CN111704115A - A granular α -Fe2O3Preparation of Fe having microwave absorbing Properties4Method of N - Google Patents
A granular α -Fe2O3Preparation of Fe having microwave absorbing Properties4Method of N Download PDFInfo
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- CN111704115A CN111704115A CN202010477013.3A CN202010477013A CN111704115A CN 111704115 A CN111704115 A CN 111704115A CN 202010477013 A CN202010477013 A CN 202010477013A CN 111704115 A CN111704115 A CN 111704115A
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 229910000727 Fe4N Inorganic materials 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229940045348 brown mixture Drugs 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- YYXHRUSBEPGBCD-UHFFFAOYSA-N azanylidyneiron Chemical compound [N].[Fe] YYXHRUSBEPGBCD-UHFFFAOYSA-N 0.000 abstract description 11
- 229910017464 nitrogen compound Inorganic materials 0.000 abstract description 9
- 239000011358 absorbing material Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 238000012512 characterization method Methods 0.000 abstract description 2
- 238000011056 performance test Methods 0.000 abstract description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 235000017281 sodium acetate Nutrition 0.000 abstract 1
- 239000001632 sodium acetate Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 238000005121 nitriding Methods 0.000 description 5
- 229910000859 α-Fe Inorganic materials 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0622—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with iron, cobalt or nickel
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2006/42—Magnetic properties
Abstract
The invention provides a granular α -Fe2O3Preparation of Fe having microwave absorbing Properties4The method uses ferric chloride hexahydrate, sodium acetate, ethylene glycol and the like as main raw materials and adopts a hydrothermal method to synthesize granular α -Fe2O3The synthesized material is proved to have high crystallinity by XRD performance test, and the synthesized α -Fe is proved to have shape characterization by SEM2O3The iron-nitrogen compound is granular and has a surface drum-shaped. The test of magnetic strength is carried out by a vibration magnetometer, the synthesized iron-nitrogen compound is proved to have good magnetic performance, and the test of wave absorbing performance is carried out on the nitrided iron-nitrogen compound by a vector network instrument, thereby proving that the invention has good magnetic performanceThe iron-nitrogen compound low frequency band has good wave absorbing performance, high practical application value and good application prospect in the fields of microwave absorbing materials, electromagnetic protection and the like.
Description
Technical Field
The invention belongs to the field of microwave absorption material preparation, and particularly relates to Fe with microwave absorption performance4N and a preparation method thereof.
Background
Stealth (stealth technology), is a technology that changes its own detectable signal characteristics by various technical means to reduce the probability of the opposite detection system finding itself to the maximum extent. According to the target detection prevention feature, the stealth technology types can be classified into visible light stealth, infrared stealth, radar or microwave stealth, laser stealth, acoustic wave stealth and the like. According to the introduction of relevant data, in the detection of targets of aircraft in battle, the radar accounts for about 60%, the infrared accounts for about 30%, and the other accounts for about 10%. The radar stealth approaches of the current aircraft mainly comprise the following three approaches: firstly, radar absorbing materials (RAM for short) are applied to a target to absorb and attenuate radar detection waves, so that the radar scattering sectional area is reduced; secondly, the radar cross section (RCS for short) of the target is reduced through the appearance structure design of the target; third, impedance stealth. Due to the limited potential of the contoured structural stealth design and the potential for compromising the aerodynamic performance of the aircraft, the material stealth design has become a hotspot in today's stealth technology research. The wave-absorbing material has the advantages of good wave-absorbing performance, simple process, easy adjustment and the like, and plays a major role in stealth technology.
The radar wave-absorbing material can be divided into an electric loss type and a magnetic loss type according to a wave-absorbing principle, wherein the electric loss type comprises resistance loss and dielectric loss; according to the forming process and the bearing capacity, the method can be divided into a structural type and a coating type. The electric loss type wave-absorbing material comprises graphite, carbon black, carbon nano tubes, carbon fibers, silicon carbide fibers and the like. The magnetic loss type wave-absorbing material comprises ferrite, iron nitrogen compound, magnetic metal micro powder, polycrystalline fiber and the like.
Ferrite is the most mature wave absorbing agent researched at present, has magnetic loss capacity and dielectric loss capacity, has high density and poor temperature stability, and limits the application of the ferrite in wave absorbing materials. Iron nitrogen compounds are widely used in various fields, such as magnetic recording materials. Compared with the common metal powder absorbent, the iron-nitrogen compound has the advantages of low density, good corrosion resistance, good magnetic performance and the like; with Fe4For example, N has a higher temperature stability than ferrite absorbers, and has the advantage of strongly attenuating electromagnetic waves over a wider temperature range.
At present, most of iron-nitrogen compounds are obtained by nitriding iron powder, but the iron powder is easy to oxidize, and the nitriding treatment is carried out only by treating before nitriding, so that the treatment is complex. At present, nitriding treatment is carried out by using ammonia gas and hydrogen according to different proportions, and the hydrogen is flammable and explosive, so that great potential safety hazards exist.
Disclosure of Invention
The invention provides a granular α -Fe2O3Preparation of Fe having microwave absorbing Properties4N method, which is safer than the prior art method, and the obtained Fe4N has good wave-absorbing performance and magnetic performance.
The invention provides a granular α -Fe2O3Preparation of Fe having microwave absorbing Properties4The method of N, comprising the steps of:
(1) FeCl is added3·6H2O、CH3COONa is dissolved in water, ethylene glycol is added dropwise, the mixture is transferred to a reaction kettle, the mixture reacts for 6-24 hours at the temperature of 180-220 ℃, a reddish brown mixture is obtained, and the mixture is washed and dried to obtain a reddish brown solid α -Fe2O3；
(2) α -Fe obtained in the step (1)2O3Placing the mixture in a porcelain boat, vacuumizing, introducing nitrogen, heating to 500-600 ℃ at the speed of 5 ℃/min, introducing ammonia, and keeping the temperature for 3-7 h to obtain Fe4N。
Preferably, in step (1), FeCl3·6H2O、CH3The molar ratio of COONa is 1: 3.
Preferably, in step (1), the amount of ethylene glycol added is 0.375 times the total volume of the solution.
Preferably, in step (1), the reaction temperature is 200 ℃.
Preferably, in step (2), the temperature is raised to 520 ℃ at a rate of 5 ℃/min.
Preferably, in the step (2), the reaction time is 3-5 h.
Fe as described above4N can be applied to the fields of microwave absorption materials, electromagnetic protection and the like.
The invention has the beneficial effects that: the method of the invention uses FeCl3·6H2O、CH3α -Fe is prepared by taking COONa and ethylene glycol as raw materials2O3Then nitriding treatment is carried out by nitrogen protection and ammonia decomposition to obtain iron-nitrogen compound, the operation steps are relatively simple, and the synthesized α -Fe2O3Uniform grain diameter, high crystallinity and good dispersibility, made of α -Fe2O3Prepared Fe4The wave absorbing performance of N is excellent. Compared with ferrite, the Fe prepared by the method of the invention4N has good wave-absorbing performance and magnetic performance. Therefore, the invention has high practical application value.
Drawings
FIG. 1 is α -Fe of one embodiment of the present invention2O3And Fe4XRD pattern of N.
FIG. 2 is α -Fe of one embodiment of the present invention2O3(a) And Fe4SEM image of N (b)
FIG. 3 is Fe according to an embodiment of the present invention4Magnetic hysteresis curve of N.
FIG. 4 is Fe according to an embodiment of the present invention4N reflection loss plot.
Detailed Description
The invention is further illustrated by example 1.
Example 1
(1) Preparation of α -Fe in granular form2O3
6.765g FeCl was weighed3·6H2O in 10mL of water, 6.155g of CH were weighed3Dissolving COONa in 30mL of water, mixing and stirring the COONa and the water uniformly, dropwise adding 15mL of ethylene glycol, stirring for 30min by magnetic force, transferring the mixture into a 100mL reaction kettle, reacting for 12h at 200 ℃ to obtain a red-brown mixed liquid, washing with water and ethanol for multiple times, and drying the product at 60 ℃ in vacuum to obtain a red-brown solid α -Fe2O3Grinding into powder with a mortar for later use;
(2) preparation of iron-nitrogen compound Fe4N
α -Fe synthesized in the step (1)2O3Uniformly spreading in a corundum porcelain boat, vacuumizing, introducing nitrogen, heating to 520 ℃ at the speed of 5 ℃/min, introducing ammonia gas, keeping the temperature for 5 hours, closing the ammonia gas, introducing nitrogen gas, and naturally cooling to room temperature to obtain the iron-nitrogen compound Fe4N。
Through XRD performance test, the position of the diffraction peak of the sample is matched with that of a standard diffraction card (NO.06-0627), and the synthesis of pure-phase Fe is proved4N and high crystallinity, morphology characterization by SEM demonstrated synthetic α -Fe2O3Is granular, nitrided Fe4N is in an interlaced network shape. Testing of the intensity of the magnetic force by means of a vibrating magnetometer, Fe4The saturation magnetization of N was 176.5emu/g, confirming that the synthesized Fe4N has good magnetic force performance and is used for measuring Fe by a vector network instrument4The wave absorbing performance of concentric rings which are made of N and paraffin according to the mass ratio of 1:1 and have the thickness of 2mm, the inner diameter of 3.04mm and the outer diameter of 7mm is tested, and the Fe-based composite material is proved to be Fe4N has good wave-absorbing performance, has high practical application value and has good application prospect in the fields of microwave absorbing materials, electromagnetic protection and the like.
Thus, the method of the present invention uses FeCl3·6H2O、CH3COONa as raw material, adding ethylene glycol to control α -Fe2O3To obtain α -Fe2O3Further α -Fe2O3Reacting with ammonia gas to obtain pure phase Fe4N。
Claims (9)
1. A granular α -Fe2O3Preparation of Fe having microwave absorbing Properties4The method of N, comprising the steps of:
(1) FeCl is added3·6H2O、CH3COONa is dissolved in water, ethylene glycol is added dropwise, the mixture is transferred to a reaction kettle, the mixture reacts for 6-24 hours at the temperature of 180-220 ℃, a reddish brown mixture is obtained, and the mixture is washed and dried to obtain a reddish brown solid α -Fe2O3；
(2) α -Fe obtained in the step (1)2O3Placing the mixture in a porcelain boat, vacuumizing, introducing nitrogen, heating to 500-600 ℃ at the speed of 5 ℃/min, introducing ammonia, and keeping the temperature for 3-7 h to obtain Fe4N。
2. The method of claim 1, wherein: in step (1), FeCl3·6H2O、CH3The molar ratio of COONa is 1: 3.
3. The method of claim 1, wherein: in step (1), ethylene glycol was added in an amount of 0.375 times the total volume of the solution.
4. The method of claim 1, wherein: in step (1), the reaction temperature was 200 ℃.
5. The method of claim 1, wherein: in step (2), the temperature was raised to 520 ℃ at a rate of 5 ℃/min.
6. The method of claim 1, wherein: in the step (2), the reaction time is 3-5 h.
7.Fe4N material, its characterized in that: obtained by the process according to any one of claims 1 to 6.
8. Fe of claim 74And (3) application of the N material.
9. Use according to claim 8, characterized in that: said Fe4The N material is applied to the field of microwave absorption materials or electromagnetic protection.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113955725A (en) * | 2021-11-23 | 2022-01-21 | 深圳市北测检测技术有限公司 | Novel preparation of low-frequency nano wave-absorbing material Fe4Method of N |
| CN114554819A (en) * | 2022-02-25 | 2022-05-27 | 山东大学 | Electromagnetic wave absorber based on iron-based metal organic framework material and preparation method thereof |
| CN114920217A (en) * | 2022-06-14 | 2022-08-19 | 浙江工业大学 | Porous iron-based nitride material with high wave-absorbing performance and preparation method thereof |
| CN114554819B (en) * | 2022-02-25 | 2024-05-03 | 山东大学 | Electromagnetic wave absorber based on iron-based metal organic framework material and preparation method thereof |
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| CN104192815A (en) * | 2014-08-27 | 2014-12-10 | 山东大学 | Dendritic iron nitride powder and preparation method thereof |
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2020
- 2020-05-29 CN CN202010477013.3A patent/CN111704115A/en active Pending
Patent Citations (4)
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Non-Patent Citations (1)
| Title |
|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113955725A (en) * | 2021-11-23 | 2022-01-21 | 深圳市北测检测技术有限公司 | Novel preparation of low-frequency nano wave-absorbing material Fe4Method of N |
| CN114554819A (en) * | 2022-02-25 | 2022-05-27 | 山东大学 | Electromagnetic wave absorber based on iron-based metal organic framework material and preparation method thereof |
| CN114554819B (en) * | 2022-02-25 | 2024-05-03 | 山东大学 | Electromagnetic wave absorber based on iron-based metal organic framework material and preparation method thereof |
| CN114920217A (en) * | 2022-06-14 | 2022-08-19 | 浙江工业大学 | Porous iron-based nitride material with high wave-absorbing performance and preparation method thereof |
| CN114920217B (en) * | 2022-06-14 | 2023-10-31 | 浙江工业大学 | Porous iron-based nitride material with high wave absorbing performance and preparation method thereof |
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