CN113249092A - Metal organic framework complex composite wave-absorbing powder and preparation method thereof - Google Patents
Metal organic framework complex composite wave-absorbing powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of wave-absorbing materials, in particular to a preparation method of metal organic framework complex composite wave-absorbing powder. The method specifically comprises the steps of reacting iron salt, cobalt salt, organic ligand and organic solvent by a solvothermal method to generate Co/Fe-MOFs (cobalt-iron metal organic framework complex), and coating the surface of the obtained Co/Fe-MOFs wave-absorbing powder with a layer of SiO again by a silica sol heating coating process2Rust-proof shell layer to obtain SiO2The coated Co/Fe-MOFs composite wave-absorbing powder is subjected to high-temperature reaction sintering to obtain Co/Fe-MOFs @ SiO with regulated and controlled micro-morphology2Composite wave-absorbing powder. The microwave absorbing material not only effectively inhibits the eddy current effect through dielectric isolation, but also has the advantages of oxidation resistance, corrosion resistance and high temperature resistance, so that the microwave absorbing material has wider application possibility.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a preparation method of metal organic framework complex composite wave-absorbing powder.
Background
The wave-absorbing material is a material which can absorb or greatly weaken the electromagnetic wave received by the surface of the wave-absorbing material and convert the electromagnetic energy into other forms of energy to be dissipated or disappear due to interference, thereby reducing the interference of the electromagnetic wave, and has wide application in various aspects in the military and civil fields. The magnetic metal organic framework material is considered as a material with great potential by scholars at home and abroad due to adjustable and controllable micro-morphology, high porosity and large specific surface area, so that the magnetic metal organic framework material is widely concerned and applied. The cobalt and iron metal materials can be used as node metals for constructing the metal organic frame by virtue of extremely high magnetic conductivity and magnetization intensity and simultaneously introducing the advantages of dielectric loss and magnetic loss, and are applied to the magnetic metal organic frame wave-absorbing composite material to excite more excellent wave-absorbing performance. However, when facing high temperature or corrosive environment, iron metal may cause unstable designed electromagnetic parameters due to oxidation and corrosion, which affects its wave absorbing performance and service life, and iron metal has high conductivity, and is easy to have severe eddy effect at high frequency, which reduces the penetration of electromagnetic wave, thereby reducing the wave absorbing performance of the material.
The existing composite wave-absorbing material product of magnetic metal has a simple structure, the micro appearance is mostly of a one-dimensional or two-dimensional structure, the preparation process cannot realize targeted regulation and control on the micro appearance, and the wide application requirement on the wave-absorbing material is difficult to meet; pure magnetic metal elements have good magnetic loss mechanism, but lack dielectric loss matching to achieve good impedance matching; and the addition of the iron element causes the composite wave-absorbing powder to have the defects of easy corrosion, reduced absorption loss caused by eddy current effect and the like, and is not beneficial to long-time production and use in the follow-up process.
Therefore, the technical problem to be solved by the technical personnel in the field is urgent, how to provide a wave-absorbing material which effectively inhibits the eddy current effect and has oxidation corrosion resistance and a preparation method thereof, so that the wave-absorbing material has more extensive and excellent wave-absorbing performance.
Disclosure of Invention
The invention aims to provide SiO2Cobalt-iron organic framework formulation for regulating and controlling microscopic morphology by sol coating combined reaction sintering methodThe preparation method of the composite wave-absorbing powder of the compound not only effectively inhibits the eddy current effect through dielectric isolation treatment, but also has the advantages of oxidation resistance, corrosion resistance and high temperature resistance, so that the wave-absorbing material has wider application possibility.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of metal organic framework complex composite wave-absorbing powder, which comprises the following steps:
(1) stirring and mixing an organic ligand, cobalt salt and ferric salt in an organic solvent to form slurry A;
(2) heating the slurry A to generate a cobalt-iron metal organic framework complex Co/Fe-MOFs to obtain slurry B;
(3) cooling the slurry B to room temperature and then drying to obtain wave-absorbing powder C;
(4) placing the wave-absorbing powder C in ethylene glycol, adding tetraethoxysilane, stirring, and heating to obtain slurry D;
(5) cooling the slurry D to room temperature and drying to obtain composite wave-absorbing powder E;
(6) and sintering the composite wave-absorbing powder E to obtain composite wave-absorbing powder F.
Preferably, the molar ratio of the organic ligand, the cobalt salt, the ferric salt and the organic solvent in the step (1) is 7-9: 2-4: 0.8-1.5: 50-55.
Preferably, the stirring step in the step (1) is to perform ultrasonic oscillation and mechanical stirring simultaneously, the ultrasonic power is 280-320W, and the mechanical stirring speed is 1800-2300 r/min.
Preferably, the heating temperature in the step (2) is 120-200 ℃, and the time is 48-72 hours.
Preferably, the ethylene glycol is added in the step (4) in a ratio of 1-3 g/L, and the tetraethoxysilane is added in a ratio of 15-25 g/L.
Preferably, the heating temperature in the step (4) is 120-150 ℃, and the time is 1-4 h.
Preferably, the stirring step in the step (4) is to perform ultrasonic oscillation and mechanical stirring simultaneously, the ultrasonic power is 280-320W, and the mechanical stirring speed is 1800-2300 r/min.
Preferably, the sintering temperature in the step (6) is 570-630 ℃, and the time is 1.5-2.5 h.
Preferably, the organic ligand is one or more of bipyridyl, triphenylamine tricarboxylate, terephthalic acid and pyrazine.
Preferably, the cobalt salt is one of cobalt acetate, cobalt sulfate, cobalt chloride and cobalt nitrate; the ferric salt is one of ferric nitrate, ferric sulfate and ferric chloride.
Preferably, the organic solvent is one of N, N-dimethylformamide, methanol, toluene and ethanol.
The invention provides a metal organic framework complex composite wave-absorbing powder, which is characterized in that a layer of SiO is coated on the outer layer of Co/Fe-MOFs structural particles2And the microscopic appearance of the shell layer is a porous particle accumulation structure.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
the invention discloses a new SiO2Preparation method of composite wave-absorbing powder of cobalt-iron organic framework complex with microstructure regulated and controlled by sol coating combined reaction sintering method and SiO2The coated Co/Fe-MOFs wave-absorbing powder. Iron salt, cobalt salt, organic ligand and organic solvent are reacted by a solvothermal method to generate Co/Fe-MOFs (cobalt-iron metal organic framework complex), and the obtained absorbing powder surface of the Co/Fe-MOFs is coated with a layer of SiO (silicon dioxide) again by a secondary solvothermal process2Rust-proof shell layer to obtain SiO2The coated Co/Fe-MOFs composite wave-absorbing powder is subjected to high-temperature reaction sintering to obtain Co/Fe-MOFs @ SiO with regulated and controlled micro-morphology2Composite wave-absorbing powder.
The invention utilizes the difference of the solvent thermal temperature as the driving force, adopts the combination of the cobalt-iron metal organic framework complex and the dielectric material, and constructs a porous three-dimensional structure by depending on the special structural characteristics of the MOF material, thereby greatly increasing the refraction and absorption of the microwave in the wave-absorbing material and effectively improving the wave-absorbing performance; the surface of the wave-absorbing powder is coated with a layer of SiO by a secondary solvothermal method2Shell layer for effectively preventing composite wave-absorbing powderCorrosion loss of the body during production or use; finally, by combining a high-temperature reaction sintering process, the adjustable three-dimensional structure composite wave-absorbing material with high porosity can be obtained, the complex appearance of the material is favorable for the refraction and absorption of electromagnetic waves, and SiO is reserved2On the premise of excellent mechanical property with MOF material, various absorption mechanisms are introduced, thereby improving SiO2The coated Co/Fe-MOFs composite wave-absorbing material has comprehensive wave-absorbing performance.
Drawings
FIG. 1 shows the wave-absorbing properties of the metal organic framework complex composite wave-absorbing powder prepared in example 1 under different thicknesses;
FIG. 2 shows the wave-absorbing properties of the metal organic framework complex composite wave-absorbing powder prepared in example 1 at a thickness of 3.9 mm;
FIG. 3 shows the wave-absorbing properties of the uncoated composite wave-absorbing powder prepared in comparative example 1 at different thicknesses.
Detailed Description
The invention makes metal cobalt salt, metal iron salt and organic ligand fully and uniformly dispersed in organic solvent, then carries out solvothermal synthesis, then obtains Co/Fe-MOFs wave-absorbing powder, and then coats a layer of SiO by a secondary solvothermal method2And combining the shell layer with a reaction sintering process to obtain the adjustable three-dimensional structure composite wave-absorbing material with high porosity.
The invention provides a preparation method of metal organic framework complex composite wave-absorbing powder, which comprises the following steps:
(1) stirring and mixing an organic ligand, cobalt salt and ferric salt in an organic solvent to form slurry A;
(2) heating the slurry A to generate a cobalt-iron metal organic framework complex Co/Fe-MOFs to obtain slurry B;
(3) cooling the slurry B to room temperature and then drying to obtain wave-absorbing powder C;
(4) placing the wave-absorbing powder C in ethylene glycol, adding tetraethoxysilane, stirring, and heating to obtain slurry D;
(5) cooling the slurry D to room temperature and drying to obtain composite wave-absorbing powder E;
(6) and sintering the composite wave-absorbing powder E to obtain composite wave-absorbing powder F.
Preferably, the molar ratio of the organic ligand, the cobalt salt, the ferric salt and the organic solvent in the step (1) is 7-9: 2-4: 0.8-1.5: 50-55.
Preferably, the stirring step in the step (1) is to perform ultrasonic oscillation and mechanical stirring simultaneously, the ultrasonic power is 280-320W, and the mechanical stirring speed is 1800-2300 r/min.
Preferably, the heating temperature in the step (2) is 120-200 ℃, and the time is 48-72 hours.
Preferably, the ethylene glycol is added in the step (4) in a ratio of 1-3 g/L, and the tetraethoxysilane is added in a ratio of 15-25 g/L.
Preferably, the heating temperature in the step (4) is 120-150 ℃, and the time is 1-4 h.
Preferably, the stirring step in the step (4) is to perform ultrasonic oscillation and mechanical stirring simultaneously, the ultrasonic power is 280-320W, and the mechanical stirring speed is 1800-2300 r/min.
Preferably, the sintering temperature in the step (6) is 570-630 ℃, and the time is 1.5-2.5 h.
Preferably, the organic ligand is one or more of bipyridyl, triphenylamine tricarboxylate, terephthalic acid and pyrazine.
Preferably, the cobalt salt is one of cobalt acetate, cobalt sulfate, cobalt chloride and cobalt nitrate; the ferric salt is one of ferric nitrate, ferric sulfate and ferric chloride.
Preferably, the organic solvent is one of N, N-dimethylformamide, methanol, toluene and ethanol.
The following will explain the preparation method of the metal organic framework complex composite wave-absorbing powder provided by the present invention in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Mixing bipyridine, cobalt acetate, ferric nitrate and N, N-dimethylformamide according to a molar ratio of 7:2:0.8:50, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 300W, the mechanical stirring speed is 2000r/min, and uniformly stirring to form slurry A;
(2) pouring the slurry A into a reaction kettle, putting the reaction kettle into a 120 ℃ oven, and taking out the reaction kettle after 72 hours to obtain slurry B;
(3) cooling the slurry B to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain wave-absorbing powder C;
(4) putting the wave-absorbing powder C into ethylene glycol in a ratio of 1g/L, adding tetraethoxysilane in a ratio of 15g/L, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 300W, the mechanical stirring speed is 2000r/min, putting the mixture into a reaction kettle after uniformly stirring, putting the reaction kettle into a 120 ℃ drying oven, and taking out the reaction kettle after 4 hours to obtain slurry D;
(5) cooling the slurry D to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain composite wave-absorbing powder E;
(6) and (3) putting the composite wave-absorbing powder E into a tube furnace, sintering for 2.5 hours at 570 ℃, and cooling the tube furnace to room temperature to obtain composite wave-absorbing powder F, namely the metal organic framework complex composite wave-absorbing powder.
The metal organic framework complex composite wave-absorbing powder obtained in the embodiment has high performance, and the minimum reflection loss value is-45.6 dB and the wave-absorbing bandwidth below-10 dB is 1.68GHz under the conditions that the thickness is 3.9mm and 10.48GHz is obtained.
Example 2
(1) Mixing triphenylamine tricarboxylate, cobalt sulfate, ferric sulfate and methanol according to a molar ratio of 8:3:1:52, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 280W, the mechanical stirring speed is 2200r/min, and uniformly stirring to form slurry A;
(2) pouring the slurry A into a reaction kettle, putting the reaction kettle into a drying oven at 150 ℃ for 60 hours, and taking out to obtain slurry B;
(3) cooling the slurry B to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain wave-absorbing powder C;
(4) putting the wave-absorbing powder C into ethylene glycol at a ratio of 2g/L, adding tetraethoxysilane at a ratio of 20g/L, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 280W, the mechanical stirring speed is 2200r/min, after uniformly stirring, putting the mixture into a reaction kettle, putting the reaction kettle into a 130 ℃ drying oven, and taking out the reaction kettle after 3 hours to obtain slurry D;
(5) cooling the slurry D to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain composite wave-absorbing powder E;
(6) and (3) putting the composite wave-absorbing powder E into a tube furnace, sintering for 2h at the temperature of 600 ℃, and cooling the tube furnace to room temperature to obtain composite wave-absorbing powder F, namely the metal organic framework complex composite wave-absorbing powder.
The metal organic framework complex composite wave-absorbing powder obtained in the embodiment has high performance, and is characterized in that the minimum reflection loss value is-42.7 dB and the wave-absorbing bandwidth is 3.42GHz under the conditions that the thickness is 4mm and the frequency is 9.44 GHz.
Example 3
(1) Mixing terephthalic acid, cobalt chloride, ferric chloride and toluene according to a molar ratio of 9:4:1.5:55, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 320W, the mechanical stirring speed is 2100r/min, and uniformly stirring to form slurry A;
(2) pouring the slurry A into a reaction kettle, putting the reaction kettle into a 200 ℃ oven, and taking out after 48 hours to obtain slurry B;
(3) cooling the slurry B to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain wave-absorbing powder C;
(4) putting the wave-absorbing powder C into ethylene glycol in a ratio of 3g/L, adding tetraethoxysilane in a ratio of 25g/L, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 320W, the mechanical stirring speed is 2100r/min, after stirring uniformly, putting the mixture into a reaction kettle, putting the reaction kettle into an oven at 150 ℃ for 1h, and taking out the mixture to obtain slurry D;
(5) cooling the slurry D to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain composite wave-absorbing powder E;
(6) and (3) putting the composite wave-absorbing powder E into a tube furnace, sintering for 1.5h at 630 ℃, and cooling the tube furnace to room temperature to obtain composite wave-absorbing powder F, namely the metal organic framework complex composite wave-absorbing powder.
The metal organic framework complex composite wave-absorbing powder obtained in the embodiment has high performance, and is characterized in that the minimum reflection loss value is-46.8 dB and the wave-absorbing bandwidth is 2.86GHz under the conditions that the thickness is 3.3mm and the 10.4GHz is obtained.
Example 4
(1) Mixing pyrazine, cobalt nitrate, ferric sulfate and ethanol according to a molar ratio of 7.5:3:1.2:53, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 290W, the mechanical stirring speed is 2300r/min, and uniformly stirring to form slurry A;
(2) pouring the slurry A into a reaction kettle, putting the reaction kettle into a 180 ℃ oven, and taking out the reaction kettle after 52 hours to obtain slurry B;
(3) cooling the slurry B to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain wave-absorbing powder C;
(4) putting the wave-absorbing powder C into ethylene glycol at a ratio of 2.5g/L, adding tetraethoxysilane at a ratio of 22g/L, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 290W, the mechanical stirring speed is 2300r/min, after uniformly stirring, putting the mixture into a reaction kettle, putting the reaction kettle into a drying oven at the temperature of 140 ℃, taking out the mixture after 1.2h, and obtaining slurry D;
(5) cooling the slurry D to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain composite wave-absorbing powder E;
(6) and (3) putting the composite wave-absorbing powder E into a tube furnace, sintering for 1.3h at the temperature of 620 ℃, and cooling the tube furnace to room temperature to obtain composite wave-absorbing powder F, namely the metal organic framework complex composite wave-absorbing powder.
The metal organic framework complex composite wave-absorbing powder obtained in the embodiment has high performance, and is characterized in that the minimum reflection loss value is-42.8 dB and the wave-absorbing bandwidth is 2.14GHz under the conditions that the thickness is 3.8mm and the frequency is 9.52 GHz.
Comparative example 1
(1) Mixing triphenylamine tricarboxylate, cobalt sulfate, ferric sulfate and methanol according to a molar ratio of 8:3:1:52, simultaneously performing ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 280W, the mechanical stirring speed is 2200r/min, and uniformly stirring to form slurry A;
(2) pouring the slurry A into a reaction kettle, putting the reaction kettle into a drying oven at 150 ℃ for 60 hours, and taking out to obtain slurry B;
(3) cooling the slurry B to room temperature, and drying in a vacuum drying oven at 65 ℃ to obtain wave-absorbing powder C;
(4) and (3) putting the wave-absorbing powder C into a tube furnace, sintering for 2h at 600 ℃, and cooling the tube furnace to room temperature to obtain wave-absorbing powder D, namely the metal organic framework complex wave-absorbing powder.
The wave-absorbing powder of the metal organic framework complex obtained in the comparative example obtains the minimum reflection loss value of-10.3 dB and the wave-absorbing bandwidth below-10 dB of 0.16GHz under the conditions that the thickness is 6mm and the frequency is 6.96 GHz.
According to the embodiment and the comparative example, the invention provides the preparation method of the metal organic framework complex composite wave-absorbing powder, and the metal organic framework complex composite wave-absorbing powder obtained by the preparation method has excellent wave-absorbing performance and can effectively prevent the corrosion loss of the composite wave-absorbing powder in the production or use process.
As shown in attached drawings 1-3, the metal organic framework complex composite wave-absorbing powder prepared in the embodiment 1 of the invention has the minimum reflection loss value of-45.6 dB and the wave-absorbing bandwidth below-10 dB of 1.68GHz under the conditions that the thickness is 3.9mm and the 10.48 GHz; the wave-absorbing powder of the metal organic frame complex prepared by the comparative example has the minimum reflection loss value of-10.3 dB and the wave-absorbing bandwidth below-10 dB of 0.16GHz under the condition that the thickness is 6mm and 6.96 GHz. Compared with the uncoated composite material prepared by the comparative example, the metal organic framework complex composite wave-absorbing powder prepared by the invention has higher wave-absorbing bandwidth under the condition of thinner thickness.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of metal organic framework complex composite wave-absorbing powder is characterized by comprising the following steps:
(1) stirring and mixing an organic ligand, cobalt salt and ferric salt in an organic solvent to form slurry A;
(2) heating the slurry A to generate a cobalt-iron metal organic framework complex Co/Fe-MOFs to obtain slurry B;
(3) cooling the slurry B to room temperature and then drying to obtain wave-absorbing powder C;
(4) placing the wave-absorbing powder C in ethylene glycol, adding tetraethoxysilane, stirring, and heating to obtain slurry D;
(5) cooling the slurry D to room temperature and drying to obtain composite wave-absorbing powder E;
(6) and sintering the composite wave-absorbing powder E to obtain composite wave-absorbing powder F.
2. The preparation method of the metal organic framework complex composite wave-absorbing powder according to claim 1, wherein the molar ratio of the organic ligand, the cobalt salt, the iron salt and the organic solvent in the step (1) is 7-9: 2-4: 0.8-1.5: 50-55.
3. The preparation method of the metal organic framework complex composite wave-absorbing powder according to claim 1 or 2, wherein the heating temperature in the step (2) is 120-200 ℃ and the time is 48-72 hours.
4. The preparation method of the metal organic framework complex composite wave-absorbing powder according to claim 1, wherein ethylene glycol is added in the step (4) in a proportion of 1-3 g/L, and tetraethoxysilane is added in a proportion of 15-25 g/L.
5. The preparation method of the metal organic framework complex composite wave-absorbing powder according to claim 4, wherein the heating temperature in the step (4) is 120-150 ℃ and the time is 1-4 h.
6. The preparation method of the metal organic framework complex composite wave-absorbing powder according to claim 1, wherein the sintering temperature in the step (6) is 570-630 ℃, and the time is 1.5-2.5 h.
7. The method for preparing the metal-organic framework complex composite wave-absorbing powder according to claim 1 or 2, wherein the organic ligand is one or more of bipyridine, triphenylamine tricarboxylate, terephthalic acid and pyrazine.
8. The method for preparing the metal organic framework complex composite wave-absorbing powder according to claim 7, wherein the cobalt salt is one of cobalt acetate, cobalt sulfate, cobalt chloride and cobalt nitrate; the ferric salt is one of ferric nitrate, ferric sulfate and ferric chloride.
9. The method for preparing the metal organic framework complex composite wave-absorbing powder according to claim 1, wherein the organic solvent is one of N, N-dimethylformamide, methanol, toluene and ethanol.
10. The metal-organic framework complex composite wave-absorbing powder prepared by the preparation method of the metal-organic framework complex composite wave-absorbing powder according to any one of claims 1 to 9, wherein the metal-organic framework complex composite wave-absorbing powder is prepared by coating a layer of SiO on the outer layer of Co/Fe-MOFs structural particles2And the microscopic appearance of the shell layer is a porous particle accumulation structure.
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| CN115785905A (en) * | 2022-10-25 | 2023-03-14 | 浙江工业大学 | MOF (Metal organic framework) derived carbon-based wave-absorbing material with low calcination temperature as well as preparation method and application thereof |
| CN117126419A (en) * | 2023-10-26 | 2023-11-28 | 德州学院 | Cobalt metal organic framework crystal material for gas separation and preparation method and application thereof |
| CN117126419B (en) * | 2023-10-26 | 2024-01-02 | 德州学院 | Cobalt metal organic framework crystal material for gas separation and preparation method and application thereof |
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