xu.Shell thickness-dependent microwave
absorption of core–shell Fe3O4@C composites.ACS Appl.Mater.Interfaces 2014,6,
12997-13006.).However Fe in the prior art3O4Wave absorbing agent still remains this many deficiency:1.Fe3O4The performance of wave absorbing agent
It is concentrated mainly on Ku (12-18GHz) wave band, and radio communication and radar-frequency band mostly concentrate on X (8~12) and C (4
~8) wave band；2. preparation process is complicated, time-consuming, low yield, and of high cost；3. current Fe3O4Wave absorbing agent is mainly that binary is multiple
The performance study of condensation material, single component material needs further in-depth, and the still mould of the relationship between microstructure and electromagnetic parameter
Paste.
Invention content
Goal of the invention：Technical problem to be solved by the invention is to provide a kind of porous flake Fe3O4Electromagnetic wave absorption agent, should
The sheet porous structural of electromagnetic wave absorption agent makes it have low density and good dielectric properties.
The present invention also technical problems to be solved are to provide above-mentioned porous flake Fe3O4The preparation method of electromagnetic wave absorption agent, should
Preparation method can prepare the Fe of structure in the form of sheets3O4Electromagnetic wave absorption agent, and preparation process is simple, at low cost, can be suitable for
Industrialization large-scale production.
In order to solve the above technical problems, the technology used in the present invention means are：
A kind of porous flake Fe3O4Electromagnetic wave absorption agent, the Fe3O4Electromagnetic wave absorption agent structure in the form of sheets, each laminated structure
It is upper that there are multiple pore structures.
Wherein, a diameter of 4.7~6.0 μm of each laminated structure, thickness are 0.59~0.7 μm.
Wherein, the aperture of each pore structure is 10~110nm.
Above-mentioned porous flake Fe3O4The preparation method of electromagnetic wave absorption agent, specifically comprises the following steps：
Step 1, solvent-thermal method prepares α-Fe2O3：The desired amount of ferric acetyl acetonade is dissolved in triethylene glycol solvent, it is molten
Solution completely after, then toward suitable NaOH solution is added in mixed solution, obtain mixed material；Mixed material is placed in the anti-of sealing
It answers in container and keeps the temperature 4 hours at 200~220 DEG C, obtain head product；By head product after centrifuge washing, drying, forerunner is obtained
Body α-Fe2O3；
Step 2, presoma α-Fe step 1 obtained2O3It is dispersed in containing reducing agent NaBH4Aqueous solution in, mixed
Mixture is placed in the reaction vessel of sealing after complete and keeps the temperature 12 hours at 160~170 DEG C, initial product is obtained, after reaction
Obtained initial product is subjected to dipping magnetic inclination analysis separation, obtains porous flake Fe3O4Electromagnetic wave absorption agent.
Wherein, in step 1, the volume of the triethylene glycol solvent is 40~60mL, and the addition of ferric acetyl acetonade is
The addition volume of 0.6g, NaOH solution are 2~20mL.
Wherein, a concentration of 6mol/L of the NaOH solution.
Compared with the prior art, technical solution of the present invention have the advantage that for：
Porous flake Fe of the present invention3O4Electromagnetic wave absorption agent is compared to traditional Fe3O4Absorbing material and Fe3O4Based composites
With absorption intensity height, the wide feature of effective absorption band under low thickness, and excellent absorbing property is concentrated mainly on X and C
Wave band；The preparation method of the present invention is simple for process, at low cost, without complicated synthesis device, it can be achieved that scale high-volume is raw
Production.
Description of the drawings
Fig. 1 is Fe made from the embodiment of the present invention 1,2,33O4The X ray diffracting spectrum of electromagnetic wave absorption agent；
Fig. 2 is Fe made from the embodiment of the present invention 13O4- 2 SEM photograph；
Fig. 3 is Fe made from the embodiment of the present invention 23O4- 10 SEM photograph；
Fig. 4 is Fe made from the embodiment of the present invention 33O4- 20 SEM photograph；
Fig. 5 is Fe made from the embodiment of the present invention 13O4- 2 reflection loss collection of illustrative plates；
Fig. 6 is Fe made from the embodiment of the present invention 23O4- 10 reflection loss collection of illustrative plates；
Fig. 7 is Fe made from the embodiment of the present invention 33O4- 20 reflection loss collection of illustrative plates；
Fig. 8 is Fe made from the embodiment of the present invention 23O4- 10 Effective frequency width of absorption figure.
Specific implementation mode
Technical scheme of the present invention is described further below in conjunction with the drawings and specific embodiments.
Porous flake Fe of the present invention3O4Electromagnetic wave absorption agent structure in the form of sheets has multiple pore structures in each laminated structure,
The electromagnetic wave absorption agent first uses solvent-thermal method to prepare α-Fe2O3, recycle NaBH4Reduction method prepares porous flake Fe3O4Electromagnetism is inhaled
Wave agent.
Embodiment 1
Porous flake Fe of the present invention3O4The preparation method of electromagnetic wave absorption agent, includes the following steps：
Step 1, solvent-thermal method prepares α-Fe2O3：0.6g ferric acetyl acetonades, dissolving are added in 60mL triethylene glycol solvents
After completely, then toward the NaOH solution (providing alkaline environment) of a concentration of 6mol/L of addition 2mL in mixed solution, continue to stir 1h
Afterwards, mixed material is obtained；Mixed material is sealed in reaction kettle, 4h is kept the temperature under the conditions of 200 DEG C, obtains head product；It will be first
Product obtains presoma α-Fe after centrifuge washing, drying2O3；Labeled as α-Fe2O3-2；Obtained presoma α-Fe2O3- 2
In porous laminated structure, only laminated structure is than relatively thin；
Step 2,0.1g presoma α-Fe step 1 obtained2O3It is dispersed in 30mL distilled water, then in distilled water
Add 10mmol NaBH4, after ultrasonic 15min, mixed material is sealed in reaction kettle, 12 hours are kept the temperature at 160 DEG C,
Up to final product after natural cooling, it is labeled as Fe3O4- 2, due to presoma α-Fe2O3- 2 laminated structures are than relatively thin, because before this
It drives body plate shape structure and has been destroyed after reduction and become graininess.
Embodiment 2
Porous flake Fe of the present invention3O4The preparation method of electromagnetic wave absorption agent, includes the following steps：
Step 1, solvent-thermal method prepares α-Fe2O3：0.6g ferric acetyl acetonades, dissolving are added in 50mL triethylene glycol solvents
After completely, then toward the NaOH solution of a concentration of 6mol/L of addition 10mL in mixed solution, continues after stirring 1h, obtain mixture
Material；Mixed material is sealed in reaction kettle, 4h is kept the temperature under the conditions of 200 DEG C, obtains head product；Head product is washed through centrifugation
After washing, drying, presoma α-Fe are obtained2O3；Labeled as α-Fe2O3-10；Obtained presoma α-Fe2O3- 10 be also in porous flake
Structure, and laminated structure thickness is moderate；
Step 2,0.1g presoma α-Fe step 1 obtained2O3It is dispersed in 30mL distilled water, then into distilled water
Add 10mmolNaBH4, after ultrasonic 15min, mixed material is sealed in reaction kettle, 12 hours are kept the temperature at 160 DEG C, from
So Fe is labeled as up to final product after cooling3O4- 10, due to presoma α-Fe2O3- 10 laminated structure thickness are thick, because before this
It is still porous laminated structure after reduction to drive body plate shape structure.
Embodiment 3
Porous flake Fe of the present invention3O4The preparation method of electromagnetic wave absorption agent, includes the following steps：
Step 1, solvent-thermal method prepares α-Fe2O3：0.6g ferric acetyl acetonades, dissolving are added in 40mL triethylene glycol solvents
After completely, then toward the NaOH solution of a concentration of 6mol/L of addition 20mL in mixed solution, continues after stirring 1h, obtain mixture
Material；Mixed material is sealed in reaction kettle, 4h is kept the temperature under the conditions of 200 DEG C, obtains head product；Head product is washed through centrifugation
After washing, drying, presoma α-Fe are obtained2O3；Labeled as α-Fe2O3-20；
Step 2,0.1g presoma α-Fe step 1 obtained2O3It is dispersed in 30mL distilled water, then into distilled water
Add 10mmolNaBH4, after ultrasonic 15min, mixed material is sealed in reaction kettle, 12 hours are kept the temperature at 160 DEG C, from
So Fe is labeled as up to final product after cooling3O4-10。
Fig. 1 is Fe made from the embodiment of the present invention 1,2,33O4The X ray diffracting spectrum of electromagnetic wave absorption agent, can from Fig. 1
Go out, wherein only Fe3O4Characteristic peak, final product group known to Binding experiment principle becomes Fe3O4。
Fig. 2 is Fe made from the embodiment of the present invention 13O4- 2 SEM photograph, figure it is seen that presoma laminated structure
Substantially it is destroyed, and forms many irregular particles.
Fig. 3 is Fe made from the embodiment of the present invention 23O4- 10 SEM photograph, from figure 3, it can be seen that higher in NaOH content
Under conditions of Fe3O4The structure of porous flake is formd, the diameter of laminated structure is about 4.70 μm, and thickness is about 0.59 μm.
Fig. 4 is Fe made from the embodiment of the present invention 33O4- 20 SEM photograph, with the further raising of NaOH content, piece
It is 6.0 μm that the diameter of shape structure, which increases, and it is 0.7 μm that thickness, which increases, illustrates that the increase of NaOH content is conducive to Fe3O4Laminated structure
Growth.
Fig. 5 is Fe made from the embodiment of the present invention 13O4- 2 reflection loss collection of illustrative plates, from fig. 5, it can be seen that embodiment 1 is made
The Fe obtained3O4Its absorbing property of -2 absorbing materials is poor, best reflection loss value deficiency -14dB and the frequency bandwidth less than -10dB
Only 2.3GHz.
Fig. 6 is Fe made from the embodiment of the present invention 23O4- 10 reflection loss collection of illustrative plates, from fig. 6, it can be seen that embodiment 2 is made
The Fe obtained3O4- 10 absorbing materials show excellent absorbing property.At 2.05 thickness mm, reflection loss value can reach-
49.0dB；At 2.25 thickness mm, the frequency bandwidth less than -10dB is 4.32 (7.52~11.84) GHz.Thus illustrate, it is porous
The generation of laminated structure is conducive to improve the electromagnetic wave absorption performance of material.
Fig. 7 is Fe made from the embodiment of the present invention 33O4- 20 reflection loss collection of illustrative plates, from figure 7 it can be seen that at this point, product
Absorbing property is between Fe3O4- 2 and Fe3O4Between -10.Reflection loss value is up to -27dB and less than -10dB's under 1.85 thickness mm
Frequency bandwidth is 3.0GHz.
Fig. 8 is Fe made from the embodiment of the present invention 23O4- 10 Effective frequency width of absorption figure, from figure 8, it is seen that working as coating
For thickness between 2.05 and 3.05mm, Effective frequency width of absorption (RL≤- 10dB) can almost cover entire C-band and X-band.
Currently, traditional graininess Fe3O4Electromagnetic wave absorption agent, in low-frequency band, absorbing property cannot meet under low thickness (≤3mm)
Reach wider effective absorption band (>=4GHz).So the Fe of sheet porous structural of the present invention3O4Electromagnetic wave absorption agent can be used as excellent
Different low-frequency electromagnetic wave absorbing material.In addition, prior art granular Fe3O4Not only absorbing property is not so good as this for electromagnetic wave absorption agent
The Fe of invention porous flake3O4Electromagnetic wave absorption agent, and wherein also contain other carbon fiber impurity, and the porous flake of the present invention
Fe3O4Electromagnetic wave absorption agent only has the Fe of laminated structure3O4。
Porous flake Fe of the present invention3O4Electromagnetic wave absorption agent first uses a step solvent structure α-Fe2O3Presoma, then
Reducing agent NaBH4Under the action of, by presoma α-Fe2O3It is reduced to the Fe with porous laminated structure3O4.The porous flake of synthesis
Structure is conducive to improve the dielectric property of material, enhances its impedance matching property and interfacial polarization loss, while pore structure is deposited
In the density for advantageously reducing wave absorbing agent.
Claims (8)
1. a kind of porous flake Fe3O4Electromagnetic wave absorption agent, it is characterised in that：The Fe3O4Electromagnetic wave absorption agent structure in the form of sheets, each
There are multiple pore structures in laminated structure.
2. porous flake Fe according to claim 13O4Electromagnetic wave absorption agent, it is characterised in that：The diameter of each laminated structure
It it is 4.7~6.0 μm, thickness is 0.59~0.7 μm.
3. porous flake Fe according to claim 13O4Electromagnetic wave absorption agent, it is characterised in that：The aperture of pore structure be 10~
110nm。
4. a kind of porous flake Fe described in claim 13O4The preparation method of electromagnetic wave absorption agent, which is characterized in that include specifically
Following steps：
Step 1, solvent-thermal method prepares α-Fe2O3：The desired amount of ferric acetyl acetonade is dissolved in triethylene glycol solvent, has been dissolved
Quan Hou, then toward suitable NaOH solution is added in mixed solution, obtain mixed material；The reaction that mixed material is placed in sealing is held
In device at 200~220 DEG C held for some time, obtain head product；By head product after centrifuge washing, drying, forerunner is obtained
Body α-Fe2O3；
Step 2, presoma α-Fe step 1 obtained2O3It is dispersed in containing reducing agent NaBH4Aqueous solution in, mixing completely after
Mixture is placed in in the reaction vessel of sealing the held for some time at 160~170 DEG C, obtains initial product, it will after reaction
Obtained initial product carries out dipping magnetic inclination analysis separation, obtains porous flake Fe3O4Electromagnetic wave absorption agent.
5. porous flake Fe according to claim 43O4The preparation method of electromagnetic wave absorption agent, it is characterised in that：In step 1,
The volume of the triethylene glycol solvent is 40~60mL, and the addition of ferric acetyl acetonade is 0.6g, the addition volume of NaOH solution
For 2~20mL.
6. porous flake Fe according to claim 53O4The preparation method of electromagnetic wave absorption agent, it is characterised in that：The NaOH
A concentration of 6mol/L of solution.
7. porous flake Fe according to claim 43O4The preparation method of electromagnetic wave absorption agent, it is characterised in that：In step 1,
The soaking time is 4h.
8. porous flake Fe according to claim 43O4The preparation method of electromagnetic wave absorption agent, it is characterised in that：In step 2,
The soaking time is 12h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518454A (en) * | 2020-05-28 | 2020-08-11 | 北京环境特性研究所 | Composition and method for preparing C-band electromagnetic functional coating |
Citations (2)
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| CN102001712A (en) * | 2010-12-16 | 2011-04-06 | 苏州康立达纳米生物工程有限公司 | Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template |
| CN103723773A (en) * | 2012-10-16 | 2014-04-16 | 国家纳米科学中心 | Hydrosol of ferroferric oxide nanoparticles and preparation method and application thereof |
-
2018
- 2018-04-25 CN CN201810382761.6A patent/CN108483508B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001712A (en) * | 2010-12-16 | 2011-04-06 | 苏州康立达纳米生物工程有限公司 | Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template |
| CN103723773A (en) * | 2012-10-16 | 2014-04-16 | 国家纳米科学中心 | Hydrosol of ferroferric oxide nanoparticles and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| ANDRIS ŠUTKA ET AL.: ""Precipitation synthesis of magnetite Fe3O4 nanoflakes"", 《CERAMICS INTERNATIONAL》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518454A (en) * | 2020-05-28 | 2020-08-11 | 北京环境特性研究所 | Composition and method for preparing C-band electromagnetic functional coating |
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Effective date of registration: 20220906 Address after: No. 29, Hongshan Road, Jincheng Town, Jintan District, Changzhou City, Jiangsu Province 213251 Patentee after: CHANGZHOU WEISI SHUANGLIAN TECHNOLOGY CO.,LTD. Address before: No. 29, Qinhuai District, Qinhuai District, Nanjing, Jiangsu Patentee before: Nanjing University of Aeronautics and Astronautics |