CN108529578B - Preparation method of high-stability nano black phosphorus/three-dimensional graphene composite material - Google Patents
Preparation method of high-stability nano black phosphorus/three-dimensional graphene composite material Download PDFInfo
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Abstract
The invention relates to a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material, and belongs to the technical field of composite materials. Mixing a nano black phosphorus dispersion liquid and a graphene oxide dispersion liquid at the temperature of 5-30 ℃ under the inert gas atmosphere, and performing ultrasonic treatment to obtain a dispersion liquid A; and under the inert gas atmosphere, treating the dispersion liquid A by using liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material. Under the catalytic action of nano black phosphorus, graphene oxide can be reduced into graphene under the ultrasonic condition, and the black phosphorus and the graphene form a strong bonding effect in the reduction process.
Description
Technical Field
The invention relates to a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material, and belongs to the technical field of composite materials.
Background
Black phosphorus is a two-dimensional layered material that has emerged recently, similar to graphite. Due to the unique crystal structure and energy band structure of the black phosphorus, the black phosphorus has good application prospects in the fields of energy storage, catalysis and the like. Compared with the nano black phosphorus, the block black phosphorus has the defects of slow ionic and electronic conduction, small reaction active area and the like, so that the block black phosphorus needs to be subjected to nanocrystallization in actual application, namely the nano black phosphorus (black phosphorus alkene or black phosphorus quantum dots) is prepared. Although the nano black phosphorus has the specific advantages of the nano material, the practical application has fundamental obstacles: the phosphorus-based material has poor conductivity and is easily oxidized when meeting the surrounding environment. Therefore, it is necessary to compound nano black phosphorus with a highly conductive graphene material. On one hand, the problem of poor conductivity of single nano black phosphorus is improved, and on the other hand, the stability of the nano black phosphorus is improved. The preparation method of the existing nano black phosphorus/graphene composite material mainly comprises the following steps: first, the black phosphorus is physically mixed with the graphene. The black phosphorus and the graphene in the composite material obtained by the method only interact through Van der Waals force, and the defect that the nano black phosphorus is easy to oxidize cannot be fundamentally overcome; secondly, mixing the black phosphorus alkene with the graphene oxide, and then realizing the reduction of the graphene oxide through a plasma sintering process to obtain the black phosphorus alkene/graphene composite material. Although the composite material obtained by the method has a strong bonding effect between the black phosphorus alkene and the graphene oxide, the plasma sintering process is complex, the energy consumption is high, and the industrial production is not facilitated. And the reported nano black phosphorus/graphene composite materials are all two-dimensional structures. Compared with the composite material with a three-dimensional structure, the electrolyte and ion conductivity of the two-dimensional composite material is poor, and the active area is smaller.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material, under the catalytic action of nano black phosphorus, graphene oxide can be reduced into graphene under the ultrasonic condition, and the black phosphorus and the graphene form strong bonding action in the reduction process; the method has the advantages of simple operation, high efficiency and mild reaction conditions.
A preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing the nano black phosphorus dispersion liquid with the graphene oxide dispersion liquid at the temperature of 5-30 ℃ under the inert gas atmosphere, and performing ultrasonic treatment to obtain a dispersion liquid A;
(2) under the inert gas atmosphere, treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain a nano black phosphorus/three-dimensional graphene nano composite material;
the mass ratio of the nano black phosphorus to the graphene oxide in the step (1) is 1 (1-4);
the nano black phosphorus in the step (1) is black phospholene, black phosphorus quantum dots or black phosphorus nanowires; the dispersion solvent of the nano black phosphorus dispersion liquid is water, ethanol, dimethyl sulfoxide, N-methyl pyrrolidone, isopropanol, N-dimethylformamide, ethylene carbonate or 1-butyl-trimethyl imidazole dicyandiamide; the dispersion solvent of the graphene oxide dispersion liquid is water, ethanol, dimethyl sulfoxide, N-methyl pyrrolidone, isopropanol, N-dimethylformamide, ethylene carbonate or 1-butyl-trimethyl imidazole dicyandiamide;
the ultrasonic pretreatment in the step (1) is carried out by adopting an ultrasonic cell cleaner and/or a cell crusher, the power of the ultrasonic cell cleaner is 150-300W, the power of the cell crusher is 500-1500W, and the ultrasonic treatment time is 0.5-3 h;
the inert gas is one or two of argon, nitrogen and helium;
the nano black phosphorus dispersion liquid is obtained by adding nano black phosphorus into a dispersion solvent and carrying out ultrasonic pretreatment by an ultrasonic cell cleaner and/or a cell crusher;
the graphene oxide aqueous dispersion is as followsThe document "Large reversible capacity of high quality graphics sheets as an anode material for lithium-ion batteries" or the document "Porous SnO2Prepared from @ C/graphene nanocomposite with 3D carbon conductive network as a super anode material for lithium-ion batteries';
the invention has the beneficial effects that:
(1) according to the invention, nano black phosphorus and graphene oxide are directly mixed, and under the action of the nano black phosphorus, the reduction of the graphene oxide and the formation of a nano black phosphorus/graphene composite material can be realized only by one-step ultrasound;
(2) the method has the characteristics of high speed, high efficiency, energy conservation, environmental protection, low requirement on equipment and low cost;
(3) the method combines ultrasonic and liquid nitrogen freezing to process nano black phosphorus and graphene oxide to form a nano black phosphorus/three-dimensional graphene composite material with a three-dimensional porous structure; the nano black phosphorus/three-dimensional graphene composite material has a larger active area, higher conductivity and ion transmission performance; the nano black phosphorus and the graphene in the nano black phosphorus/three-dimensional graphene composite material form a strong P-O-C bond, so that the problem of poor stability of the nano black phosphorus is solved.
Drawings
FIG. 1 is a scanning electron microscope image of the nano black phosphorus/three-dimensional graphene composite material of example 1;
FIG. 2 is an element distribution diagram of the nano black phosphorus/three-dimensional graphene composite material of example 1;
FIG. 3 is C of graphene oxide of example 11SA spectrogram;
FIG. 4 shows C of the nano black phosphorus/three-dimensional graphene composite material of example 11SA spectrogram;
FIG. 5 is P of the nano black phosphorus/three-dimensional graphene composite of example 12PA spectrogram;
fig. 6 is a linear voltammogram and a tafel slope diagram of the nano black phosphorus/three-dimensional graphene composite material of example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1: a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing a nano black phosphorus dispersion liquid (the nano black phosphorus dispersion liquid is nano black phosphorus alkene/water dispersion liquid) and a graphene oxide dispersion liquid (the graphene oxide dispersion liquid is graphene oxide/water dispersion liquid) at the temperature of 15 ℃ under the atmosphere of inert gas (argon), and performing ultrasonic treatment to obtain a dispersion liquid A; wherein the concentration of the nano black phosphorus dispersion liquid (nano black phosphorus alkene/water dispersion liquid) is 1mg/mL, the concentration of the graphene oxide dispersion liquid (graphene oxide/water dispersion liquid) is 4mg/mL, and the mass ratio of the nano black phosphorus to the graphene oxide is 1: 4; the ultrasonic treatment is ultrasonic pretreatment by adopting an ultrasonic cell cleaner, the power of the ultrasonic cell cleaner is 200W, and the treatment time of the ultrasonic cell cleaner is 1 h;
(2) under the inert gas (argon) atmosphere, treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain a nano black phosphorus/three-dimensional graphene nano composite material;
a scanning electron microscope image of the nano black phosphorus/three-dimensional graphene nanocomposite material obtained in the embodiment is shown in fig. 1, and as can be seen from fig. 1, the black phosphorus/three-dimensional graphene nanocomposite material has a three-dimensional porous structure;
the element distribution diagram of the nano black phosphorus/three-dimensional graphene nanocomposite obtained in the embodiment is shown in fig. 2, and it can be known from fig. 2 that phosphorus and carbon are uniformly distributed;
c of graphene oxide of the present example1SThe spectrum of the nano black phosphorus/three-dimensional graphene nanocomposite material C obtained in the example is shown in FIG. 31SThe spectrogram is shown in fig. 4, and as can be seen from fig. 3 to 4, graphene oxide is reduced into graphene under the action of ultrasonic waves and nano black phosphorus;
p of the nano black phosphorus/three-dimensional graphene nanocomposite obtained in the embodiment2PThe spectrogram is shown in fig. 5, and as can be seen from fig. 5, the graphene and the black phosphorus alkene form a P-O-C bond through ultrasound, which has a strong bonding effect, and indicates that the nano black phosphorus/three-dimensional graphene nanocomposite materialWill have good stability;
fig. 6 shows that the linear voltammetry scan and the tafel slope plot of the nano black phosphorus/three-dimensional graphene nanocomposite obtained in this example are shown in fig. 6, and as can be seen from fig. 6, the initial potential of the nanocomposite is 0.56V, and the tafel slope is 105mv/dec, which indicates that the nano black phosphorus/three-dimensional graphene nanocomposite prepared in this example has good electrocatalytic oxygen evolution performance.
Example 2: a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing a nano black phosphorus dispersion liquid (the nano black phosphorus dispersion liquid is a black phosphorus quantum dot/N-methylpyrrolidone dispersion liquid) and a graphene oxide dispersion liquid (the graphene oxide dispersion liquid is a graphene oxide/N-methylpyrrolidone dispersion liquid) at the temperature of 25 ℃ under the atmosphere of inert gas (nitrogen), and performing ultrasonic treatment to obtain a dispersion liquid A; wherein the concentration of the nano black phosphorus dispersion liquid (black phosphorus quantum dot/N-methylpyrrolidone dispersion liquid) is 1mg/mL, the concentration of the graphene oxide dispersion liquid (graphene oxide/N-methylpyrrolidone dispersion liquid) is 4mg/mL, and the mass ratio of the nano black phosphorus to the graphene oxide is 1: 1; the ultrasonic treatment is ultrasonic pretreatment by adopting a cell crusher, the cell crusher is 1500W, and the ultrasonic treatment time is 0.5 h;
(2) under the inert gas (nitrogen) atmosphere, treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material;
scanning electron microscopy, XPS characterization and electrocatalytic oxygen evolution performance test are carried out on the nano black phosphorus/three-dimensional graphene nano composite material prepared in the embodiment, detection and analysis show that the composite material has a three-dimensional network structure, the nano phosphorus and the graphene in the composite material form a P-O-C bond, and the composite material has good electrocatalytic performance through linear volt-ampere scanning test.
Example 3: a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing a nano black phosphorus dispersion liquid (the nano black phosphorus dispersion liquid is a black phosphorus quantum dot/1-butyl-trimethyl imidazole dicyandiamide dispersion liquid) and a graphene oxide dispersion liquid (the graphene oxide dispersion liquid is a graphene oxide 1-butyl-trimethyl imidazole dicyandiamide dispersion liquid) at the temperature of 25 ℃ under the atmosphere of inert gas (nitrogen), and performing ultrasonic treatment to obtain a dispersion liquid A; wherein the concentration of the nano black phosphorus dispersion liquid (black phosphorus quantum dot/1-butyl-trimethyl imidazole dicyandiamide dispersion liquid) is 1mg/mL, the concentration of the graphene oxide dispersion liquid (graphene oxide/1-butyl-trimethyl imidazole dicyandiamide dispersion liquid) is 4mg/mL, and the mass ratio of the nano black phosphorus to the graphene oxide is 1: 3; the ultrasonic treatment is ultrasonic pretreatment by adopting an ultrasonic cleaner, the power of the ultrasonic cleaner is 300W, and the treatment time of the ultrasonic cleaner is 2 h;
(2) under the inert gas (nitrogen) atmosphere, treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material;
scanning electron microscopy, XPS characterization and electrocatalytic oxygen evolution performance test are carried out on the nano black phosphorus/three-dimensional graphene nano composite material prepared in the embodiment, and detection and analysis show that the composite material has a three-dimensional network structure, and the nano phosphorus and the graphene in the composite material form a P-O-C bond; the linear voltammetry scanning test shows that the composite material has good electrocatalytic performance.
Example 4: a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing a nano black phosphorus dispersion liquid (the nano black phosphorus dispersion liquid is a black phosphorus quantum dot/N, N-dimethylformamide dispersion liquid) and a graphene oxide dispersion liquid (the graphene oxide dispersion liquid is a graphene oxide/N, N-dimethylformamide dispersion liquid) at the temperature of 30 ℃ under the atmosphere of inert gas (nitrogen), and performing ultrasonic treatment to obtain a dispersion liquid A; wherein the concentration of the nano black phosphorus dispersion liquid (black phosphorus quantum dot/N, N-dimethylformamide dispersion liquid) is 1mg/mL, the concentration of the graphene oxide dispersion liquid (graphene oxide/N, N-dimethylformamide dispersion liquid) is 4mg/mL, and the mass ratio of the nano black phosphorus to the graphene oxide is 1: 4; the ultrasonic treatment is ultrasonic pretreatment by adopting an ultrasonic cleaner, the power of the ultrasonic cleaner is 300W, and the treatment time of the ultrasonic cell cleaner is 1 h;
(2) under the atmosphere of inert gas (mixed gas of argon gas/nitrogen gas), treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material;
scanning electron microscopy, XPS characterization and electrocatalytic oxygen evolution performance test are carried out on the nano black phosphorus/three-dimensional graphene nano composite material prepared in the embodiment, detection and analysis show that the composite material has a three-dimensional network structure, the nano phosphorus and the graphene in the composite material form a P-O-C bond, and the linear voltammetry scanning test shows that the composite material has good electrocatalytic performance.
Example 5: a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing a nano black phosphorus dispersion liquid (the nano black phosphorus dispersion liquid is a black phosphorus quantum dot/ethanol dispersion liquid) and a graphene oxide dispersion liquid (the graphene oxide dispersion liquid is a graphene oxide ethanol dispersion liquid) at the temperature of 25 ℃ under the atmosphere of inert gas (nitrogen), and performing ultrasonic treatment to obtain a dispersion liquid A; wherein the concentration of the nano black phosphorus dispersion liquid (black phosphorus quantum dot/ethanol dispersion liquid) is 1mg/mL, the concentration of the graphene oxide dispersion liquid (graphene oxide/ethanol dispersion liquid) is 4mg/mL, and the mass ratio of the nano black phosphorus to the graphene oxide is 1: 3; the ultrasonic treatment is ultrasonic pretreatment by adopting an ultrasonic cleaner and a cell crusher, wherein the power of the ultrasonic cleaner is 150W, the ultrasonic time is 0.5h, the power of the cell crusher is 1000W, and the ultrasonic time is 0.5 h;
(2) under the inert gas (nitrogen) atmosphere, treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material;
scanning electron microscopy, XPS characterization and electrocatalytic oxygen evolution performance test are carried out on the nano black phosphorus/three-dimensional graphene nano composite material prepared in the embodiment, detection and analysis show that the composite material has a three-dimensional network structure, the nano phosphorus and the graphene in the composite material form a P-O-C bond, and the linear voltammetry scanning test shows that the composite material has good electrocatalytic performance.
Example 6: a preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material comprises the following specific steps:
(1) mixing a nano black phosphorus dispersion liquid (the nano black phosphorus dispersion liquid is a black phosphorus quantum dot/isopropanol dispersion liquid) and a graphene oxide dispersion liquid (the graphene oxide dispersion liquid is a graphene oxide isopropanol dispersion liquid) at the temperature of 25 ℃ under the atmosphere of inert gas (nitrogen), and performing ultrasonic treatment to obtain a dispersion liquid A; wherein the concentration of the nano black phosphorus dispersion liquid (black phosphorus quantum dot/isopropanol dispersion liquid) is 1mg/mL, the concentration of the graphene oxide dispersion liquid (graphene oxide/isopropanol dispersion liquid) is 4mg/mL, and the mass ratio of the nano black phosphorus to the graphene oxide is 1: 1; the ultrasonic treatment is ultrasonic pretreatment by adopting a cell crusher, and the ultrasonic treatment time is 2 hours;
(2) under the inert gas (nitrogen) atmosphere, treating the dispersion liquid A obtained in the step (1) by liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material;
scanning electron microscopy, XPS characterization and electrocatalytic oxygen evolution performance test are carried out on the nano black phosphorus/three-dimensional graphene nano composite material prepared in the embodiment, detection and analysis show that the composite material has a three-dimensional network structure, the nano phosphorus and the graphene in the composite material form a P-O-C bond, and the linear voltammetry scanning test shows that the composite material has good electrocatalytic performance.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (3)
1. A preparation method of a high-stability nano black phosphorus/three-dimensional graphene composite material is characterized by comprising the following specific steps:
(1) mixing the nano black phosphorus dispersion liquid with the graphene oxide dispersion liquid at the temperature of 5-30 ℃ under the inert gas atmosphere, and performing ultrasonic treatment to obtain a dispersion liquid A; the mass ratio of the nano black phosphorus to the graphene oxide is 1 (1-4), ultrasonic pretreatment is carried out by adopting an ultrasonic cell cleaner and/or a cell crusher, the power of the ultrasonic cell cleaner is 150-300W, the power of the cell crusher is 500-1500W, and the ultrasonic treatment time is 0.5-3 h;
(2) and (2) under the inert gas atmosphere, treating the dispersion liquid A obtained in the step (1) by using liquid nitrogen, and freeze-drying to obtain the nano black phosphorus/three-dimensional graphene nano composite material.
2. The preparation method of the high-stability nano black phosphorus/three-dimensional graphene composite material according to claim 1, wherein the preparation method comprises the following steps: the nano black phosphorus in the step (1) is black phospholene, black phosphorus quantum dots or black phosphorus nanowires; the dispersion solvent of the nano black phosphorus dispersion liquid is water, ethanol, dimethyl sulfoxide, N-methyl pyrrolidone, isopropanol, N-dimethylformamide, ethylene carbonate or 1-butyl-trimethyl imidazole dicyandiamide; the dispersion solvent of the graphene oxide dispersion liquid is water, ethanol, dimethyl sulfoxide, N-methyl pyrrolidone, isopropanol, N-dimethylformamide, ethylene carbonate or 1-butyl-trimethyl imidazole dicyandiamide.
3. The preparation method of the high-stability nano black phosphorus/three-dimensional graphene composite material according to claim 1, wherein the preparation method comprises the following steps: the inert gas is one or two of argon, nitrogen and helium.
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| CN109592962B (en) * | 2019-01-28 | 2020-08-04 | 北京航空航天大学 | Preparation method of bionic ternary system graphene-black phosphorus nanocomposite film |
| CN110627049A (en) * | 2019-11-04 | 2019-12-31 | 青岛大学 | Preparation method and application of graphene-loaded black phosphorus quantum dot |
| CN111422840B (en) * | 2020-04-01 | 2022-12-13 | 东华理工大学 | Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof |
| CN111554908B (en) * | 2020-05-19 | 2021-08-03 | 上海健康医学院 | Three-dimensional porous black phosphorus alkene/graphene for magnesium ion battery and preparation method and application thereof |
| CN111892026A (en) * | 2020-07-30 | 2020-11-06 | 河南大学 | Preparation method of black phosphorus quantum dot and graphene composite nano material |
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