CN117623312A - Method for preparing molybdenum carbide/carbon nanospheres based on electrostatic spinning technology and application of molybdenum carbide/carbon nanospheres - Google Patents
Method for preparing molybdenum carbide/carbon nanospheres based on electrostatic spinning technology and application of molybdenum carbide/carbon nanospheres Download PDFInfo
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- 239000002077 nanosphere Substances 0.000 title claims abstract description 62
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910039444 MoC Inorganic materials 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 35
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 20
- 238000005516 engineering process Methods 0.000 title claims abstract description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 238000009987 spinning Methods 0.000 claims abstract description 15
- 238000004146 energy storage Methods 0.000 claims abstract description 13
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 12
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 8
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 8
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 8
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000011049 filling Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001523 electrospinning Methods 0.000 claims description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 16
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
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- 239000000835 fiber Substances 0.000 description 5
- 239000002071 nanotube Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000003487 electrochemical reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a method for preparing molybdenum carbide/carbon composite nanospheres based on an electrostatic spinning technology, which comprises the following steps: adding ammonium molybdate into dimethylformamide, stirring for 2 hours, then adding polyacrylonitrile, and stirring for 6 hours to obtain spinning solution; and (3) filling the spinning solution into a 10mL syringe for electrostatic spinning to obtain precursor nanospheres Mo@PAN, and placing the precursor nanospheres Mo@PAN in a tubular furnace for heat treatment to obtain the molybdenum carbide/carbon composite nanospheres. Also provides the application in the fields of electrocatalytic hydrogen evolution, energy storage, coating materials and the like. The molybdenum carbide/carbon composite nanospheres prepared by the method have uniform size distribution and good dispersibility. The spherical structure has good mechanical property, can ensure the structural stability of the material in the application process, and prevents the microstructure of the material from being damaged. Meanwhile, the spherical morphology of the nanometer scale provides a higher specific surface area, which provides more active sites for the material in the applications of catalysis, energy storage and the like and is beneficial to improving the material performance.
Description
Technical Field
The invention belongs to the technical field of functional material preparation, and particularly relates to a method for preparing molybdenum carbide/carbon composite nanospheres based on an electrostatic spinning technology and application thereof.
Background
Molybdenum carbide (Mo) 2 C) Is a functional material with high melting point and high thermal stability, and has important application in a plurality of fields such as catalysis, energy storage, electromagnetic wave absorption and the like. The molybdenum carbide is easy to form rich interface structures in the process of compounding with the carbon material, which is beneficial to further improving the service performance of the material. Mo (Mo) 2 The preparation of C nanospheres has been widely studied and there are several existing synthetic techniques. Some of the most common production of Mo 2 The method for C nanospheres comprises the following steps:
1. chemical Vapor Deposition (CVD): this is a method of thermally decomposing a vapor precursor on a substrate to form Mo 2 C, technology of C. This method is relatively simple and scalable, but it requires high temperatures and can produce non-uniform particle sizes, and requires high temperature or high pressure conditions, which can be difficult to achieve and maintain.
2. Solvothermal synthesis: the method involves dissolving precursors using a solvent, and then heating them under high pressure conditions to form Mo 2 And C, nanospheres. This method can produce uniform particle size but requires careful control of reaction conditions and is time consuming.
3. Hydrothermal synthesis: the method involves using an aqueous solution containing a precursor and then heating under high pressure conditions to form Mo 2 And C, nanospheres. The method is relatively simple, has uniform particle size, but has higher reaction conditionsIs not limited.
4. Template auxiliary synthesis: the method involves guiding Mo using a template (e.g., porous material) 2 And C, formation of nanospheres. This method can produce uniform particle size and shape, but requires the preparation of a suitable template.
Many of the existing methods are difficult to apply to large-scale industrial production, which can limit their practical application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing molybdenum carbide/carbon composite nanospheres based on an electrostatic spinning technology and application thereof, and the molybdenum carbide/carbon composite nanospheres prepared by the method have uniform size distribution and good dispersibility, and can be applied to the fields of catalysis, energy storage, sensing and the like.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing molybdenum carbide/carbon composite nanospheres based on an electrostatic spinning technology comprises the following steps:
s1, adding ammonium molybdate into dimethylformamide, stirring for 2 hours, then adding polyacrylonitrile, and stirring for 6 hours to obtain spinning solution;
s2, filling the spinning solution obtained in the step S1 into a 10mL syringe for electrostatic spinning to obtain a precursor nanosphere Mo@PAN;
the electrostatic spinning method comprises the following steps: connecting a stainless steel flat-mouth needle with the inner diameter of 1.40mm and the outer diameter of 1.80mm to a positive electrode, placing tinfoil on a receiving plate, connecting the receiving plate to a negative electrode, wherein the distance between the two plates is 9cm, the voltage is 16kV high voltage, and the speed of a propeller is 2mm/h;
s3, placing the precursor nanospheres Mo@PAN obtained in the step S2 in a tube furnace, and performing heat treatment in a nitrogen atmosphere to obtain molybdenum carbide/carbon composite nanospheres; the heat treatment procedure is as follows: heating from room temperature to 800 ℃ at a heating rate of 1 ℃/min, preserving heat for 2 hours, naturally cooling to room temperature, and stopping introducing nitrogen when the temperature is reduced to 100 ℃.
Preferably, the ammonium molybdate, dimethylformamide and polyacrylonitrile are used in an amount ratio of 0.07656g in S1: 10mL:0.0957g.
Preferably, the average particle diameter of the molybdenum carbide/carbon composite nanospheres in S3 is 160nm.
The invention also provides application of the molybdenum carbide/carbon composite nanospheres prepared by the method, wherein the molybdenum carbide/carbon composite nanospheres are used for catalysis, energy storage or sensing; in the catalytic field, this particular structure of spheres provides a high specific surface area, which provides more active sites for the catalytic reaction. Can better play roles in the processes of hydrogenation, dehydrogenation, hydrodesulfurization and the like. The spherical molybdenum carbide/carbon nano-particles can be used as electrode materials of energy storage devices such as lithium ion batteries, supercapacitors and the like. The high specific surface area of the material can promote efficient electrochemical reaction and enhance energy storage property; meanwhile, the spherical structure has good mechanical property, and can ensure the structural stability of the material in the application process and prevent the microstructure of the material from being damaged. In applications in the field of coating materials, spherical molybdenum carbide particles can be used as a coating or additive to improve the properties of the material. They can improve wear resistance, hardness and high temperature stability after being incorporated into a coating or composite.
Compared with the prior art, the invention has the following advantages:
1. the invention has simple experimental equipment, does not need complex experimental instruments, saves a great deal of experimental cost and has mild experimental conditions. Only ammonium molybdate and PAN were used as raw materials during the whole preparation process (solvent DMF had volatilized in electrospinning), and electrospinning technology and high temperature heat treatment process. In the heat treatment process, impurity components except molybdenum carbide and carbon can be completely decomposed and removed in a gas form, and the prepared sample has high purity and lower impurity content, so that a relatively simple and lower-cost method is provided for preparing the molybdenum carbide/carbon composite nanospheres.
2. The preparation method controls the size and shape of particles, and the molybdenum carbide/carbon composite nanospheres with good dispersibility and uniform size can be obtained controllably by selecting a proper high polymer system (PAN high polymer and DMF solvent) and preparing spinning solution and carrying out electrostatic spinning technology.
3. The performance and application of the invention: compared with other molybdenum carbide forms (such as porous molybdenum carbide nano-fibers), the nanospheres have higher surface areas, and the higher surface areas provide more active sites for catalytic reaction, so that the catalytic activity is improved. At the same time, the nanotubes may vary in length, diameter and morphology, the nanospheres exhibit uniform morphology and size distribution, their uniformity ensures stable performance in a variety of applications, and the spherical morphology of the nanospheres makes it easier for them to enter the surface region, making reactant molecules or gases more accessible. This accessibility increases the efficiency of the catalytic reaction by increasing the utilization of the active sites. Furthermore, nanotubes are prone to bending or collapsing under certain conditions, while nanospheres generally have higher mechanical stability, their robustness enables their use in harsh reaction environments and provides durability in a variety of applications.
There are also some differences between nanospheres and them in application. The nanospheres can be used as catalysts for hydrogen generation reactions, fuel cells, electrochemical reactions, chemical syntheses, and the like. It can also be used as a reinforcing agent for metal matrix composites, providing better mechanical properties and thermal stability. In addition, the nanospheres can be used for electrochemical energy storage devices such as super capacitors, lithium ion batteries and the like, and provide higher energy storage and rapid charge and discharge characteristics.
4. The preparation method has expandability and repeatability, and the high-temperature heat treatment and electrostatic spinning technology can easily produce spherical molybdenum carbide in a larger scale. The process can be consistently reproduced, ensuring reliable and consistent results for different production lots.
The invention is described in further detail below with reference to the drawings and examples.
Drawings
Fig. 1 is an SEM scanning electron microscope image of precursor nanospheres mo@pan of example 1 of the present invention.
Fig. 2 is an SEM scanning electron microscope image of the molybdenum carbide/carbon composite nanospheres of example 1 of the present invention.
Fig. 3 is an XRD pattern of the molybdenum carbide/carbon composite nanospheres of example 1 of the present invention.
FIG. 4 is an SEM scanning electron micrograph of Mo@PVP-5, mo@PVP-3, mo@PVP-2, [email protected] and Mo@PVP-1 of example 1 of the present invention.
FIG. 5 is an SEM image of a sample obtained from a Mo@PVP-1 precursor of example 1 of the present invention after a high temperature heat treatment.
FIG. 6 is an SEM scanning electron micrograph of Mo@PAN-1, mo@PAN-2 and Mo@PAN-3 of example 1 of the present invention.
Detailed Description
Example 1
The method for preparing the molybdenum carbide/carbon composite nanospheres based on the electrostatic spinning technology comprises the following steps:
s1, adding 0.07656g of ammonium molybdate into 10mL of Dimethylformamide (DMF), stirring for 2h, then adding 0.0957g of polyacrylonitrile (PAN, average molecular weight: 149900-151000), and stirring for 6h to obtain spinning solution;
s2, filling the spinning solution obtained in the step S1 into a 10mL syringe for electrostatic spinning to obtain a precursor nanosphere Mo@PAN;
the electrostatic spinning method comprises the following steps: connecting a stainless steel flat-mouth needle with an inner diameter of 1.40mm and an outer diameter of 1.80mm to a positive electrode, placing tinfoil on a receiving plate, connecting the receiving plate to a negative electrode, wherein the distance between the two plates is 9cm, the voltage is 16kV high voltage, and the speed of a propeller is 2mm/h so as to push the syringe;
as shown in fig. 1, which is an SEM scanning electron microscope image of precursor nanospheres mo@pan, the morphology of the sample is mainly beads with uniform size distribution, the sphericity of the beads is good, few fibers are arranged among the beads, but the content of the fibers is very limited.
S3, placing the precursor nanospheres Mo@PAN obtained in the step S2 in a tube furnace, and performing heat treatment in a nitrogen atmosphere to obtain molybdenum carbide/carbon (Mo) with an average particle size of 160nm 2 C/C) composite nanospheres; the heat treatment procedure is as follows: heating from room temperature to 800 ℃ at a heating rate of 1 ℃/min, preserving heat for 2 hours, naturally cooling to room temperature, and stopping introducing nitrogen when the temperature is reduced to 100 ℃.
As shown in an SEM image of the molybdenum carbide/carbon composite nanospheres, the material still maintains the form of beads, the particles are basically free of fibrous adhesion, the beads have good dispersibility and uniform size distribution, as shown in the figure 2.
XRD analysis of the final product thus prepared was carried out as shown in FIG. 3, and it was found that the XRD pattern contained a molybdenum carbide diffraction peak having a high peak intensity and an amorphous diffraction peak of carbon, and that no diffraction peak of other impurity components was present. Indicating that during the reaction, molybdenum carbide components with better crystallization state are generated.
The impurity content in the final product prepared by the method is low, only ammonium molybdate and PAN are used as raw materials (solvent DMF is volatilized in electrostatic spinning) in the preparation process, and under the condition of high-temperature heat treatment, impurity elements (such as N, O, H and the like) are completely decomposed and removed in a gas form, so that the prepared sample has high purity and low impurity content.
In the embodiment, a proper high polymer system (PAN high polymer and DMF solvent) is selected, and a spinning solution with specific concentration is prepared, so that the molybdenum carbide/carbon composite nanospheres with good dispersibility and uniform size can be obtained through the electrostatic spinning technology.
In the selection of the polymer system, attempts were also made to prepare precursors using the PVP system (PVP polymer+absolute ethanol solvent) and explored the effect of different spin fluid concentrations on the morphology of electrospun precursors. As shown in fig. 4, SEM scanning electron microscope photographs of mo@pvp precursor samples obtained after electrospinning using PVP spinning solutions of different concentrations. Wherein Mo@PVP-5 (a), mo@PVP-3 (b), mo@PVP-2 (c), [email protected] (d) and Mo@PVP-1 (e) represent the PVP content of the spinning solution of 5,3,2,1.5 and 1wt% respectively. It can be seen that as the concentration of PVP in the spinning solution decreases, the morphology of the precursor gradually changes from fiber to bead, but the morphology uniformity of the precursor bead obtained with the PVP system is poor. As shown in FIG. 5, an SEM scanning electron microscope image of a sample is obtained after Mo@PVP-1 precursor is subjected to high temperature heat treatment, and it can be seen that the morphology of the obtained sample beads cannot be completely maintained after the precursor is subjected to high temperature heat treatment, obvious adhesion occurs between particles, and the dispersibility is poor.
Based on the determination of PAN as a polymer system, the optimal concentration of PAN solution is further explored, and as shown in FIG. 6, SEM scanning electron microscope pictures of Mo@PAN precursor samples obtained by adopting PAN spinning solutions with different concentrations through electrostatic spinning are obtained. Wherein Mo@PAN-1 (a), mo@PAN-2 (b) and Mo@PAN-3 (c) represent the content of PAN in the spinning solution to be 1,2 and 3 weight percent respectively. It can be seen that when the PAN concentration in the dope is higher (mo@pan-3), the morphology of the sample is spindle-shaped, and as the PAN concentration decreases (mo@pan-2), the particles become spherical, but there is still a large number of fibers between the particles; at a PAN concentration of 1wt% (mo@pan-1), the particle morphology was essentially spherical with little fiber content, being the best uniformity, dispersibility of the particle morphology in all samples. Thus, a PAN polymer system (PAN polymer+DMF solvent) was selected and the concentration of PAN in the dope was 1wt%.
Compared with the nano tube, the nano ball of the invention has higher surface area of 124.7m 2 The higher surface area provides more active sites for the catalytic reaction, thereby increasing the catalytic activity. At the same time, the nanotubes may vary in length, diameter and morphology, the nanospheres exhibit uniform morphology and size distribution, their uniformity ensures stable performance in a variety of applications, and the spherical morphology of the nanospheres makes it easier for them to enter the surface region, making reactant molecules or gases more accessible. This accessibility increases the efficiency of the catalytic reaction and, by increasing the availability of active sites. Furthermore, nanotubes are prone to bending or collapsing under certain conditions, while nanospheres generally have higher mechanical stability, their robustness enables their use in harsh reaction environments and provides durability in a variety of applications. Molybdenum carbide/carbon (Mo 2 C/C) the compound nanospheres have high sphericity, uniform size and good dispersibility.
There are also some differences between nanospheres and them in application. The nanospheres can be used as catalysts for hydrogen generation reactions, fuel cells, electrochemical reactions, chemical syntheses, and the like. It can also be used as a reinforcing agent for metal matrix composites, providing better mechanical properties and thermal stability. In addition, the nanospheres can be used for electrochemical energy storage devices such as super capacitors, lithium ion batteries and the like, and provide higher energy storage and rapid charge and discharge characteristics.
The embodiment also provides the molybdenum carbide prepared by the methodCarbon (Mo) 2 C/C) composite nanospheres, which are used in the fields of catalysis, energy storage, coating, sensing and the like. In the catalytic field, this particular structure of spheres provides a high surface area, which provides more active sites for the catalytic reaction. The electrochemical test result shows that the molybdenum carbide/carbon nanospheres show excellent electrocatalytic hydrogen evolution performance when the current density is 10mA/cm -2 When in an acidic system, the molybdenum carbide/carbon nanosphere catalyst has an overpotential of 110mV/s and exhibits excellent stability. In addition, the spherical molybdenum carbide nano particles can be used as electrode materials of energy storage devices such as lithium ion batteries, supercapacitors and the like. Their high surface area promotes efficient electrochemical reactions and enhances energy storage properties. In applications in the field of coating materials, spherical molybdenum carbide particles can be used as a coating or additive to improve the properties of the material. They can improve wear resistance, hardness and high temperature stability after being incorporated into a coating or composite.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (4)
1. The method for preparing the molybdenum carbide/carbon composite nanospheres based on the electrostatic spinning technology is characterized by comprising the following steps of:
s1, adding ammonium molybdate into dimethylformamide, stirring for 2 hours, then adding polyacrylonitrile, and stirring for 6 hours to obtain spinning solution;
s2, filling the spinning solution obtained in the step S1 into a 10mL syringe for electrostatic spinning to obtain a precursor nanosphere Mo@PAN;
the electrostatic spinning method comprises the following steps: connecting a stainless steel flat-mouth needle with the inner diameter of 1.40mm and the outer diameter of 1.80mm to a positive electrode, placing tinfoil on a receiving plate, connecting the receiving plate to a negative electrode, wherein the distance between the two plates is 9cm, the voltage is 16kV high voltage, and the speed of a propeller is 2mm/h;
s3, placing the precursor nanospheres Mo@PAN obtained in the step S2 in a tube furnace, and performing heat treatment in a nitrogen atmosphere to obtain molybdenum carbide/carbon composite nanospheres; the heat treatment procedure is as follows: heating from room temperature to 800 ℃ at a heating rate of 1 ℃/min, preserving heat for 2 hours, naturally cooling to room temperature, and stopping introducing nitrogen when the temperature is reduced to 100 ℃.
2. The method for preparing the molybdenum carbide/carbon composite nanospheres based on the electrospinning technology according to claim 1, wherein the dosage ratio of the ammonium molybdate, the dimethylformamide and the polyacrylonitrile in S1 is 0.07656g:10mL:0.0957g.
3. The method for preparing the molybdenum carbide/carbon composite nanospheres based on the electrospinning technology according to claim 1, wherein the average particle size of the molybdenum carbide/carbon composite nanospheres in S3 is 160nm.
4. Use of a molybdenum carbide/carbon composite nanosphere prepared according to the method of any one of claims 1-3, wherein the molybdenum carbide/carbon composite nanosphere is used for catalysis, energy storage or sensing.
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