CN117343693A - FeSiB-based double-layer core-shell structure wave-absorbing color-changing material and preparation method thereof - Google Patents
FeSiB-based double-layer core-shell structure wave-absorbing color-changing material and preparation method thereof Download PDFInfo
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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
- 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
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
Abstract
The invention relates to the technical field of a wave-absorbing color-changing material, and discloses a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material and a preparation method thereof, wherein the preparation method comprises the following steps: placing a quartz boat filled with spherical FeSiB alloy into a CVD rotary furnace, starting the rotary furnace, heating the rotary furnace to 750-1100 ℃, and then introducing inert gas loaded with ethanol into the rotary furnace for reaction to prepare carbon-coated spherical FeSiB powder; uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, and heating in a water bath at 120-200 ℃ for 8-32h to obtain a mixed solution; and washing the mixed solution by adopting absolute ethyl alcohol, then carrying out magnetic separation and drying to obtain the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material. The wave-absorbing color-changing material prepared by the invention has better impedance matching and larger reflection loss value, and a larger water contact angle ensures good water absorption and dehydration performance, and can realize the wet color-changing effect, thereby having better wave-absorbing performance and color-changing performance.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing color-changing materials, and particularly relates to a FeSiB-based wave-absorbing color-changing material with a double-layer core-shell structure and a preparation method thereof.
Background
With the development of 5G technology, electronic technology is widely applied to the fields of communication, industry, military, electronic equipment and the like, and electronic equipment and wireless communication are rushing into the lives of people, so that many convenience is brought to daily life. Meanwhile, the harm of electromagnetic radiation to human health and electrical equipment is increasingly prominent, and becomes a serious environmental pollution problem, which is attracting a great deal of attention worldwide. Thus, control of electromagnetic wave radiation and pollution is urgent. Microwave absorbing materials can convert electromagnetic wave energy into thermal energy or dissipate it, providing an effective way to solve this problem. In the military field, under the transformation of different environments (forest, desert and ocean), the color of the wave-absorbing material is too single, so that the stealth effect of the wave-absorbing material is reduced, and even in the environment with larger color contrast, the stealth function of the wave-absorbing material is lost. How to meet the requirements of high-performance wave-absorbing materials with easy color change, thin thickness, strong absorption and light weight is a great challenge for wave-absorbing materials. Therefore, it is urgent to develop a bifunctional material having good microwave absorbing and discoloration properties.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material and a preparation method thereof, and aims to solve the problems of poor color-changing capability, larger reflection loss and unmatched electromagnetic impedance of the existing wave-absorbing material.
The technical scheme of the invention is as follows:
a preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the following steps:
placing a quartz boat filled with spherical FeSiB alloy into a CVD rotary furnace, and then introducing inert gas with the gas flow rate of 20-70ml/min into the rotary furnace to empty the air in the rotary furnace;
starting a rotary furnace, heating the interior of the rotary furnace to 750-1100 ℃, and then introducing inert gas loaded with ethanol into the rotary furnace, wherein the gas flow is 20-70ml/min, and the reaction time is 20-40min; stopping introducing inert gas after the reaction is completed, naturally cooling to room temperature, and taking out to obtain carbon-coated spherical FeSiB powder;
uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, and heating in a water bath at 120-200 ℃ for 8-32h to obtain a mixed solution;
washing the mixed solution by absolute ethyl alcohol, then carrying out magnetic separation and drying to obtain NiBr 2 C in-situ polymerized spherical FeSiB composite material, namely FeSiB-based double-layer core-shell structure wave-absorbing color-changing material.
The preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the step of preparing a composite material, wherein the inert gas is one or more of helium, nitrogen and argon.
The preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the step of uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, wherein the carbon-coated spherical FeSiB powder is 5-20 parts, the nickel nitrate pentahydrate is 3-9 parts, the potassium bromide is 1.5-4.5 parts and the deionized water is 50-80 parts in weight.
The preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the following steps of (1) preparing a carbon-coated spherical FeSiB powder material and nickel nitrate pentahydrate in a weight ratio of 2:1.
The preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the step of starting a rotary furnace, wherein the rotating speed of the rotary furnace is 20-40r/min.
The preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the steps of washing the mixed solution with absolute ethyl alcohol, then performing magnetic separation, and drying at 47-70 ℃.
The FeSiB-based double-layer core-shell structure wave-absorbing color-changing material is prepared by adopting the preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material.
The beneficial effects are that: the preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material provided by the invention has the advantages of low cost, mild process conditions, convenience in operation and easiness in large-scale industrial application of products; and NiBr prepared by the invention 2 Spherical FeSiB composite material prepared by in-situ polymerization of-CFeSiB@C@NiBr 2 ) The water-absorbing and dewatering agent has better impedance matching and larger reflection loss value, a larger water contact angle ensures good water-absorbing and dewatering performance, and can realize the effect of wet-induced color change, thereby having better wave-absorbing performance and color change performance and being beneficial to the practical application in the field of national defense and military industry.
Drawings
FIG. 1 is a flow chart of a preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material.
FIG. 2 is an SEM image of the spherical FeSiB alloy of the present invention before and after cladding; wherein a and b are SEM pictures of spherical FeSiB alloy before cladding, c and d are SEM pictures of FeSiB@C obtained in example 1, and e and f are FeSiB@C@NiBr obtained in example 1 2 SEM images of (a).
FIG. 3 shows a spherical FeSiB alloy of the present invention, feSiAl@C obtained in example 1 and FeSiAl@C@NiBr obtained in example 1 2 Is a XRD pattern of (C).
FIG. 4 shows a spherical FeSiB alloy of the present invention, feSiAl@C obtained in example 1 and FeSiAl@C@NiBr obtained in example 1 2 Is a Raman spectrum of (c).
FIG. 5 shows the hydrothermal synthesis of FeSiB@C@NiBr under the conditions of nickel nitrate pentahydrate and potassium bromide with different concentrations 2 Wave absorbing properties of the sample; wherein (a, d) is FeSiB@C@NiBr obtained in example 1 2 (b, e) is FeSiB@C@NiBr obtained in example 2 2 (c, f) is FeSiB@C@NiBr obtained in example 3 2 Is a graph of the wave absorbing performance of (a).
FIG. 6 shows FeSiB@C@NiBr obtained in example 1 of the invention 2 Color change process diagram of composite structure under different conditions.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments.
Magnetic metal powders have excellent magnetic properties, and have recently emerged as various wave-absorbing materials. Spherical FeSiB metal powder is a soft magnetic material, which has received considerable attention recently among various wave absorbers, in terms of its high magnetic permeability, relatively low resistivity, high saturation magnetization and no noble metal content. Spherical FeSiB metal powder has higher magnetic loss capability in the microwave frequency band, but the dielectric constant of the spherical FeSiB metal powder is far greater than the magnetic permeability, so that serious impedance mismatch is caused. Since FeSiB metal powder alone does not achieve optimal wave-absorbing performance, it is necessary to combine with other materials to improve its impedance matching and increase attenuation constant to enhance microwave absorption. The composite low dielectric material on the surface of the spherical FeSiB can adjust the impedance matching, is an effective method for improving the microwave absorption capacity, and effectively reduces the complex dielectric constant of the composite material, thereby adjusting and controlling the impedance matching with free space and enhancing the wave absorbing effect. And the outermost layer of the surface of the FeSiB metal powder is coated with a layer of color-changing material, so that the surface interface polarization of the wave-absorbing material can be increased, the wave-absorbing performance of the wave-absorbing material can be improved, the color of the wave-absorbing material can be gradually changed along with the change of the environment, the wave-absorbing material is integrated with the surrounding environment, the stealth effect of the material is enhanced, and the FeSiB-based composite material has the dual functions of wave-absorbing and color-changing.
Based on the above, the invention provides a preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material, as shown in figure 1, which comprises the following steps:
s10, placing a quartz boat filled with spherical FeSiB alloy into a CVD rotary furnace, and then introducing inert gas with the gas flow rate of 20-70ml/min into the rotary furnace to empty the air in the rotary furnace;
s20, starting a rotary furnace, heating the temperature in the rotary furnace to 750-1100 ℃, and then introducing inert gas loaded with ethanol into the rotary furnace, wherein the gas flow is 20-70ml/min, and the reaction time is 20-40min; stopping introducing inert gas after the reaction is completed, naturally cooling to room temperature, and taking out to obtain carbon-coated spherical FeSiB powder;
s30, uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, and heating in a water bath at 120-200 ℃ for 8-32h to obtain a mixed solution;
s40, washing the mixed solution by adopting absolute ethyl alcohol, then carrying out magnetic separation and drying to obtain NiBr 2 -C in situ polymerizationThe spherical FeSiB composite material is a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material.
Specifically, the invention adopts a chemical vapor deposition method, and firstly, a carbon layer structure is coated on the surface of spherical FeSiB at the temperature of 750-1100 ℃ in a furnace to obtain FeSiB@C powder; then, feSiB@C powder is added into a mixed solution of nickel nitrate pentahydrate and potassium bromide by adopting a hydrothermal synthesis method, and the mixture is heated in a water bath for 8-32 hours at 120-200 ℃ to enable nickel bromide generated by the reaction to polymerize on the surface of spherical FeSiB@C in situ. FeSiB@C@NiBr prepared by the method 2 The micro-morphology is spherical, the grain diameter is about 15 mu m, the surface is of a nano-sheet array structure, the surface interface polarization is improved compared with FeSiB and FeSiB@C, the stability and the specific surface area are good, and NiBr is polymerized on the surface of FeSiB@C in situ 2 The core-shell structure effectively improves the microwave absorption performance and the color-changing performance of the spherical FeSiB soft magnetic powder. Spherical FeSiB@C@NiBr prepared by the method 2 The core-shell structure has better impedance matching and larger reflection loss value, and a larger water contact angle ensures good water absorption and dehydration performance, thus realizing the effect of wet color change; therefore, the composite material has better wave absorbing performance and color changing performance, and is beneficial to the practical application in the field of national defense and military industry.
In some embodiments, the inert gas is one or more of helium, nitrogen, and argon, but is not limited thereto.
In some embodiments, in the step of uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, the carbon-coated spherical FeSiB powder is used in an amount of 5-20 parts by weight, the nickel nitrate pentahydrate is used in an amount of 3-9 parts by weight, the potassium bromide is used in an amount of 1.5-4.5 parts by weight, and the deionized water is used in an amount of 50-80 parts by weight. Experiments in the embodiment show that in the weight part range, the nickel bromide generated by the reaction can be polymerized on the surface of the spherical FeSiB@C to form NiBr with a double-layer core-shell structure 2 -C spherical FeSiB composite polymerized in situ.
In some specific embodiments, the weight ratio of the carbon-coated spherical FeSiB powder to the nickel nitrate pentahydrate is 2:1, but is not limited thereto.
In some embodiments, the rotating furnace is started at a rotating speed of 20-40r/min, but is not limited thereto.
In some embodiments, the mixed solution is washed with absolute ethanol, then magnetically separated, and dried at 47-70 deg.c, but is not limited thereto.
In some embodiments, a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material is further provided, wherein the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material is prepared by the preparation method.
The invention is further illustrated by the following examples:
example 1
A preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the following steps:
putting 20g of spherical FeSiB alloy powder into a quartz boat and placing the quartz boat into a CVD rotary furnace, and then introducing nitrogen with the air flow of 50ml/min into the furnace to exhaust air in a hollow pipe; starting a CVD rotary furnace, and increasing the temperature in the furnace to 800 ℃; then, firstly introducing nitrogen into the ethanol solution, then introducing nitrogen loaded with ethanol into the furnace, wherein the air flow is 50ml/min, and the reaction is 30min; after the reaction is finished, stopping introducing inert gas, naturally cooling to room temperature, and taking out to obtain a spherical FeSiB@C sample uniformly coated with carbon;
uniformly mixing 10g of prepared spherical FeSiB@C powder, 3g of nickel nitrate pentahydrate, 1.5g of potassium bromide and 50g of deionized water, and heating in a water bath at 150 ℃ for 24 hours to obtain a mixed solution A;
washing the mixed solution A by absolute ethyl alcohol for 6 times, magnetically separating and drying to obtain NiBr with double-layer core-shell structure 2 Spherical FeSiAl@C@NiBr polymerized in situ 2 A composite material.
The prepared FeSiAl@C@NiBr 2 The mass ratio of the composite material to the paraffin is 7:3 are pressed into coaxial ring samples and their electromagnetic parameters are measured using an N5230A vector network analyzer in the frequency range of 0.5GHz-18.0 GHz. Electromagnetic parameters of different structures can reflect the microwave absorption performance of the materialGood or bad(s) of (a).
Example 2
A preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the following steps:
this embodiment differs from embodiment 1 in that: the prepared spherical FeSiB@C powder 15g, nickel nitrate pentahydrate 6g, potassium bromide 3g and 60g deionized water are uniformly mixed and heated in a water bath at 150 ℃ for 24 hours to obtain a mixed solution A. The remaining steps were the same as in example 1. Obtain the NiBr with a double-layer core-shell structure 2 Spherical FeSiAl@C@NiBr polymerized in situ 2 A composite material.
Example 3
A preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material comprises the following steps:
this embodiment differs from embodiment 1 in that: uniformly mixing 20g of prepared spherical FeSiB@C powder, 9g of nickel nitrate pentahydrate, 4.5g of potassium bromide and 80g of deionized water, and heating in a water bath at 150 ℃ for 24 hours to obtain a mixed solution A. The remaining steps were the same as in example 1. Obtain the NiBr with a double-layer core-shell structure 2 Spherical FeSiAl@C@NiBr polymerized in situ 2 A composite material.
Test case
For the spherical FeSiB alloy, feSiB@C and FeSiB@C@NiBr in example 1 2 The result of electron microscope photographing is shown in FIG. 2, wherein a and b in FIG. 2 are SEM images of spherical FeSiB alloy at 100um, c and d in FIG. 2 are SEM images of FeSiB@C at 5um and 1um, and e and f in FIG. 2 are FeSiB@C@NiBr 2 From the SEM image at 1um, it can be seen that the morphology of the FeSiB alloy powder is as shown in fig. 2 (a, b), the average diameter of the prepared FSB alloy powder is about 10-15 μm, the spherical powder surface is smooth, and the sphericity is good. The carbon synthesis FSB@C hybridization was deposited on the FeSiB surface by CCVD process, and a plurality of nano-sized small particles appeared on the FeSiB microsphere surface, and the hybridized particles coupled with the nano particles were formed respectively, as shown in FIG. 2 (c, d). FeSiB@C@NiBr was observed by high magnification SEM 2 Meets the gradient structure, discovers that the FSB@C microsphere is grown on the NiBr on the surface 2 The nanoplatelets are uniformly covered, without excessive local accumulation, uniformly distributed, and the nanoplateletsThe average length of the sheet may reach hundreds of nanometers, as shown in fig. 2 (e-f).
For the spherical FeSiB alloy, feSiB@C and FeSiB@C@NiBr in example 1 2 X-ray diffraction analysis was performed to obtain an XRD pattern as shown in FIG. 3. As can be seen in FIG. 3, niBr 2 -C in situ polymerized on the spherical FeSiB surface.
For the spherical FeSiB alloy, feSiB@C and FeSiB@C@NiBr in example 1 2 Chemical elemental analysis was performed to obtain a Raman spectrum as shown in FIG. 4, and FeSiB@C and FeSiB@C@NiBr were found in FIG. 4 2 At 1348cm -1 (D band) and 1580cm -1 Two distinct peaks appear near (G band), indicating carbon deposition at FSB@C and FSB@C@NiBr 2 Is a surface of the substrate. Further FSB@C@NiBr 2 With a higher I D /I G (1.03) shows that the material has higher charge transfer capability, and is beneficial to improving dielectric loss and microwave energy dissipation.
For FeSiB@C@NiBr prepared in examples 1-3 2 The sample was subjected to a Hill Performance test, the results of which are shown in FIG. 5, wherein a and d are FeSiB@C@NiBr obtained in example 1 2 B and e are FeSiB@C@NiBr obtained in example 2 2 C and f are FeSiB@C@NiBr obtained in example 3 2 Is a graph of the wave absorbing performance of (a). In FIG. 5 (c, f) it is shown that FSB@C@NiBr 2 The sample reached-59 dB at 3.0mm, and the effective bandwidth covered almost the entire X-band (8.0-12.0 GHz). Notably, under hydrothermal synthesis conditions, niBr 2 Rich interfaces (nanoplatelet arrays) and dipole polarization are brought about at fsb@c. The unique nano-sheet structure can promote the entry and reflection attenuation of electromagnetic waves, thereby improving the absorption performance of the composite gradient material. In contrast, the pure FSB and FSB@C have only limited RL values of-23 dB at 3.0mm (FIG. 5 (a, d)) and-33 dB at 3.5mm (FIG. 5 (b, e)), respectively, indicating that FSB and FSB@C are disadvantageous for practical use.
FeSiB@C@NiBr prepared in example 1 2 The sample was subjected to a color change test under different conditions, and the results are shown in FIG. 6. As can be seen from the results in FIG. 6, feSiB@C@NiBr was obtained at room temperature and humidity of 50% 2 Gradually absorbs moisture, and the time for changing the color from yellow to green is longer, which is about 80s. When the temperature reaches 55 ℃ and the humidity is 10 percent, feSiB@C@NiBr 2 The water is rapidly lost, and the time for converting the color of the water from green to yellow is short, which is about 40s.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (7)
1. A preparation method of a FeSiB-based double-layer core-shell structure wave-absorbing color-changing material is characterized by comprising the following steps:
placing a quartz boat filled with spherical FeSiB alloy into a CVD rotary furnace, and then introducing inert gas with the gas flow rate of 20-70ml/min into the rotary furnace to empty the air in the rotary furnace;
starting a rotary furnace, heating the interior of the rotary furnace to 750-1100 ℃, and then introducing inert gas loaded with ethanol into the rotary furnace, wherein the gas flow is 20-70ml/min, and the reaction time is 20-40min; stopping introducing inert gas after the reaction is completed, naturally cooling to room temperature, and taking out to obtain carbon-coated spherical FeSiB powder;
uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, and heating in a water bath at 120-200 ℃ for 8-32h to obtain a mixed solution;
washing the mixed solution by absolute ethyl alcohol, then carrying out magnetic separation and drying to obtain NiBr 2 C in-situ polymerized spherical FeSiB composite material, namely FeSiB-based double-layer core-shell structure wave-absorbing color-changing material.
2. The method for preparing the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material according to claim 1, wherein the inert gas is one or more of helium, nitrogen and argon.
3. The method for preparing the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material according to claim 1, wherein in the step of uniformly mixing the carbon-coated spherical FeSiB powder, nickel nitrate pentahydrate, potassium bromide and deionized water, the carbon-coated spherical FeSiB powder is used in an amount of 5-20 parts by weight, the nickel nitrate pentahydrate is used in an amount of 3-9 parts by weight, the potassium bromide is used in an amount of 1.5-4.5 parts by weight, and the deionized water is used in an amount of 50-80 parts by weight.
4. The preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material is characterized in that the weight ratio of the carbon-coated spherical FeSiB powder to the nickel nitrate pentahydrate is 2:1.
5. The method for preparing the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material according to claim 1, wherein in the step of starting the rotary furnace, the rotating speed of the rotary furnace is 20-40r/min.
6. The method for preparing the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material according to claim 1, wherein absolute ethyl alcohol is adopted to wash the mixed solution, then magnetic separation is carried out, and in the step of drying, the drying temperature is 47-70 ℃.
7. The FeSiB-based double-layer core-shell structure wave-absorbing color-changing material is characterized by being prepared by adopting the preparation method of the FeSiB-based double-layer core-shell structure wave-absorbing color-changing material according to any one of claims 1-6.
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