CN115636948A - Preparation method of Fe-P composite stealth material - Google Patents
Preparation method of Fe-P composite stealth material Download PDFInfo
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- CN115636948A CN115636948A CN202211371631.5A CN202211371631A CN115636948A CN 115636948 A CN115636948 A CN 115636948A CN 202211371631 A CN202211371631 A CN 202211371631A CN 115636948 A CN115636948 A CN 115636948A
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Abstract
The invention relates to the technical field of stealth materials, in particular to a preparation method of a Fe-P composite stealth material, which comprises the following steps: respectively weighing a proper amount of ferric chloride hexahydrate and terephthalic acid to prepare a precursor; weighing a proper amount of precursor, ultrasonically dispersing the precursor in deionized water, adding phytic acid with the concentration of 70%, stirring at room temperature, centrifugally cleaning, collecting a product, and performing vacuum drying; step three, heating and preserving the obtained sample under the protection of nitrogen atmosphere, then naturally cooling, and collecting the sample; weighing a sample, mixing the sample with paraffin, heating and melting the mixture, pressing the mixture into a circular ring with the inner diameter of 3.04mm and the outer diameter of 7mm, and testing the electromagnetic parameters of the sample in the frequency range of 1-18GHz by using a coaxial method. Compared with the prior art, the Fe-P composite stealth material prepared by the invention has excellent wave-absorbing performance, the optimal reflection loss reaches-67.6 dB (2 mm), and the effective absorption bandwidth reaches 5.1GHz. Meanwhile, the MOF derivative has very light weight, and meets the design requirements of thinness, lightness, width and strength.
Description
Technical Field
The invention relates to the technical field of stealth materials, in particular to a preparation method of a Fe-P composite stealth material.
Background
Modern military technology is continuously updated, and the war form is also changed greatly. Various novel weapons are on the spot constantly, and the tracking, detection, identification means of each country are also more and more advanced, if do not add the protection, military facilities and aircraft are very easily found, are tracked and attacked by the enemy, bring huge threat to national defense safety. In order to reduce the tracking and monitoring of a weapon system in war and improve the penetration and depth striking capability of the weapon system, the research of a new generation stealth technology is particularly important.
The microwave absorbing material is a functional material which can convert electromagnetic energy incident to the surface of the microwave absorbing material into heat energy or other energy through modes of dielectric loss or magnetic loss and the like so as to be consumed, and when the electromagnetic wave emitted by an enemy radar is incident to own weapons, the stealth material can absorb the loss, so that the threat that the own weapons are exposed is effectively reduced. The novel broadband, light and thin and high-absorption wave-absorbing material has great application value.
The existing common iron/iron oxide stealth materials usually have higher density, and the effective absorption bandwidth needs to be further improved, so that the development requirement of the light wave-absorbing material is difficult to meet.
MOFs materials have the advantages of light weight, porosity, simple preparation process, easy regulation and control of size and shape and the like, and are widely researched in the fields of adsorption, catalysis, biomedicine and the like. Among the MOFs, materials ZIF-67, ZIF-8, MIL-88A, MIL-88B, and others have been extensively studied (Huang M, wang L, pei K, et al. Multimedia-Controllable Synthesis of MOF-Derived Co @ N-bed Carbon Composite with Magnetic-Dielectric Synthesis Microwave Absorption [ J ]. Small,2020,16 (14): 20058
Gu W,Lv J,Quan B,et al.Achieving MOF-derived one-dimensional porous ZnO/C nanofiber with lightweight and enhanced microwave response by an electrospinning method[J].Journal of Alloys and Compounds,2019,806:983-991
Man Z,Li P,Zhou D,et al.Two Birds with One Stone:FeS2@C Yolk–Shell Composite for High-Performance Sodium-Ion Energy Storage and Electromagnetic Wave Absorption[J].Nano Letters,2020,20(5):3769-3777
Xiang Z, song Y, xiong J, et al, enhanced electromagnetic wave absorption of nanoporous fe3o4@ Carbon composites derived from metal-organic structures [ J ]. Carbon,2019, 142), have been demonstrated to have very excellent microwave absorption properties, however, few studies on the wave absorption of MIL-101 (Fe) have been reported and studies on the use of MIL-101 (Fe) derivatives doped with phosphorus in light high-intensity wave-absorbing materials have not been reported yet.
Disclosure of Invention
Aiming at the problem that the prior stealth material is difficult to meet the requirements of light weight and strong absorption, the invention provides a preparation method of a Fe-P composite stealth material. So as to prepare the stealth material which can meet the requirements of thinness, lightness, width, strength and the like.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of a Fe-P composite stealth material comprises the following steps:
respectively weighing a proper amount of ferric chloride hexahydrate and terephthalic acid to prepare a precursor;
weighing a proper amount of precursor, ultrasonically dispersing the precursor in deionized water, adding phytic acid with the concentration of 70%, stirring at room temperature, centrifugally cleaning, collecting a product, and performing vacuum drying;
step three, heating and preserving the temperature of the obtained sample under the protection of nitrogen atmosphere, then naturally cooling, and collecting the sample;
weighing a sample, mixing the sample with paraffin, heating and melting the mixture, pressing the mixture into a circular ring with the inner diameter of 3.04mm and the outer diameter of 7mm, and testing the electromagnetic parameters of the sample in the frequency range of 1GHz-18GHz by using a coaxial method.
Preferably, the preparation process of the precursor in the step (one) is as follows:
(A) Ultrasonically dissolving ferric chloride hexahydrate and terephthalic acid into N, N-dimethylformamide;
(B) Transferring the solution to a polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in an oven, preserving heat at a certain temperature and reacting;
(C) After the reaction is finished, naturally cooling the reaction kettle to room temperature, and centrifugally collecting reddish brown precipitate;
(D) Washing with deionized water and absolute ethyl alcohol for many times, and drying in a vacuum oven to obtain the precursor.
Preferably, the mass of ferric chloride hexahydrate in step (A) is 2g to 5g, the mass of terephthalic acid is 0.6g to 1g, and the volume of N, N-dimethylformamide is 40ml to 80ml.
Preferably, in the step (B), the reaction heat preservation temperature is 100-150 ℃, and the heat preservation reaction time is 15-30 h.
Preferably, the drying temperature in the step (D) is 50-80 ℃, and the drying time is 20-40 h.
Preferably, the mass of the precursor in the step (II) is 1g-2g, the volume of the deionized water is 80ml-100ml, the volume of the phytic acid is 1ml-5ml, the vacuum drying temperature is 40 ℃ to 80 ℃, and the vacuum drying time is 24h-48h.
Preferably, the heating temperature in the step (III) is 600-1000 ℃, and the heat preservation time is 2-4 h.
Preferably, the mass mixing ratio of the sample to the paraffin in the step (IV) is 2-4.
The beneficial effects of the invention are:
compared with the prior art, the Fe-P composite stealth material prepared by the invention has excellent wave-absorbing performance, the optimal reflection loss reaches-67.6 dB (2 mm), and the effective absorption bandwidth reaches 5.1GHz. Meanwhile, the MOF derivative has very light weight, and meets the design requirements of thinness, lightness, width and strength.
Drawings
The invention is further illustrated with reference to the following figures and examples:
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a topographical view of a precursor of the present invention;
FIG. 3 is a sample morphology map after sintering in accordance with the present invention;
FIG. 4 is a wave-absorbing performance diagram of the Fe-P composite stealth material.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further explained in the following with the accompanying drawings and the embodiments.
As shown in fig. 1, a preparation method of a Fe-P composite stealth material comprises the following specific preparation processes:
respectively weighing a proper amount of ferric chloride hexahydrate and terephthalic acid, ultrasonically dissolving the ferric chloride hexahydrate and the terephthalic acid in N, N-Dimethylformamide (DMF), then transferring the solution to a polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in an oven, preserving heat at a certain temperature, and reacting. After the reaction is finished, naturally cooling the reaction kettle to room temperature, centrifuging and collecting the reddish brown precipitate, washing the precipitate with deionized water and absolute ethyl alcohol for multiple times, placing the precipitate in a vacuum oven for drying to obtain a precursor, and collecting the precursor for later use. The precursor is shown in figure 2.
The method comprises the following steps of preparing ferric chloride hexahydrate, terephthalic acid, N-dimethylformamide, drying at 50-80 ℃ for 15-30 h, wherein the mass of the ferric chloride hexahydrate is 2-5 g, the mass of the terephthalic acid is 0.6-1 g, the volume of the N, N-dimethylformamide is 40-80 mL, the reaction heat preservation temperature is 100-150 ℃, and the drying time is 20-40 h.
And (II) weighing a proper amount of precursor, ultrasonically dispersing the precursor in deionized water, adding phytic acid (with the concentration of 70%), stirring at room temperature, centrifugally cleaning, collecting a product, and drying in vacuum.
Wherein the mass of the precursor is 1g-2g, the volume of the deionized water is 80mL-100mL, the volume of the phytic acid is 1mL-5mL, the vacuum drying temperature is 40-80 ℃, and the drying time is 24h-48h.
And (III) heating and preserving the temperature of the obtained sample under the protection of nitrogen atmosphere, then naturally cooling, and collecting the sample. The sample was heated as shown in FIG. 3.
Wherein the heating temperature is 600-1000 ℃, and the heat preservation time is 2-4 h.
Weighing a sample, mixing the sample with paraffin, heating and melting the mixture, pressing the mixture into a circular ring with the inner diameter of 3.04mm and the outer diameter of 7mm, and testing the electromagnetic parameters of the sample in the frequency range of 1GHz-18GHz by using a coaxial method. As shown in fig. 4.
Wherein the mixing ratio of the sample to paraffin is 2-4.
Compared with the prior art, the Fe-P composite stealth material prepared by the invention has excellent wave-absorbing performance, the optimal reflection loss reaches-67.6 dB (2 mm), and the effective absorption bandwidth reaches 5.1GHz. Meanwhile, the MOF derivative has very light weight, and meets the design requirements of thinness, lightness, width and strength.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A preparation method of a Fe-P composite stealth material is characterized by comprising the following steps: the method comprises the following steps:
respectively weighing a proper amount of ferric chloride hexahydrate and terephthalic acid to prepare a precursor;
weighing a proper amount of precursor, ultrasonically dispersing the precursor in deionized water, adding phytic acid with the concentration of 70%, stirring at room temperature, centrifugally cleaning, collecting a product, and performing vacuum drying;
step three, heating and preserving the obtained sample under the protection of nitrogen atmosphere, then naturally cooling, and collecting the sample;
weighing a sample, mixing the sample with paraffin, heating and melting the mixture, pressing the mixture into a circular ring with the inner diameter of 3.04mm and the outer diameter of 7mm, and testing the electromagnetic parameters of the sample in the frequency range of 1GHz-18GHz by using a coaxial method.
2. The method for preparing the Fe-P composite stealth material according to claim 1, characterized in that: the preparation process of the precursor in the step (I) comprises the following steps:
(A) Dissolving ferric chloride hexahydrate and terephthalic acid in N, N-dimethylformamide by ultrasonic;
(B) Transferring the solution into a polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in an oven, preserving heat at a certain temperature and carrying out reaction;
(C) After the reaction is finished, naturally cooling the reaction kettle to room temperature, and centrifugally collecting reddish brown precipitate;
(D) Washing with deionized water and absolute ethyl alcohol for many times, and drying in a vacuum oven to obtain the precursor.
3. The method for preparing the Fe-P composite stealth material according to claim 2, characterized in that: in the step (A), the mass of ferric chloride hexahydrate is 2g-5g, the mass of terephthalic acid is 0.6g-1g, and the volume of N, N-dimethylformamide is 40ml-80ml.
4. The method for preparing the Fe-P composite stealth material according to claim 2, characterized in that: in the step (B), the reaction temperature is kept between 100 and 150 ℃, and the reaction time is kept between 15 and 30 hours.
5. The method for preparing the Fe-P composite stealth material according to claim 2, characterized in that: in the step (D), the drying temperature is 50-80 ℃, and the drying time is 20-40 h.
6. The method for preparing the Fe-P composite stealth material according to claim 1, characterized in that: in the step (II), the mass of the precursor is 1g-2g, the volume of the deionized water is 80ml-100ml, the volume of the phytic acid is 1ml-5ml, the vacuum drying temperature is 40 ℃ to 80 ℃, and the vacuum drying time is 24h-48h.
7. The method for preparing the Fe-P composite stealth material according to claim 1, characterized in that: in the step (III), the heating temperature is 600-1000 ℃, and the heat preservation time is 2-4 h.
8. The method for preparing the Fe-P composite stealth material according to claim 1, characterized in that: in the step (IV), the mass mixing ratio of the sample to the paraffin is 2-4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104022301A (en) * | 2014-06-23 | 2014-09-03 | 天津大学 | Macromolecular phytic acid supported metal organic framework composite membrane as well as preparation method and application thereof |
| CN110201718A (en) * | 2019-05-29 | 2019-09-06 | 上海电力学院 | A kind of preparation and application of red phosphorus/ferrous metals organic framework composite material |
| CN112225950A (en) * | 2020-10-28 | 2021-01-15 | 北京航空航天大学 | Preparation method of environment-friendly Fe @ C composite wave-absorbing material |
| CN113061930A (en) * | 2021-03-23 | 2021-07-02 | 广东工业大学 | Preparation method of transition metal phosphide |
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- 2022-11-03 CN CN202211371631.5A patent/CN115636948A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104022301A (en) * | 2014-06-23 | 2014-09-03 | 天津大学 | Macromolecular phytic acid supported metal organic framework composite membrane as well as preparation method and application thereof |
| CN110201718A (en) * | 2019-05-29 | 2019-09-06 | 上海电力学院 | A kind of preparation and application of red phosphorus/ferrous metals organic framework composite material |
| CN112225950A (en) * | 2020-10-28 | 2021-01-15 | 北京航空航天大学 | Preparation method of environment-friendly Fe @ C composite wave-absorbing material |
| CN113061930A (en) * | 2021-03-23 | 2021-07-02 | 广东工业大学 | Preparation method of transition metal phosphide |
Non-Patent Citations (1)
| Title |
|---|
| JUE LIU等: "Fire-resistant iron-based phosphates/phosphorus-doped carbon composites derived from phytic acid-treated metal organic frameworks as high-efficiency microwave absorbers", 《CARBON》, vol. 200, pages 1 - 2 * |
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