CN110524004B - Preparation method of size-adjustable monodisperse nano-porous Fe @ C core-shell structure - Google Patents
Preparation method of size-adjustable monodisperse nano-porous Fe @ C core-shell structure Download PDFInfo
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Abstract
The invention discloses a preparation method of a monodisperse nano-porous Fe @ C core-shell structure with adjustable size, which comprises the steps of adding polyvinylpyrrolidone (PVP) powder into a mixed solution of water and ethanol, and uniformly stirring to obtain a clarified liquid; adding ferrous salt solution into the clarified solution, introducing argon and stirring in an ice-water bath for 30min to obtain light green solution; dropwise addition of sodium borohydride (NaBH)4) And (3) solution, centrifugally washing and drying the obtained black product, and carrying out heat treatment at different temperatures and heat preservation time to obtain Fe @ C core-shell structure powder. The method is simple in process and low in cost, and the monodisperse nano porous Fe @ C core-shell structure powder with adjustable size shows excellent electromagnetic wave absorption performance by regulating and controlling components and reaction time in a mixed solution of water and ethanol as well as heat treatment temperature and time, is suitable for large-scale industrial production, and has good application prospect.
Description
Technical Field
The invention belongs to the field of materials, relates to a preparation method of a nano material, and particularly relates to a preparation method of size-adjustable monodisperse nano porous Fe @ C core-shell structure powder.
Background
The ferromagnetic metal micro-nano material has the advantages of high saturation magnetization, high Snoek's cut-off frequency, high Curie temperature, strong absorption of electromagnetic waves in a wide frequency range and the like, and is an ideal material for preparing an ultrathin electromagnetic wave absorption coating with excellent performance. However, the ferromagnetic metal micro-nano particles are easily oxidized in the air and easily corroded in an acidic environment, and due to high surface activity, the ferromagnetic metal micro-nano particles are easily agglomerated, and for the current situation, improvement of the electromagnetic wave absorption performance of the ferromagnetic nano metal through various ways has become a research hotspot at present. The methods reported in the literature mainly include surface insulation treatment, doping of dielectric elements, coating of dielectric layers, and the like. The preparation method of the ferromagnetic nano metal mainly focuses on a hydrothermal method or a thermal oxidation method, and the method needs to be carried out in a high-temperature or high-pressure environment, so that the process is relatively complex, and the large-scale preparation of the material is greatly restricted.
Therefore, a synthesis mode with low cost and good controllability is developed, ferromagnetic nano metal particles can be coated by the dielectric layer, and the method has important significance for improving the electromagnetic wave absorption performance of ferromagnetic nano metal and expanding the application of the ferromagnetic nano metal. Literature search shows that: at home and abroad, no literature reports about the use of water-ethanol as a solvent, PVP as a surfactant and a carbon source, and sodium borohydride (NaBH)4) The research result of preparing Fe @ C nano particles by using the reducing agent through normal-temperature liquid-phase reduction.
Disclosure of Invention
The invention aims to provide a preparation method of size-adjustable powder with a nano-porous Fe @ C core-shell structure, which has simple process steps and can obtain a size-adjustable material with a nano-porous Fe @ C core-shell structure.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of size-adjustable monodisperse nano porous Fe @ C core-shell structure powder comprises the following steps:
1) adding PVP powder with a certain mass into mixed solutions of water and ethanol with different proportions, and uniformly stirring to obtain a clear solution;
2) adding a ferrous salt solution with a certain molar concentration into the clarified solution, and stirring and dissolving for 15min in an ice-water bath to obtain a light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) adding sodium borohydride (NaBH) with a certain molar concentration4) Dropwise adding the solution into the solution to obtain black precipitate, separating, repeatedly washing, centrifuging, and freeze-drying to obtain a primary product Fe @ PVP powder;
4) placing Fe @ PVP powder in a tube furnace, H2And (3) carrying out high-temperature heat treatment in the atmosphere, and adjusting the temperature and time of the heat treatment to obtain the final product size-adjustable powder with the nano porous Fe @ C core-shell structure.
The step 1) is uniformly stirred at 15-35 ℃ for 10-30 min.
The average molecular weight of the PVP is 3000-400000.
The volume ratio of the absolute ethyl alcohol in the mixed solution of water and ethyl alcohol is 0-75%.
The ferrous salt solution in the step 2) can be ferrous chloride, ferrous nitrate or ferrous sulfate.
The washing in the step 3) is centrifugal washing, and the washing solvent is water and absolute ethyl alcohol.
The centrifugal washing frequency is 5-8 times, each time lasts for 3-5 min, and the centrifugal rotating speed is 7000-9000 rpm/min.
The temperature of freeze drying in the step 3) is-40 ℃, the pressure is 120Pa, and the time is 10-25 h.
The primary product Fe @ PVP obtained in the step 3) is of a core-shell structure.
The heat treatment in the step 4) comprises the steps of ventilating for 30min at room temperature, heating to 500 ℃, and keeping the temperature for 0-2h, wherein the heating rate is 5-20 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the size-adjustable monodisperse powder with the nano-porous Fe @ C core-shell structure, provided by the invention, comprises the steps of adding PVP powder into mixed solutions of water and ethanol in different proportions, and uniformly stirring to obtain a clear solution; adding a ferrous chloride solution into the clarified solution, and stirring in an ice-water bath to obtain a light green solution; dropwise adding NaBH4 solution, centrifugally washing and drying the obtained black product, and further carrying out high-temperature heat treatment to obtain the size-adjustable powder with the nano-porous Fe @ C core-shell structure. The method is simple in process and low in cost, the monodisperse powder with the nano porous Fe @ C core-shell structure with adjustable size can be obtained by adjusting the components, the stirring temperature and the heat treatment time of the mixed solution of water and ethanol, the method is suitable for large-scale industrial production, and the obtained Fe @ C core-shell structure powder has excellent electromagnetic wave absorption performance and good application prospect.
Drawings
FIG. 1 is an SEM image and particle size statistics of nano Fe @ C powder prepared in example 1 of the present invention;
FIG. 2 is an SEM image and particle size statistics of the nano Fe @ C powder prepared in example 2 of the present invention;
FIG. 3 is an SEM image and particle size statistics of the nano Fe @ C powder prepared in example 3 of the present invention;
FIG. 4 is an SEM image and particle size statistics of the nano Fe @ C powder prepared in example 4 of the present invention;
FIG. 5 is an SEM image of nano Fe @ C powder prepared in example 5 of the present invention;
FIG. 6 is a TEM image of nano Fe @ C powder prepared in example 5 of the present invention;
FIG. 7 is a TEM image of nano Fe @ C powder prepared in example 6 of the present invention;
FIG. 8 is a graph showing the electromagnetic wave absorption properties of the nano Fe @ C powder prepared in example 5 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
1) 1g of PVP powder was added to 30mL of a mixed solution of water and ethanol (V)Water (W)/VEthanol30mL/0mL), and stirring uniformly to obtain a clear liquid;
2) adding 95mg ferrous chloride powder into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding 45ml of NaBH4 solution with the concentration of 100mM into the solution to obtain black precipitate, separating the black precipitate, repeatedly washing, centrifuging, and freeze-drying to obtain monodisperse Fe sphere powder;
the morphology of the powder obtained in example 1 is shown in FIG. 1, and it can be seen that the powder is monodisperse spheres with an average particle size of about 724 nm.
Example 2
1) 1g of PVP powder was added to 30mL of a mixed solution of water and ethanol (V)Water (W)/VEthanol22.5mL/7.5mL), and stirring uniformly to obtain a clear liquid;
2) adding 95mg ferrous chloride powder into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding 45ml of NaBH4 solution with the concentration of 100mM into the solution to obtain black precipitate, separating, repeatedly washing, centrifuging, and freeze-drying to obtain monodisperse Fe powder;
the morphology of the monodisperse Fe powder obtained in example 2 is shown in fig. 2, and it can be seen that the powder has a monodisperse spherical morphology with an average particle size of about 656 nm.
Example 3
1) 1g of PVP powder was added to 30mL of a mixed solution of water and ethanol (V)Water (W)/VEthanol15mL/15mL), and stirring uniformly to obtain a clear liquid;
2) adding 95mg ferrous chloride powder into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding 45ml of NaBH4 solution with the concentration of 100mM into the solution to obtain black precipitate, separating, repeatedly washing, centrifuging, and freeze-drying to obtain monodisperse Fe powder;
the morphology of the powder obtained in example 3 is shown in FIG. 3, and it can be seen that the powder has a monodisperse spherical morphology and an average particle diameter of about 466 nm.
Example 4
1) 1g of PVP powder was added to 30mL of a mixed solution of water and ethanol (V)Water (W)/VEthanol7.5mL/22.5mL), and stirring uniformly to obtain a clear liquid;
2) adding 95mg ferrous chloride powder into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding 45ml of NaBH4 solution with the concentration of 100mM into the solution to obtain black precipitate, separating, repeatedly washing, centrifuging, and freeze-drying to obtain monodisperse Fe powder;
the morphology of the powder obtained in example 4 is shown in FIG. 4, and it can be seen that the powder has a monodisperse spherical morphology with an average particle size of about 311 nm.
Example 5
1) 1g of PVP powder was added to 30mL of a mixed solution of water and ethanol (V)Water (W)/VEthanol5mL/20mL), and stirring uniformly to obtain a clear liquid;
2) adding 95mg ferrous chloride powder into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding 45ml of NaBH4 solution with the concentration of 100mM into the solution to obtain black precipitate, separating the black precipitate, repeatedly washing, centrifuging, and freeze-drying to obtain a primary product Fe @ PVP powder;
4) placing Fe @ PVP powder in a tube furnace, H2And (3) carrying out high-temperature heat treatment under the atmosphere, ventilating for 30min at room temperature, heating to 500 ℃, and keeping the temperature for 2h, wherein the heating rate is 5 ℃/min, so that the final product size-adjustable powder with the nano-porous Fe @ C core-shell structure is obtained.
The morphology of the nanoporous Fe @ C core-shell structure powder obtained in example 5 is shown in FIGS. 5 and 6, and it can be seen that the powder is in a nanosphere shape, a porous structure appears in the core part, and the average particle size is about 170 nm.
Example 6
1) 1g of PVP powder was added to 30mL of a mixed solution of water and ethanol (V)Water (W)/VEthanol5mL/20mL), and stirring uniformly to obtain a clear liquid;
2) adding 95mg ferrous chloride powder into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, exhausting for 15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding 45ml of NaBH4 solution with the concentration of 100mM into the solution to obtain black precipitate, separating the black precipitate, repeatedly washing, centrifuging, and freeze-drying to obtain a primary product Fe @ PVP powder;
4) placing Fe @ PVP powder in a tube furnace, H2And (3) carrying out high-temperature heat treatment under the atmosphere, ventilating for 30min at room temperature, heating to 500 ℃, and keeping the temperature for 2h, wherein the heating rate is 20 ℃/min, so that the final product size-adjustable powder with the nano-porous Fe @ C core-shell structure is obtained.
The shape of the nanoporous Fe @ C core-shell structure powder obtained in example 6 is shown in FIG. 7, and it can be seen that the shape of the powder is nanosphere, a gap is formed in the middle of the core shell, and the particle size is about 170 nm.
Claims (7)
1. A preparation method of a monodisperse nano-porous Fe @ C core-shell structure with adjustable size is characterized by comprising the following steps:
1) adding 0.5-3g of PVP powder into mixed solutions of water and ethanol in different proportions, and uniformly stirring to obtain a clear solution; vWater (W)/VEthanol＝30mL/0mL；VWater (W)/VEthanol＝22.5mL/7.5mL；VWater (W)/VEthanol＝15mL/15mL；
2) Adding ferrous salt solution with molar concentration of 10-200mM into the clarified solution, stirring and dissolving in ice water bath for 15min to obtain light green solution; introducing Ar gas into the solution, and exhausting for 10-15min to prevent Fe2+Oxidized to ensure that the whole reaction system is in Ar atmosphere;
3) dropwise adding NaBH4 solution with the molar concentration of 50-300mM into the solution to obtain black precipitate, separating, repeatedly washing, centrifuging, and freeze-drying to obtain a primary product Fe @ PVP powder;
4) placing Fe @ PVP powder in a tube furnace, H2And (3) carrying out high-temperature heat treatment in a gas atmosphere, adjusting the temperature and time of the heat treatment, ventilating for 30-60min at room temperature, heating to 500 ℃, and keeping the temperature for 0-2h, wherein the heating rate is 5-30 ℃/min, so that the final product of the nano porous Fe @ C core-shell structure powder with adjustable size is obtained.
2. The preparation method of the monodisperse nanoporous Fe @ C core-shell structure with the adjustable size according to claim 1, wherein the preparation method comprises the following steps: the average molecular weight of PVP used in the step 1) is 3000-400000.
3. The preparation method of the monodisperse nanoporous Fe @ C core-shell structure with the adjustable size according to claim 1, wherein the preparation method comprises the following steps: the stirring is carried out for 5-10 min at 15-35 ℃.
4. The preparation method of the monodisperse nanoporous Fe @ C core-shell structure with the adjustable size according to claim 1, wherein the preparation method comprises the following steps: the ferrous salt solution in the step 2) can be ferrous chloride, ferrous nitrate and ferrous sulfate.
5. The preparation method of the monodisperse nanoporous Fe @ C core-shell structure with the adjustable size according to claim 1, wherein the preparation method comprises the following steps: the washing in the step 3) is centrifugal washing, and the washing solvent is water and absolute ethyl alcohol.
6. The preparation method of the monodisperse nanoporous Fe @ C core-shell structure with the adjustable size according to claim 5, wherein the preparation method comprises the following steps: the centrifugal washing frequency is 2-5 times, each time lasts for 1-5 min, and the centrifugal rotating speed is 7000-9000 rpm/min.
7. The preparation method of the monodisperse nanoporous Fe @ C core-shell structure with the adjustable size according to claim 1, wherein the preparation method comprises the following steps: the temperature of freeze drying in the step 3) is-40 to-56 ℃, the pressure is 50-120Pa, and the time is 10-25 h.
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