CN113387357A - Preparation method of MXene folded nanospheres - Google Patents

Preparation method of MXene folded nanospheres Download PDF

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Publication number
CN113387357A
CN113387357A CN202110832772.1A CN202110832772A CN113387357A CN 113387357 A CN113387357 A CN 113387357A CN 202110832772 A CN202110832772 A CN 202110832772A CN 113387357 A CN113387357 A CN 113387357A
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mxene
folded
nanospheres
nozzle
preparing
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吴语
张骥弟
林爱平
赵玬浇
王淑芬
曹磊
熊仕显
顾锋
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Suzhou Weizhi Electronic Technology Co ltd
Jiangxi University of Science and Technology
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Suzhou Weizhi Electronic Technology Co ltd
Jiangxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/0828—Carbonitrides or oxycarbonitrides of metals, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/921—Titanium carbide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/949—Tungsten or molybdenum carbides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

The invention discloses a preparation method of MXene folded nanospheres, which comprises the following steps: the preparation method of the MXene folded nanosphere comprises the following steps: step 1, MXene ink configuration; step 2, preparing and conveying MXene fog drops; step 3, controlling MXene aerosol droplets; step 4, collecting MXene folded nanospheres; the MXene folded nanospheres prepared by the method have obvious spherical appearance and obvious pores, so that the self-stacking phenomenon is avoided; the MXene folded nanospheres and the preparation method thereof provided by the invention have the advantages that the used raw materials are easy to obtain, the preparation process is simple, the environment-friendly effect is realized, the operability is strong, and the MXene folded nanospheres are suitable for continuous preparation.

Description

Preparation method of MXene folded nanospheres
Technical Field
The invention relates to the field of nano material preparation, in particular to a preparation method of MXene folded nanospheres.
Background
MXene is a two-dimensional material developed in recent years, shows excellent electrical, mechanical, magnetic, optical and thermal properties due to a unique structure, and has a good application prospect in the fields of energy storage, catalysis, luminescence, biology and the like. At present, most of researches and applications of MXene nano materials are single-layer or few-layer MXene nanosheets formed on the basis of flaking, but due to the existence of van der Waals force between the MXene nanosheets, the MXene nanosheets are easy to stack, a large number of active sites on the MXene surface cannot play a role, and therefore the MXene nano materials cannot fully play performance advantages when being applied to the fields of photoelectricity, energy sources and the like. Compared with stacked nanosheets, the MXene nanospheres not only have huge specific surface area, but also provide space for the transmission of electrolyte ions when being applied to the field of energy. But due to the high bending rigidity of the MXene nanosheets, the MXene nanosheets are difficult to bend into balls by the traditional method.
Disclosure of Invention
The invention aims to provide a preparation method of MXene folded nanospheres, and solves the problems that the performance and application of conventional MXene nano materials are influenced due to self-stacking.
The invention is realized in such a way that a preparation method of MXene folded nanospheres comprises the following steps:
step 1, MXene ink configuration;
step 2, preparing and conveying MXene fog drops;
step 3, controlling MXene aerosol droplets;
and 4, collecting MXene folded nanospheres.
The further technical scheme of the invention is as follows: in the step 1, the MXene ink is configured as follows: placing MXene raw materials in the dispersion liquid to obtain a solution with the mass concentration of 0.1-100 g/L.
The further technical scheme of the invention is as follows: the MXene raw material is composed of one or more of titanium nitride, molybdenum nitride, titanium carbide, vanadium carbide, molybdenum carbide and titanium carbonitride.
The further technical scheme of the invention is as follows: the dispersion liquid is as follows: one or more of deionized water, methanol, ethanol, ethylene glycol, glycerol, dimethylformamide, and N-methylpyrrolidone.
The further technical scheme of the invention is as follows: in the step 2, MXene fog drops are prepared as follows:
ultrasonic atomization or pneumatic atomization.
The further technical scheme of the invention is as follows: during ultrasonic atomization, atomizing a fog mass with aerosol droplet diameter of 0.5-50 μm, connecting carrier gas A to an atomization bottle, connecting a fog outlet of the atomization bottle to a nozzle through a pipeline, wherein the ultrasonic atomization frequency is 20 KHz-2.4 MHz, and the carrier gas A is 1-400 sccm.
The further technical scheme of the invention is as follows: during pneumatic atomization, carrier gas A is connected to an atomization bottle, atomized aerosol fog droplets with diameters of 0.5-100 microns are atomized, a fog outlet of the atomization bottle is connected to a fog droplet screening device through a pipeline, the treated fog droplets with diameters of 0.5-50 microns are obtained, and then the atomized aerosol fog droplets are connected to a nozzle through a pipeline, wherein the carrier gas A is 100-1500 sccm.
The further technical scheme of the invention is as follows: in the step 3, the MXene aerosol droplets are controlled as follows: the fog cluster is led into a nozzle with a conical nested structure inside, bound gas B with the flow rate of 20-1000 sccm is communicated to the side of the fog cluster to form an annular bound gas flow field, the temperature of carrier gas is 10-60 ℃, and the diameter of the nozzle is 50-1000 microns.
The further technical scheme of the invention is as follows: in the step 4, the collection of MXene folded nanospheres is as follows: and (3) spraying the aerosol droplets obtained in the step (3) through a nozzle spray head, and depositing the aerosol droplets on a substrate with a preheated surface to finally obtain an MXene folded nano-sphere structure, wherein the preheating temperature of the substrate is 25-300 ℃.
The invention has the beneficial effects that: 1. the MXene folded nanospheres prepared by the method have obvious spherical appearance and obvious pores, so that the self-stacking phenomenon is avoided.
2. The MXene folded nanospheres and the preparation method thereof provided by the invention have the advantages that the used raw materials are easy to obtain, the preparation process is simple, the environment-friendly effect is realized, the operability is strong, and the MXene folded nanospheres are suitable for continuous preparation.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of MXene pleated nanospheres provided by the invention;
fig. 2 is a single-layer or few-layer Ti3C2Tx SEM photograph of the method for preparing MXene pleated nanospheres provided by the invention;
fig. 3 is an SEM photograph of a Ti3C2Tx pleated nanosphere prepared by the method of the present invention;
fig. 4 is a TEM photograph of Ti3C2Tx folded nanospheres of the method for preparing MXene folded nanospheres provided by the invention.
Detailed Description
The first embodiment is as follows: a preparation method of MXene folded nanospheres comprises the following steps:
1) selecting one or more of a certain amount of titanium nitride, molybdenum nitride, titanium carbide, vanadium carbide, molybdenum carbide and titanium carbonitride as MXene raw materials, placing the MXene raw materials into a dispersion liquid consisting of one or more of a certain amount of deionized water, methanol, ethanol, ethylene glycol, glycerol, dimethylformamide and N-methylpyrrolidone to obtain a solution with the mass concentration of 0.1-100 g/L, and carrying out ultrasonic treatment.
2) And (2) putting the MXene ink quantitatively selected and prepared in the step 1) into an ultrasonic atomization bottle, atomizing the ink into a fog cluster by using an ultrasonic atomizer, wherein the fog cluster consists of micron-sized aerosol droplets comprising MXene nanosheets, and a carrier gas A is communicated with the ultrasonic atomization bottle to generate a flowing MXene aerosol fog cluster.
3) Introducing the MXene aerosol mist from the step 2) into a nozzle along with the airflow through a pipeline. Wherein, the nozzle is internally provided with a conical nested structure, the side of the nozzle is communicated with bound gas B, and the bottom of the nozzle is provided with a micron-sized spray head. Under the control of the nozzle, aerosol droplets carrying MXene are finely sprayed out by a micron-sized spray head.
4) And (3) spraying the aerosol droplets sprayed in the step 3) through a nozzle spray head, and depositing the aerosol droplets on a substrate with a preheated surface to finally obtain the MXene folded nanosphere structure.
Preferably, the frequency of the ultrasonic atomizer in the step 2) is 20 KHz-2.4 MHz, the flow of the carrier gas A communicated into the ultrasonic atomization bottle is 1-400 sccm, and the particle size of atomized aerosol droplets is 0.5-50 μm.
Preferably, the flow rate of the bound gas B communicated with the lateral side in the step 3) is 20-1000 sccm, and the temperature of the bound gas B is 10-60 ℃; the diameter of the micron-sized spray head arranged at the bottom of the spray nozzle is 50-1000 mu m.
Preferably, the temperature of the surface preheating substrate in the step 4) is 25-300 ℃.
Example two: a preparation method of MXene folded nanospheres comprises the following steps:
1) selecting one or more of a certain amount of titanium nitride, molybdenum nitride, titanium carbide, vanadium carbide, molybdenum carbide and titanium carbonitride as MXene raw materials, placing the MXene raw materials in a dispersion liquid consisting of one or more of a certain amount of deionized water, methanol, ethanol, ethylene glycol, glycerol, dimethylformamide and N-methylpyrrolidone to obtain an MXene ink solution with the mass concentration of 0.1-100 g/L, and carrying out ultrasonic treatment.
2) And (3) placing the MXene ink quantitatively selected and prepared in the step 1) into a pneumatic atomization bottle, and introducing carrier gas A into the pneumatic atomization bottle. The ink is atomized into a fog cluster, the fog cluster consists of micron-sized aerosol droplets containing MXene nanosheets, and the MXene aerosol fog cluster flows by the communicated carrier gas A.
3) Introducing the MXene aerosol mist from the step 2) into a mist droplet screening device along with air flow through a pipeline, connecting the screening device with an air suction C, separating and removing large-particle-size aerosol mist droplets, and leaving small-particle-size aerosol mist droplet mist.
4) Introducing the small-particle-size MXene aerosol mist from the step 3) into a nozzle along with air flow through a pipeline. Wherein, the nozzle is internally provided with a conical nested structure, the side of the nozzle is communicated with bound gas B, and the bottom of the nozzle is provided with a micron-sized spray head; under the control of the nozzle, aerosol droplets carrying MXene are finely sprayed out by a micron-sized spray head.
5) And (3) spraying the aerosol droplets sprayed in the step 4) through a nozzle spray head, and depositing the aerosol droplets on a substrate with a preheated surface to finally obtain the MXene folded nanosphere structure.
Preferably, the flow rate of the pneumatic atomization carrier gas A in the step 2) is 200-1500 sccm.
Preferably, the flow rate of the inspiration gas C is 0-1500 sccm in the step 3), and the particle size of the small-particle size aerosol fog drops is 0.5-50 μm.
Preferably, the flow rate of the bound gas B communicated with the side in the step 4) is 20-1000 sccm; the diameter of the micron-sized spray head arranged at the bottom is 50-1000 mu m.
Preferably, the temperature of the surface preheating substrate in the step 5) is 25-300 ℃.
Example three: a preparation method of MXene folded nanospheres comprises the following steps:
1) and weighing 0.1g of stripped single-layer or few-layer V2CTx MXene nanosheets, adding the nanosheets into 1000mL of ethanol, and performing ultrasonic treatment to obtain a stable dispersion liquid with a mass concentration of 0.1 g/L.
2) Placing 20mL of the MXene ink selected and prepared in the step 1) into an ultrasonic atomization bottle, atomizing the ink into micron-sized aerosol droplets containing V2CTx MXene nanosheets by using a 1.7MHz ultrasonic atomizer, wherein the particle size of the atomized aerosol droplets is 0.5-20 microns, and a carrier gas A flow of 52sccm is introduced into the ultrasonic atomization bottle to generate flowing aerosol mist clusters.
3) Introducing the MXene aerosol mist from the step 2) into a nozzle along with the airflow through a pipeline. Wherein, the inner part of the nozzle is a conical nested structure, the flow rate of the bound gas B is 116sccm, the temperature is 23 ℃, the side is communicated, and the bottom is matched with a spray head with the diameter of 300 mu m. The bound gas B flows downwards along a conical nested structure gap in the nozzle to form an annular bound flow field, the flow field is converged with micron-sized aerosol mist containing V2CTx MXene nanosheets before entering the spray head, and the formed aerosol mist is contracted to spray out the mist drops.
4) And (3) spraying the aerosol droplets sprayed in the step 3) through a nozzle spray head, and depositing the aerosol droplets on a substrate with the surface preheating temperature of 100 ℃ to finally obtain the V2CTx MXene folded nanosphere structure.
Example four: a preparation method of MXene folded nanospheres comprises the following steps:
1) and weighing 5g of stripped single-layer or few-layer Ti2NTx MXene nanosheets, adding the nanosheets into 50mL of ethylene glycol, and performing ultrasonic treatment to obtain a stable dispersion liquid with the mass concentration of 5 g/L.
2) Putting the Ti2NTx MXene ink quantitatively selected and prepared in the step 1) into a pneumatic atomization bottle, and introducing a carrier gas A with the flow of 1000sccm into the pneumatic atomization bottle. The ink is atomized into micron-sized aerosol droplets containing MXene nanosheets, the particle size of the droplets is 0.7-100 microns, and flowing MXene aerosol mist clusters are generated through pneumatic atomization.
3) Introducing the MXene aerosol mist from the step 2) into a mist droplet screening device along with air flow through a pipeline, connecting the screening device with a suction gas C with the flow of 600sccm, separating and removing the aerosol mist droplets with large particle size, and leaving the mist with the particle size of 0.7-50 microns.
4) Introducing the MXene aerosol mist with the particle size of 0.7-50 μm obtained in the step 3) into a nozzle along with air flow through a pipeline. Wherein, the inner part of the nozzle is a conical nested structure, the bottom of the nozzle is matched with a spray head with the diameter of 500 mu m, the lateral side of the nozzle is communicated with a bounding gas B with the flow of 800sccm and the temperature of 45 ℃ flows downwards along the gap of the conical nested structure in the nozzle to form an annular bounding flow field. Before entering the spray head, the annular flow field is converged with the aerosol cloud, and the beam-shaped aerosol cloud is contracted to spray out the fog drops.
5) And (3) spraying aerosol droplets sprayed in the step 4) through a nozzle spray head, depositing in a container with the surface preheating temperature of 105 ℃, and finally obtaining the Ti2NTx MXene folded nanosphere structure.
Example five: a preparation method of MXene folded nanospheres comprises the following steps:
1) 0.5g of peeled single-layer or few-layer Ti3C2Tx and V2CTx mixed MXene nanosheets are weighed, added into 100mL of dimethylformamide and subjected to ultrasonic treatment to obtain a stable dispersion liquid with the mass concentration of 5 g/L.
2) Placing 20mL of mixed MXene ink prepared in the step 1) and mixed with Ti3C2Tx and V2CTx into an ultrasonic atomization bottle, atomizing the ink into micron-sized aerosol droplets containing MXene nanosheets by using a 2.1MHz ultrasonic atomizer, wherein the particle size of the atomized aerosol droplets is 0.5-15 micrometers, and the carrier gas A flows into the ultrasonic atomization bottle at 305sccm to generate flowing aerosol mist clusters.
3) Introducing the mixed MXene aerosol mist of Ti3C2Tx and V2CTx in the step 2) into a nozzle along with the airflow through a pipeline. Wherein, the inner part of the nozzle is a conical nested structure, the flow rate of the bound gas B is 510sccm, the temperature is 60 ℃, the side is communicated, and the bottom is selectively provided with a spray head with the diameter of 700 mu m. The bound gas B flows downwards along the conical nested structure gap in the nozzle to form an annular bound flow field, the flow field is converged with micron-sized aerosol mist containing mixed MXene nano-sheets before entering the spray head, and the bundled aerosol mist is contracted to spray out mist drops.
4) Spraying aerosol droplets sprayed in the step 3) through a nozzle spray head, depositing in a container with the surface preheating temperature of 210 ℃, and finally obtaining the Ti3C2Tx and V2CTx mixed folded nano-sphere structure.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (9)

1. The preparation method of the MXene folded nanospheres is characterized by comprising the following steps of:
step 1, MXene ink configuration;
step 2, preparing and conveying MXene fog drops;
step 3, controlling MXene aerosol droplets;
and 4, collecting MXene folded nanospheres.
2. The method for preparing MXene folded nanospheres according to claim 1, wherein in step 1, MXene ink is configured as follows: placing MXene raw materials in the dispersion liquid to obtain a solution with the mass concentration of 0.1-100 g/L.
3. The method for preparing MXene folded nanospheres according to claim 2, wherein: the MXene raw material is composed of one or more of titanium nitride, molybdenum nitride, titanium carbide, vanadium carbide, molybdenum carbide and titanium carbonitride.
4. The method for preparing MXene folded nanospheres according to claim 3, wherein the dispersion liquid is: one or more of deionized water, methanol, ethanol, ethylene glycol, glycerol, dimethylformamide, and N-methylpyrrolidone.
5. The method for preparing MXene folded nanospheres according to claim 1, wherein in the step 2, MXene fog droplets are prepared by: ultrasonic atomization or pneumatic atomization.
6. The method for preparing MXene folded nanospheres according to claim 5, wherein during the ultrasonic atomization, the atomized aerosol droplets with a diameter of 0.5-50 μm are atomized and the carrier gas A is delivered to the atomizing bottle, the mist outlet of the atomizing bottle is connected to the nozzle through the pipeline, the ultrasonic atomization frequency is 20 KHz-2.4 MHz, and the carrier gas A is 1-400 sccm.
7. The method for preparing MXene folded nanospheres according to claim 6, wherein during pneumatic atomization, carrier gas A is introduced into an atomization bottle, atomized aerosol droplets with a diameter of 0.5-100 μm are atomized into a mist, a mist outlet of the atomization bottle is connected to a droplet screening device through a pipeline, the treated mist is treated to obtain a mist with a particle size of 0.5-50 μm, and then the treated mist is connected to a nozzle through a pipeline, and the carrier gas A of pneumatic atomization gas flow is 100-1500 sccm.
8. The method for preparing MXene folded nanospheres according to claim 1, wherein in step 3, MXene aerosol droplets are controlled as follows: the fog cluster is led into a nozzle with a conical nested structure inside, bound gas B with the flow rate of 20-1000 sccm is communicated to the side of the fog cluster to form an annular bound gas flow field, the temperature of carrier gas is 10-60 ℃, and the diameter of the nozzle is 50-1000 microns.
9. The method for preparing MXene folded nanospheres according to claim 1, wherein in step 4, collection of MXene folded nanospheres is as follows: and (3) spraying the aerosol droplets obtained in the step (3) through a nozzle spray head, and depositing the aerosol droplets on a substrate with a preheated surface to finally obtain an MXene folded nano-sphere structure, wherein the preheating temperature of the substrate is 25-300 ℃.
CN202110832772.1A 2021-07-22 2021-07-22 Preparation method of MXene folded nanospheres Pending CN113387357A (en)

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