CN114590845A - Wide-spectrum extinction interference material and preparation method thereof - Google Patents
Wide-spectrum extinction interference material and preparation method thereof Download PDFInfo
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- CN114590845A CN114590845A CN202210084481.3A CN202210084481A CN114590845A CN 114590845 A CN114590845 A CN 114590845A CN 202210084481 A CN202210084481 A CN 202210084481A CN 114590845 A CN114590845 A CN 114590845A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
The invention provides a wide-spectrum extinction interference material and a preparation method thereof. The method comprises the following steps: preparing a first solution and a second solution by using the first container and the second container which are subjected to the ultrasonic cleaning and the drying treatment respectively; obtaining a mixed solution of the first solution and the second solution, and preparing a CoNi-MOFs precursor suspension by aging the mixed solution; placing the CoNi-MOFs precursor suspension in a centrifuge for centrifugal treatment to obtain a CoNi-MOFs precipitate after supernatant liquid is removed, and placing the CoNi-MOFs precipitate in a vacuum drying box for drying treatment to obtain CoNi-MOFs powder as a CoNi-MOFs precursor; and (3) placing the CoNi-MOFs precursor into a tube furnace for calcination treatment to obtain CoNi-MOFs-800 powder serving as the broad-spectrum extinction interference material.
Description
Technical Field
The invention relates to the field of preparation of photo-thermal materials, in particular to a wide-spectrum extinction interference material and a preparation method thereof.
Background
The precision guidance weapon formally ascends a historical stage after Vietnam war, and along with the development of scientific technology, the weapon with single mode guidance is more and more difficult to adapt to the requirement of modern war, therefore, the dual mode guidance and even the multimode guidance become the conventional mode of the precision guidance weapon.
In order to resist the existing photoelectric guidance means and photoelectric detection technology, the smoke screen plays a key role as a passive interference means with high efficiency-cost ratio and quick use. The device can be used for effectively interfering a photoelectric detection, observation and guidance weapon system by quickly releasing a large amount of aerosol particles into the air to change the transmission characteristics of electromagnetic waves in the air, and is mainly used for shielding, deceiving, blinding and identifying. The different interference effects of the different materials also determine the interference mechanism and the interference efficiency of the different materials are different.
The metal material can better realize the rapid attenuation of electromagnetic waves due to good electromagnetic performance, but has large specific gravity and poor suspension property, so the interference time is short; typical carbon materials such as nano-graphite, graphene and the like have the advantages of large specific surface area, high stability, low density and the like, but the production cost is generally high and the cost efficiency is large. Therefore, it is an important trend in the field to develop a high-performance wide-spectrum extinction interference material which simultaneously satisfies wide interference wave band, good interference effect, low cost and easy mass production.
Disclosure of Invention
The invention aims to provide a wide-spectrum extinction interference material and a preparation method thereof, and aims to solve the technical problems in the prior art.
The invention provides a method for preparing a wide-spectrum extinction interference material for broadband extinction from an ultraviolet band to a middle and far infrared band, which comprises the following steps:
step S1, performing ultrasonic cleaning and drying treatment on a first container and a second container by using Wujie powder and deionized water, wherein the first container and the second container are beakers;
step S2 of preparing a first solution and a second solution using the first container and the second container subjected to the ultrasonic cleaning and the drying treatment, respectively; the method specifically comprises the following steps:
preparing the first solution in a first container subjected to ultrasonic cleaning and drying treatment by using cobalt nitrate hexahydrate and nickel nitrate hexahydrate as raw materials and methanol as a solvent;
preparing the second solution in a second container subjected to the ultrasonic cleaning and the drying treatment by using dimethyl imidazole as a raw material and the methanol as a solvent;
wherein the processes of preparing the first solution and the second solution are both physical mixing treatment;
step S3, dropwise adding the second solution into the first solution to obtain a mixed solution of the first solution and the second solution, and preparing a CoNi-MOFs precursor suspension by aging the mixed solution;
S4, placing the CoNi-MOFs precursor suspension in a centrifuge for centrifugal treatment to obtain CoNi-MOFs sediment after supernatant liquid is removed, and placing the CoNi-MOFs sediment in a vacuum drying box for drying treatment to obtain CoNi-MOFs powder as a CoNi-MOFs precursor;
and step S5, placing the CoNi-MOFs precursor into a tube furnace for calcination treatment to obtain CoNi-MOFs-800 powder as the broad-spectrum extinction interference material.
According to the method provided by the first aspect of the present invention, in the step S2:
in preparing the first solution, the cobalt nitrate hexahydrate has a mass of 0.45 to 0.55 grams, the nickel nitrate hexahydrate has a mass of 0.45 to 0.55 grams, and the solvent is: 15-25 ml of methanol;
in preparing the second solution, the mass of the dimethylimidazole is 4.15 to 4.25 grams, and the solvent is: 55-65 ml of methanol.
According to the method provided by the first aspect of the present invention, in the step S3, before the second solution is added dropwise to the first solution, the first solution is placed on a magnetic stirrer to be stirred, when the stirring rate reaches 390 to 420 rpm, the dropwise addition of the second solution to the first solution is started, and the stirring rate is maintained at 390 to 420 rpm until the second solution is completely added to the first solution.
According to the method provided by the first aspect of the present invention, in the step S3, the aging treatment time is 23 to 25 hours.
According to the method provided by the first aspect of the present invention, in the step S4, the centrifugation rate of the centrifugation is 7500 to 8500 rpm, and the treatment time of the centrifugation is 8 to 12 minutes.
According to the method provided by the first aspect of the present invention, in the step S4, the drying temperature of the vacuum drying oven is 60 to 80 degrees celsius, and the processing time of the drying process is 17 to 20 hours.
According to the method provided by the first aspect of the invention, in the step S4, the temperature increase rate of the tube furnace is 4 to 6 degrees celsius/minute, the calcination temperature of the calcination process is 750 to 850 degrees celsius, and the treatment time of the calcination process is 100 to 140 minutes.
The second aspect of the present invention provides a wide-spectrum extinction interference material for broadband extinction from an ultraviolet light band to a middle and far infrared band, which is prepared based on the method for preparing the wide-spectrum extinction interference material provided in the first aspect of the present invention.
In conclusion, the structure of the material is designed to optimize the material performance, so that the material has a higher specific surface area, and the scattering and absorption of incident light are enhanced; and the magnetic bimetallic MOFs are used as a precursor in combination with component optimization to increase the complexity of the morphology of the composite material, so that the composite material has better extinction characteristic in multiple bands. The original carbon skeleton structure is destroyed by high-temperature pyrolysis, so that the agglomeration of metal particles is realized, and the composite material with low cost and high photothermal conversion efficiency is obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description in the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow diagram of a method for preparing a broad spectrum extinction interference material in accordance with an embodiment of the invention;
FIGS. 2a to 2d are scanning electron micrographs of specific example 1 and comparative examples 1 to 3 according to an embodiment of the present invention;
FIG. 3 is a graph comparing reflectance curves at 200 nm to 2500 nm for specific example 1 and comparative examples 1 to 3 according to an embodiment of the present invention;
FIGS. 4a to 4d are temperature images of a specific example 1 and comparative examples 1 to 3 according to an embodiment of the present invention irradiated at an illumination intensity of 100 mW for 10 seconds;
FIG. 5 is a graph comparing transmittance curves of specific example 1 and comparative examples 1 to 3 in the mid and far infrared bands of 2.5 to 25 μm according to an embodiment of the present invention;
FIG. 6 is a graph comparing curves of mass extinction coefficients of 2.5 to 25 μm in the mid-and far-infrared bands for specific example 1 and comparative examples 1 to 3 according to an embodiment of the present invention;
FIG. 7 is a thermogravimetric plot comparing specific example 1 and comparative examples 1-3 according to an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for preparing a wide-spectrum extinction interference material, which is used for broadband extinction from an ultraviolet band to a middle and far infrared band. FIG. 1 is a flow diagram of a method for preparing a broad spectrum extinction interference material according to an embodiment of the invention; as shown in fig. 1, the method includes:
step S1, performing ultrasonic cleaning and drying treatment on a first container and a second container by using Wujie powder and deionized water, wherein the first container and the second container are beakers;
step S2 of preparing a first solution and a second solution using the first container and the second container subjected to the ultrasonic cleaning and the drying treatment, respectively; the method specifically comprises the following steps:
Preparing the first solution in a first container subjected to ultrasonic cleaning and drying treatment by using cobalt nitrate hexahydrate and nickel nitrate hexahydrate as raw materials and methanol as a solvent;
preparing the second solution in a second container subjected to the ultrasonic cleaning and the drying treatment by using dimethyl imidazole as a raw material and the methanol as a solvent;
wherein the processes of preparing the first solution and the second solution are both physical mixing treatment;
step S3, dropwise adding the second solution into the first solution to obtain a mixed solution of the first solution and the second solution, and preparing a CoNi-MOFs precursor suspension by aging the mixed solution;
s4, placing the CoNi-MOFs precursor suspension in a centrifuge for centrifugal treatment to obtain CoNi-MOFs sediment after supernatant liquid is removed, and placing the CoNi-MOFs sediment in a vacuum drying box for drying treatment to obtain CoNi-MOFs powder as a CoNi-MOFs precursor;
and step S5, placing the CoNi-MOFs precursor into a tube furnace for calcination treatment to obtain CoNi-MOFs-800 powder as the broad spectrum extinction interference material.
In some embodiments, in said step S2: in preparing the first solution, the cobalt nitrate hexahydrate has a mass of 0.45 to 0.55 grams, the nickel nitrate hexahydrate has a mass of 0.45 to 0.55 grams, and the solvent is: 15-25 ml of methanol; in preparing the second solution, the mass of the dimethylimidazole is 4.15 to 4.25 grams, and the solvent is: 55-65 ml of methanol.
In some embodiments, in the step S3, before the second solution is added dropwise to the first solution, the first solution is placed on a magnetic stirrer for stirring, when the stirring rate reaches 390 to 420 rpm, the dropwise addition of the second solution to the first solution is started, and the stirring rate is maintained at 390 to 420 rpm until the second solution is completely added to the first solution.
In some embodiments, in the step S3, the aging process is performed for 23 to 25 hours.
In some embodiments, in the step S4, the centrifugation rate of the centrifugation process is 7500 to 8500 rpm, and the processing time of the centrifugation process is 8 to 12 minutes.
In some embodiments, in the step S4, the drying temperature of the vacuum drying oven is 60 to 80 degrees celsius, and the processing time of the drying process is 17 to 20 hours.
In some embodiments, in the step S4, the temperature increase rate of the tube furnace is 4 to 6 degrees celsius/minute, the calcination temperature of the calcination process is 750 to 850 degrees celsius, and the treatment time of the calcination process is 100 to 140 minutes.
Specific example 1: preparation method of CoNi-MOFs-800 composite material
0.465 g of Co (NO 3). 6H2O and 0.465 g of Ni (NO 3). 6H2O are weighed and dispersed in 20 ml of methanol to prepare a first solution; a second solution was prepared by weighing 4.198 g of dimethylimidazole and dispersing in 40 ml of methanol. In which the preparation of the first solution and the second solution is only a physical mixing process, not a chemical reaction process (the same hereinafter).
The first solution was placed on a magnetic stirrer and stirred at a rate of 400 rpm while the second solution was added dropwise to the first solution until the second solution was completely added to the first solution, and stirring was stopped.
The resulting mixed solution was allowed to stand for 24 hours, and allowed to react completely by aging.
And centrifuging the aged suspension in a centrifuge, wherein the centrifuging time is set to be 10 minutes, and the centrifuging speed is set to be 8000 revolutions per minute.
And centrifuging the centrifuge to obtain a solution, removing supernatant to obtain a precipitate, and drying the precipitate in a vacuum drying oven at 70 ℃ for 18 hours.
And placing the dried powder into a tubular furnace for calcination, wherein the temperature rise rate of the tubular furnace is 5 ℃ per minute, the calcination temperature is 800 ℃, and the calcination time is 120 minutes.
Comparative example 1 of specific example 1: preparation method of CoNi-MOFs composite material
0.465 g of Co (NO 3). 6H2O and 0.465 g of Ni (NO 3). 6H2O are weighed and dispersed in 20 ml of methanol to prepare a first solution; a second solution was prepared by weighing 4.198 g of dimethylimidazole and dispersing in 40 ml of methanol.
The first solution was placed on a magnetic stirrer and stirred at a rate of 400 rpm while the second solution was added dropwise to the first solution until the second solution was completely added to the first solution, and stirring was stopped.
The resulting mixed solution was allowed to stand for 24 hours, and allowed to react completely by aging.
And centrifuging the aged suspension in a centrifuge, wherein the centrifuging time is set to be 10 minutes, and the centrifuging speed is set to be 8000 revolutions per minute.
And centrifuging the centrifuge to obtain a solution, removing supernatant to obtain a precipitate, and drying the precipitate in a vacuum drying oven at 70 ℃ for 18 hours.
Comparative example 2 of specific example 1: preparation method of CoNi-MOFs-400 composite material
Other procedures were the same as in example 1, and the tube furnace calcination temperature was 400 ℃.
Comparative example 3 of specific example 1: preparation method of CoNi-MOFs-600 composite material
Other procedures were the same as in example 1, and the tube furnace calcination temperature was 600 ℃.
Analysis of results
FIGS. 2a to 2d are scanning electron micrographs of specific example 1 according to an embodiment of the present invention and comparative examples 1 to 3; as shown in fig. 2a-2d, the comparative example one has a complete three-dimensional structure, the particle radius is between 500nm-1um, and as the pyrolysis temperature increases, the original carbon skeleton structure is gradually destroyed, and the particle structure is in an amorphous state, which shows that the metal nano-crystal is attached to the amorphous carbon (example one). This is because the metal ion is reduced to zero valence state at high temperature, and the carbon skeleton loses the corresponding connecting particles and is dissociated at high temperature.
FIG. 3 is a graph comparing reflectance curves at 200 nm to 2500 nm for specific example 1 and comparative examples 1-3 according to an embodiment of the present invention; as shown in fig. 3, the reflectance of the first example from 200 nm to 2500 nm is stabilized at about 5%, showing that it has no differential absorption in the wavelength band, while the reflectance of the first comparative example, the second comparative example and the third comparative example is higher than that of the first example, and the reflectance of the first comparative example and the second comparative example from 200 nm to 2500 nm shows a fluctuating state, showing that the absorption in the wavelength band is selective, and no differential absorption can be achieved.
FIGS. 4a to 4d are temperature images of a specific example 1 according to an embodiment of the present invention and comparative examples 1 to 3 irradiated at an illumination intensity of 100 mW for 10 seconds; as shown in fig. 4a to 4d, the surface temperature of the first example reached 96.63 c when irradiated for 10 seconds at an illumination intensity of 100 mw, while the surface temperature of the first comparative example was 69.53 c, the surface temperature of the second comparative example was 80.68 c, the surface temperature of the third comparative example was 88.15 c, and the performance of the three comparative examples was different from that of the first example.
FIG. 5 is a schematic representation of a system according to the present inventionThe specific example 1 of the example and the comparative examples 1 to 3 are a graph comparing transmittance curves in the mid-and far-infrared wavelength bands of 2.5 to 25 μm; FIG. 6 is a graph comparing curves of mass extinction coefficients of 2.5 to 25 μm in the mid-and far-infrared bands for specific example 1 and comparative examples 1 to 3 according to an embodiment of the present invention; as shown in fig. 5 and 6, under the same conditions, the average transmittance in this wavelength band was 82.21% for example one, 86.97% for comparative example one, 86.11% for comparative example two, and 83.94 for comparative example three. Correspondingly, under the same conditions, the average mass extinction coefficient of the embodiment I in the waveband is 2.608m 2In g, while the average mass extinction coefficient of comparative example one was 1.860m2(g) average mass extinction coefficient of comparative example one is 1.990m2In g, the average mass extinction coefficient of comparative example one is 2.335m2(ii) in terms of/g. In comparison, the first embodiment has better mid-far infrared extinction performance.
FIG. 7 is a thermogravimetric plot comparison graph (in the range of 0-800 ℃) of specific example 1 and comparative examples 1-3 according to an embodiment of the present invention; as shown in fig. 7, in the first embodiment, the mass reduction is minimal during the heating process, the mass reduction speed is also slowest, and when the temperature reaches 800 ℃, the mass loss is only 44.37%; under the same conditions, the mass loss of the comparative example I is 82.82%, the mass loss of the comparative example II is 72.29%, and the mass loss of the comparative example III is 66.86%, so that the example I has the best thermal stability.
In conclusion, the structure of the material is designed to realize the optimization of the material performance, so that the material has higher specific surface area and is beneficial to enhancing the scattering and absorption of incident light; and the magnetic bimetallic MOFs are used as a precursor in combination with component optimization to increase the complexity of the morphology of the composite material, so that the composite material has better extinction characteristic in multiple bands. The original carbon skeleton structure is destroyed by high-temperature pyrolysis, so that the agglomeration of metal particles is realized, and the composite material with low cost and high photothermal conversion efficiency is obtained.
The beneficial technical effects of the invention comprise: (1) the wide-spectrum extinction interference material can simultaneously act on ultraviolet light, visible light, near infrared and middle and far infrared wave bands, the wave bands are in a concentrated area of solar radiation energy, and the coverage spectrum is wide; (2) the composite material prepared by the invention has higher photo-thermal conversion efficiency, and can be used as a preferable material for super capacitors and seawater desalination; (3) the composite material prepared by the invention has simple preparation process, wide raw material source and low price, and is easy to carry out large-scale industrial production.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for preparing a broad spectrum extinction interference material for broadband extinction of ultraviolet to mid-far infrared bands, the method comprising:
Step S1, performing ultrasonic cleaning and drying treatment on a first container and a second container by using five cleaning powder and deionized water, wherein the first container and the second container are beakers;
step S2 of preparing a first solution and a second solution using the first container and the second container subjected to the ultrasonic cleaning and the drying treatment, respectively; the method specifically comprises the following steps:
preparing the first solution in a first container subjected to ultrasonic cleaning and drying treatment by using cobalt nitrate hexahydrate and nickel nitrate hexahydrate as raw materials and methanol as a solvent;
preparing the second solution in a second container subjected to the ultrasonic cleaning and the drying treatment by using dimethyl imidazole as a raw material and the methanol as a solvent;
wherein the processes of preparing the first solution and the second solution are both physical mixing treatment;
step S3, dropwise adding the second solution into the first solution to obtain a mixed solution of the first solution and the second solution, and preparing a CoNi-MOFs precursor suspension by aging the mixed solution;
s4, placing the CoNi-MOFs precursor suspension in a centrifuge for centrifugal treatment to obtain CoNi-MOFs sediment after supernatant liquid is removed, and placing the CoNi-MOFs sediment in a vacuum drying box for drying treatment to obtain CoNi-MOFs powder as a CoNi-MOFs precursor;
And step S5, placing the CoNi-MOFs precursor into a tube furnace for calcination treatment to obtain CoNi-MOFs-800 powder as the broad spectrum extinction interference material.
2. The method for preparing a broad spectrum extinction interference material according to claim 1, wherein in step S2:
in preparing the first solution, the cobalt nitrate hexahydrate has a mass of 0.45 to 0.55 grams, the nickel nitrate hexahydrate has a mass of 0.45 to 0.55 grams, and the solvent is: 15-25 ml of methanol;
in preparing the second solution, the mass of the dimethylimidazole is 4.15 to 4.25 grams, and the solvent is: 55-65 ml of methanol.
3. The method according to claim 2, wherein in step S3, before the second solution is added dropwise into the first solution, the first solution is placed on a magnetic stirrer to be stirred, when the stirring rate reaches 390 to 420 rpm, the dropwise addition of the second solution into the first solution is started, and the stirring rate is maintained at 390 to 420 rpm until the second solution is completely added into the first solution.
4. The method according to claim 3, wherein the aging treatment is carried out for 23 to 25 hours in step S3.
5. The method of claim 4, wherein in step S4, the centrifugation rate is 7500 to 8500 rpm and the centrifugation time is 8 to 12 minutes.
6. The method according to claim 5, wherein in the step S4, the drying temperature of the vacuum drying oven is 60 to 80 degrees Celsius, and the processing time of the drying process is 17 to 20 hours.
7. The method according to claim 1, wherein in the step S4, the temperature rise rate of the tube furnace is 4 to 6 degrees Celsius/min, the calcination temperature of the calcination process is 750 to 850 degrees Celsius, and the treatment time of the calcination process is 100 to 140 minutes.
8. A broad-spectrum extinction interference material for broadband extinction of ultraviolet to mid-and far-infrared bands, which is prepared based on a method for preparing a broad-spectrum extinction interference material according to any one of claims 1 to 7.
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