CN110591641A - Fe2O3@ MXene composite powder and preparation method thereof - Google Patents
Fe2O3@ MXene composite powder and preparation method thereof Download PDFInfo
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Abstract
The invention provides Fe2O3The @ MXene composite powder and the preparation method thereof comprise the following steps: step 1, adding Fe2O3Mixing MXene powder with (1-3): 1, and stirring at constant temperature at room temperature until the components are fully mixed; step 2, drying the mixed composite material to constant weight at room temperature to obtain Fe2O3@ MXene composite powder; mixing Fe2O3Mixing with MXene powder, high Fe content2O3Nanoparticles attached to the lamellar boundaries of MXene powders, Fe2O3The nanometer particles have uniform granularity and no agglomeration phenomenon, and the MXene powder has better interlamellar spacing uniformity; doping MXene powder with Fe2O3The nano particles can reduce the real part epsilon 'and the imaginary part epsilon' of the dielectric constant, increase the real part mu 'and the imaginary part mu' of the magnetic conductivity and increase the loss tangent value tan delta; in MXene powderMiddle doped Fe2O3The reflectivity loss of the composite material of the nano particles is reduced, and the maximum absorption peak moves to low frequency, which means that the wave absorbing capacity is improved. And the method has low preparation cost, short production period and environmental protection.
Description
Technical Field
The invention relates to the field of wave-absorbing materials, and particularly relates to Fe2O3A @ MXene composite powder and a preparation method thereof.
Background
The ferrite material is used as an important absorbent of electromagnetic waves, is a double-composite dielectric material, has both magnetic and dielectric properties, so that the ferrite material has good wave-absorbing property, low cost and small volume, and has not only magnetic absorption but also electric absorption on the electromagnetic waves in the aspect of impedance matching; in terms of attenuation matching, magnetic loss and electric loss are also sources of loss of electromagnetic waves, and the combination of the two can enable the electromagnetic waves to obtain maximum absorption and loss. The ferrite material also avoids the disadvantages such as high density, narrow absorption band and poor high temperature resistance.
Fe2O3As an iron oxide compound which is most stable at room temperature, it has good magnetic properties, low toxicity, high compatibility and strong spin polarization at room temperature, however, it is limited in high technical fields due to its inherent defects such as high density, poor temperature stability, non-ideal low-frequency absorption properties, etc.
The MXene material has the advantages of light weight, high dielectric constant, good matching property and the like, and is a potential wave-absorbing material. MXene and a magnetic wave absorbing agent are compounded to prepare a binary or multi-element composite material, which is an effective way for expanding wave absorbing frequency band, enhancing wave absorbing effect and reducing material quality.
Nano Fe2O3The fatal defect of the powder is that the surface activity is extremely high, so that serious agglomeration is caused. Therefore, the nano Fe2O3 can be loaded on the surface of the MXene serving as the emerging material to prepare Fe2O3the/MXene composite powder. In the composite powder, Fe2O3The iron oxide particles are uniformly distributed on the MXene sheet layer, so that the agglomeration phenomenon of the iron oxide particles and the MXene can be effectively reduced.
Mixing Fe2O3The composite material is compounded with MXene material, double loss absorption is realized, and the wave absorbing performance of the material is obviously improved.
At present, the reflection loss of the wave-absorbing material prepared by domestic doped articles and patents related to ferrite is poor at low frequency, and the ferrite is doped into MXene powder to form Fe2O3The research of the @ MXene composite material at low frequency is not available at present.
For example: chinese patent CN107541185A (application No. 201710661545.0) discloses different Zn2+The emission loss curve of the zinc-doped ferrite/carbon nanotube composite nanoparticle with the doping amount. There is a maximum reflection loss at high frequency 15.0GHz, approximately-23 dB. But the reflection loss at the GHz position (8.2-12.4) of the low frequency is basically near-4 dB, Zn2+The doping level has the highest reflection loss at 20%, approximately-10 dB.
Two-dimensional layered Ti3C2TXAnd preparation of composite materials and research on wave-absorbing properties [ D]Black longjiang, harabin university of industry, 2017. The magnetic permeability is low, the reflection of wave absorption performance can not be seen at (8-15) GHz, and the highest reflection loss is approximately-35 dB at 17 GHz.
Disclosure of Invention
The invention provides Fe2O3The @ MXene composite powder and the preparation method thereof solve the defects.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides Fe2O3The preparation method of the @ MXene composite powder comprises the following steps:
step 1, adding Fe2O3Mixing MXene powder with (1-3): 1, and stirring at constant temperature at room temperature until the components are fully mixed;
step 2, drying the mixed composite material to constant weight at room temperature to obtain Fe2O3@ MXene composite powder.
Preferably, in step 1, Fe2O3Mixing with MXene powder at a ratio of 1:1, were mixed.
Preferably, in step 1, the preparation of MXene powder comprises the following steps:
s1, weighing 3g of titanium-aluminum-carbon, slowly adding the titanium-aluminum-carbon into 60ml of hydrofluoric acid with the concentration of 40%, and uniformly stirring;
s2, ultrasonically cleaning the stirred mixed solution;
and S3, centrifuging the mixed solution subjected to ultrasonic cleaning by using deionized water until the pH is neutral, and drying at room temperature to obtain MXene powder.
Preferably, in step 1, Fe2O3A method of preparing a powder comprising the steps of:
s1, respectively weighing 60g of deionized water and 32g of absolute ethyl alcohol, and mixing the two to serve as a solvent;
s2, respectively weighing 21.014g of citric acid and 40.4g of ferric nitrate, adding the citric acid and the ferric nitrate into the solvent of S1, placing the mixture on a magnetic stirrer, stirring and dissolving the mixture to prepare a precursor, and stirring the precursor at a constant temperature to obtain wet gel;
s3, drying and foaming the wet gel in the S2 to obtain dry gel, and calcining the dry gel to obtain the ferric oxide powder.
Fe2O3The @ MXene composite powder is prepared based on a preparation method.
Fe2O3The preparation method of the @ MXene composite powder comprises the following steps:
step 1, preparing MXene dispersion liquid;
step 2, mixing the MXene dispersion liquid prepared in the step 1 with Fe (NO)3)3·9H2Fully mixing the O in a molar ratio of 1 (1-3), and then placing the mixture in a hydrothermal kettle for reaction; after the reaction is finished, naturally cooling;
and 3, sequentially washing, centrifuging and drying the product obtained in the step 2 to constant weight to obtain Fe2O3@ MXene composite powder.
Preferably, the preparation of MXene powder in step 1 comprises the following steps:
s1, weighing 3g of titanium-aluminum-carbon, slowly adding the titanium-aluminum-carbon into 60ml of hydrofluoric acid with the concentration of 40%, and uniformly stirring;
s2, ultrasonically cleaning the stirred mixed solution;
and S3, centrifuging the mixed solution subjected to ultrasonic cleaning by using deionized water until the pH is neutral, and drying at room temperature to obtain MXene powder.
Preferably, the preparation of the MXene dispersion in step 1: adding MXene powder into DMF, and carrying out ultrasonic washing to obtain MXene dispersion liquid.
Fe2O3The @ MXene composite powder is prepared based on a preparation method.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides Fe2O3Preparation method of @ MXene composite powder by mixing Fe2O3Mixing with MXene powder, high Fe content2O3Nanoparticles attached to the lamellar boundaries of MXene powders, Fe2O3The nanometer particles have uniform granularity and no agglomeration phenomenon, and the MXene powder has better interlamellar spacing uniformity; doping MXene powder with Fe2O3The nano particles can reduce the real part epsilon 'and the imaginary part epsilon' of the dielectric constant, increase the real part mu 'and the imaginary part mu' of the magnetic conductivity and increase the loss tangent value tan delta; doping MXene powder with Fe2O3The reflectivity loss of the composite material of the nano particles is reduced, and the maximum absorption peak moves to low frequency, which means that the wave absorbing capacity is improved. And the method has low preparation cost, short production period and environmental protection.
Drawings
FIG. 1 shows Fe prepared by direct mixing method2O3SEM picture of @ MXene composite powder;
FIG. 2 is Fe2O3The XRD patterns of the @ MXene composite powder and the MXene phase;
FIG. 3 shows that the composite material varies with Fe2O3Doping concentration composite powderWherein fig. 3a is a graph of the dielectric parameter epsilon 'with frequency, fig. 3b is a graph of the dielectric parameter epsilon "with frequency, fig. 3c is a graph of the dielectric parameter mu' with frequency, fig. 3d is a graph of the dielectric parameter mu" with frequency, fig. 3e is a graph of the dielectric parameter tan delta with frequency;
FIG. 4 shows the composite material varying with Fe2O3The wave-absorbing curve of the composite powder with doping concentration and different sample thicknesses, wherein fig. 4a is 1:1, fig. 4b is 1: 2, fig. 4c is 1: 3, wave-absorbing curve diagram;
FIG. 5 shows different Fe with the same thickness in the frequency range of (8.2-12.4) GHz2O3A wave absorption curve chart of a doping concentration powder sample;
FIG. 6 shows Fe prepared by two preparation methods2O3SEM comparative picture of @ MXene composite powder.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention provides Fe2O3The preparation method of the @ MXene composite powder comprises the following steps:
step 1, adding Fe2O3Mixing MXene powder with (1-3): 1, and stirring at room temperature for 0.5h to enable Fe2O3Mixing with MXene powder;
step 2, drying the mixed composite material to constant weight at room temperature to obtain Fe2O3@ MXene composite powder.
The preparation method of MXene powder comprises the following steps:
s1, weighing 3g of titanium-aluminum-carbon by using an electronic balance, slowly adding the titanium-aluminum-carbon into 60ml of hydrofluoric acid with the concentration of 40%, placing the mixture on a magnetic stirrer, and stirring the mixture for 24 hours at the constant temperature of 35 ℃;
s2, ultrasonically cleaning the stirred mixed solution at 35 ℃ for 60 min;
and S3, centrifuging the mixed solution subjected to ultrasonic cleaning four times by using deionized water until the pH is neutral, and drying at room temperature to obtain MXene powder.
Fe2O3A method of preparing a powder comprising the steps of:
s1, respectively weighing 60g of deionized water and 32g of absolute ethyl alcohol by using an electronic balance, and mixing the two to serve as a solvent;
s2, respectively weighing 21.014g of citric acid and 40.4g of ferric nitrate, adding the citric acid and the ferric nitrate into the solvent, placing the mixture on a magnetic stirrer, stirring and dissolving to prepare a precursor, and stirring at a constant temperature of 85 ℃ until wet gel is formed;
s3, drying and foaming at 130 ℃ to obtain dry gel, and calcining the dry gel at 600 ℃ to obtain the ferric oxide powder.
The invention also provides Fe2O3The preparation method of the @ MXene composite powder comprises the following steps:
step 1, preparing MXene dispersion liquid;
step 2, mixing the MXene dispersion liquid prepared in the step 1 with Fe (NO)3)3·9H2Fully mixing O in a molar ratio of 1 (1-3), then placing the mixture in a hydrothermal kettle, and reacting for 30 hours at the temperature of 180 ℃; after the reaction is finished, naturally cooling to obtain Fe2O3@ MXene composite powder;
step 3, the Fe obtained in the step 22O3Washing, centrifuging and drying the @ MXene composite powder to constant weight in sequence to obtain pure Fe2O3@ MXene composite powder.
Wherein, in the step 1, MXene powder is prepared;
(a) weighing 3g of titanium-aluminum-carbon by using an electronic balance, slowly adding the titanium-aluminum-carbon into 60ml of 40% hydrofluoric acid, placing the mixture on a magnetic stirrer, and stirring the mixture for 24 hours at a constant temperature of 35 ℃;
(b) ultrasonically cleaning the stirred mixed solution at 35 ℃ for 60 min;
(c) then centrifuging the mixed solution subjected to ultrasonic cleaning with deionized water for four times until the pH is close to neutral, and drying at room temperature to obtain MXene powder.
In the step 1, 1mmol of MXene powder is added into 60ml of DMF, and ultrasonic washing is carried out for 2h to obtain MXene dispersion liquid.
Example 1
Direct mixing method
1. Preparation of MXene powder
(a) Weighing 3g of titanium-aluminum-carbon by using an electronic balance, slowly adding the titanium-aluminum-carbon into 60ml of 40% hydrofluoric acid, placing the mixture on a magnetic stirrer, and stirring the mixture for 24 hours at a constant temperature of 35 ℃;
(b) ultrasonically cleaning the stirred mixed solution at 35 ℃ for 60 min;
(c) centrifuging the ultrasonically cleaned mixed solution for four times by using deionized water until the pH is close to neutral, and drying at room temperature to obtain MXene powder;
2. preparation of Fe2O3 powder
(a) Respectively weighing 60g of deionized water and 32g of absolute ethyl alcohol by using an electronic balance, and mixing the deionized water and the absolute ethyl alcohol to obtain a solvent;
(b) then, respectively weighing 21.014g of citric acid and 40.4g of ferric nitrate, adding the citric acid and the ferric nitrate into the solvent, placing the mixture on a magnetic stirrer, stirring and dissolving the mixture to prepare a precursor, and stirring the precursor at a constant temperature of 85 ℃ until wet gel is formed;
(c) drying and foaming at 130 ℃ to obtain dry gel, and calcining the dry gel at 600 ℃ to obtain ferric oxide powder;
3. 1.60g (1mmol), 3.20g (2mmol), 4.80g (3mmol) of Fe2O3 powder and 1.68g of MXene powder were stirred at room temperature for 0.5h to thoroughly mix the Fe2O3 powder and the MXene powder. The product was dried in a forced air oven at 35 ℃ for 24h to constant weight. The required Fe2O3@ MXene composite material is obtained.
And analyzing and detecting the dried powder by using an SEM (scanning Electron microscope), XRD (X-ray diffraction) and vector network analyzer.
Example 2
One-step solvothermal process
1. Preparing MXene powder;
(a) weighing 3g of titanium-aluminum-carbon by using an electronic balance, slowly adding the titanium-aluminum-carbon into 60ml of 40% hydrofluoric acid, placing the mixture on a magnetic stirrer, and stirring the mixture for 24 hours at a constant temperature of 35 ℃;
(b) ultrasonically cleaning the stirred mixed solution at 35 ℃ for 60 min;
(c) centrifuging the ultrasonically cleaned mixed solution for four times by using deionized water until the pH value is neutral, and drying at room temperature to obtain MXene powder;
2. 0.168g (1mmol) of MXene powder is weighed by an electronic balance and added into 60ml of DMF (N, N-dimethylformamide, analytical purity), and the MXene powder is ultrasonically washed for 2h to obtain MXene dispersion liquid, and 3 dispersion liquids with the same components are prepared;
3. respectively weighing 0.404g (1mmol), 0.808g (2mmol) and 1.212g (3mmol) of Fe (NO3) 3.9H 2O by an electronic balance, respectively adding into the dispersion liquid, placing on a magnetic stirrer, stirring for 1H to fully mix Fe (NO3) 3.9H 2O and MXene dispersion liquid, then transferring into a hydrothermal kettle, and reacting for 30H at the temperature of 180 ℃;
4. after the reaction is finished, the reaction kettle is naturally cooled to obtain Fe2O3@ MXene composite powder, then the composite powder is washed by deionized water and absolute ethyl alcohol and centrifuged for three times at 8000rpm, and then the composite powder is dried in a vacuum drying oven at 60 ℃ for 24h to constant weight to obtain pure Fe2O3@ MXene composite powder, and the composite powder and the Fe2O3@ MXene composite powder prepared by a direct mixing method are tested by SEM, XRD and a vector network analyzer to determine the optimal proportion.
FIGS. 1a, 1b and 1c in FIG. 1 are Fe prepared according to the specific embodiment2O3SEM image of @ MXene. It is understood from the figure that Fe2O3Prepared by a one-step solvothermal method with MXene powder in different molar ratios (1:1, 2:1, 3: 1). Fe at MXene material layer boundary with increasing doping concentration2O3The number of nano particles is increased, the stability of the composite material is promoted, and Fe is inhibited2O3And (4) agglomeration of the nano particles. The material has better interlayer spacing uniformity.
In FIG. 2, Fe prepared according to the practical examples2O3The XRD patterns of the @ MXene composite powder and the MXene phase. From the analysis of the graph, Fe appeared2O3Phase sum of more TiO2The diffraction peak of mixed phase, MXene phase, is reduced, mainly Fe2O3Predominantly phase, probably Fe2O3The introduction of (A) has an inhibiting effect on the formation of MXene phase. In conclusion, with Fe2O3The more Fe appears in the diffraction pattern2O3Phase, MXene phase, was relatively reduced, forming a new phase. .
As shown in FIG. 3, it is Fe2O3Mixing with MXene powder at different molar ratios to prepare the obtained Fe2O3@ MXene composite material with different Fe2O3Doping concentration, and a curve (a) epsilon 'of the dielectric parameters (epsilon', epsilon ', mu' and tan delta) of the composite powder changing along with frequency; (b) ε "; (c) mu'; (d) μ "; (e) tan delta.
From the graph analysis, as the doping concentration increases, the real part epsilon 'and the imaginary part epsilon' of the dielectric constant of the composite powder have obvious reduction tendency, the real part mu 'and the imaginary part mu' of the magnetic permeability greatly increase with the increase of the doping concentration, and the loss tangent value tan delta greatly increases with the increase of the doping concentration.
As shown in FIG. 4, is Fe prepared according to example 22O3@ MXene composite material with different Fe2O3The wave-absorbing curve of the composite powder with doping concentration and different sample thicknesses.
As can be seen from the analysis of the graph, the maximum absorption peak shifts to a low frequency with the increase of the thickness at a doping molar ratio of 1:1, the maximum absorption peak is near 9.0GHz and is approximately-19.1 dB with the thickness of the powder sample being 3.0mm, the maximum absorption peak shifts to a low frequency with the increase of the thickness at a doping molar ratio of 2:1, the maximum absorption peak is near 8.8GHz and is approximately-17.1 dB with the thickness of the powder sample being 3.0mm, the maximum absorption peak shifts to a low frequency with the increase of the thickness with the doping molar ratio of 3:1, and the maximum absorption peak is 8.6GHz and is approximately-14.6 dB with the thickness of the powder sample being 3.0 mm. Under the condition of the same thickness, the peak value absolute value of the maximum absorption peak is reduced along with the increase of the doping concentration; and the maximum absorption peak is shifted to low frequencies. Under the same doping ratio, the maximum absorption peak moves to low frequency along with the increase of the thickness; and when the thickness of a sample of the composite material is 3.0mm, the wave-absorbing performance is the best.
FIG. 5 shows different Fe with the same thickness (3.0mm) in the frequency range of (8.2-12.4) GHz2O3And (3) a wave absorbing curve of the doping concentration powder sample. From the analysis of the figure, it can be obtained when the same thickness of Fe is different2O3Amount of doping, depending on Fe2O3The doping amount concentration is increased, the maximum reflectivity absorption peak of the composite powder moves to the low-frequency direction, and the wave-absorbing performance is reduced. In conclusion, when the doping concentration is 1:1, the composite powder has better wave-absorbing performance.
In fig. 6, (a) is a composite powder prepared by a one-step solvothermal method, and (b) is a composite powder prepared by a direct mixing method. Compared with the compound material (a), the arrangement of the laminated structure of the compound material (b) is disordered, the number of nano particles at the boundary is large, and the surface particles of the MXene material are not uniformly distributed, which indicates that the composite material prepared by the direct mixing method can not mix MXene and Fe2O3The mixed powder is uniformly mixed, and the composite powder prepared by adopting the one-step solvothermal method can effectively reduce the accumulation of MXene lamella, effectively separate the MXene lamella and avoid Fe2O3The agglomeration among the nano particles realizes the Fe2O3High-efficiency compounding with MXene.
Claims (9)
1. Fe2O3The preparation method of the @ MXene composite powder is characterized by comprising the following steps of:
step 1, adding Fe2O3Mixing MXene powder with (1-3): 1, and stirring at constant temperature at room temperature until the components are fully mixed;
step 2, drying the mixed composite material to constant weight at room temperature to obtain Fe2O3@ MXene composite powder.
2. Fe according to claim 12O3A process for preparing the composite powder of @ MXene, wherein in step 1, Fe2O3Mixing with MXene powder at a ratio of 1:1 in a molar ratio ofAnd (4) line mixing.
3. Fe according to claim 12O3The preparation method of the @ MXene composite powder is characterized in that in the step 1, the preparation method of the MXene powder comprises the following steps:
s1, weighing 3g of titanium-aluminum-carbon, slowly adding the titanium-aluminum-carbon into 60ml of hydrofluoric acid with the concentration of 40%, and uniformly stirring;
s2, ultrasonically cleaning the stirred mixed solution;
and S3, centrifuging the mixed solution subjected to ultrasonic cleaning by using deionized water until the pH is neutral, and drying at room temperature to obtain MXene powder.
4. Fe according to claim 12O3A process for preparing the composite powder of @ MXene, wherein in step 1, Fe2O3A method of preparing a powder comprising the steps of:
s1, respectively weighing 60g of deionized water and 32g of absolute ethyl alcohol, and mixing the two to serve as a solvent;
s2, respectively weighing 21.014g of citric acid and 40.4g of ferric nitrate, adding the citric acid and the ferric nitrate into the solvent of S1, placing the mixture on a magnetic stirrer, stirring and dissolving the mixture to prepare a precursor, and stirring the precursor at a constant temperature to obtain wet gel;
s3, drying and foaming the wet gel in the S2 to obtain dry gel, and calcining the dry gel to obtain the ferric oxide powder.
5. Fe2O3An @ MXene composite powder characterized by being produced based on the production method according to claim 1.
6. Fe2O3The preparation method of the @ MXene composite powder is characterized by comprising the following steps of:
step 1, preparing MXene dispersion liquid;
step 2, mixing the MXene dispersion liquid prepared in the step 1 with Fe (NO)3)3·9H2O is 1 (1E)3) The mixture is fully mixed and then placed in a hydrothermal kettle for reaction; after the reaction is finished, naturally cooling;
and 3, sequentially washing, centrifuging and drying the product obtained in the step 2 to constant weight to obtain Fe2O3@ MXene composite powder.
7. Fe according to claim 62O3The preparation method of the @ MXene composite powder is characterized in that the preparation method of the MXene powder in the step 1 comprises the following steps:
s1, weighing 3g of titanium-aluminum-carbon, slowly adding the titanium-aluminum-carbon into 60ml of hydrofluoric acid with the concentration of 40%, and uniformly stirring;
s2, ultrasonically cleaning the stirred mixed solution;
and S3, centrifuging the mixed solution subjected to ultrasonic cleaning by using deionized water until the pH is neutral, and drying at room temperature to obtain MXene powder.
8. Fe according to claim 62O3The preparation method of the @ MXene composite powder is characterized in that the preparation method of the MXene dispersion liquid in the step 1 comprises the following steps: adding MXene powder into DMF, and carrying out ultrasonic washing to obtain MXene dispersion liquid.
9. Fe2O3An @ MXene composite powder characterized by being produced based on the production method according to claim 6.
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