CN114853020B - Nano molybdenum carbide material and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a preparation method of a nano molybdenum carbide material, which comprises the following steps of firstly preparing MoO 3 Uniformly mixing the powder with inorganic salt to obtain a Mo source precursor; then placing the solid carbon source in a low temperature area of the reaction device, and placing the solid carbon source in a high temperature area of the reaction device; introducing carrier gas, heating the reaction device, and performing heat preservation reaction; and cooling, and taking out the product obtained in the high temperature area to obtain the nano molybdenum carbide material. The invention utilizes MoO 3 The gas-phase molybdenum source intermediate generated by the inorganic salt reacts with the solid-phase carbon template, so that the rate of generating the molybdenum carbide material can be effectively accelerated, the reaction time is obviously shortened, the problems of carbon deposition on the surface of the molybdenum carbide material caused by using the gas-phase carbon source can be effectively avoided, the controllable adjustment of the morphology of the molybdenum carbide base material is realized, and a new thought can be provided for the preparation of the high-performance molybdenum carbide base material; the preparation method is simple, the reaction condition is mild, the raw materials are simple and easy to obtain, the byproducts are few, and the method is suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of functional materials and synthesis thereof, and particularly relates to a nano molybdenum carbide material and a preparation method and application thereof.
Background
Molybdenum carbide belongs to a transition metal carbide ceramic material, has high mechanical strength and high corrosion resistance, and is mainly used as an abrasive in the field of machining at first. With further intensive research, it was found that molybdenum carbide also has a very high catalytic activity. Until today, molybdenum carbide materials have been widely studied in various catalytic subdivision areas.
The hydrogen energy is a clean fuel and is a new energy which is developed under the national 'double carbon' target. In the mainstream hydrogen production technology, the water electrolysis hydrogen production is widely focused on the characteristics of high efficiency and environmental protection. The main cost source of the electrolyzed water is electric energy, and the catalyst can effectively reduce hydrogen evolution overpotential in the electrolysis process, thereby achieving the purpose of saving the electric energy. Pt/C has been widely used as a commercial hydrogen evolution catalyst in the electrolytic aquaculture industry, but its price is high, which increases the cost of hydrogen production by water electrolysis in an intangible way. Research shows that the molybdenum carbide has an electronic structure similar to Pt and has high electrocatalytic hydrogen evolution activity.
The synthesis process of the molybdenum carbide material often needs high temperature above 900 ℃, and the prepared molybdenum carbide material is easy to sinter into blocks and can not provide enough active site catalytic hydrogen evolution processes. In addition, in some synthesis methods based on gaseous carbon sources, a molybdenum carbide-based catalyst is disclosed in patent CN111841593a, gaseous carbon (CH 4 ) The use of (2) can easily lead the surface of the molybdenum carbide material to be carbon deposited, and influence the catalytic activity of the molybdenum carbide material. Further explores and optimizes the molybdenum carbide base material and the preparation process thereof, and has important research and application significance.
Disclosure of Invention
Aiming at the problems and defects existing in the prior art, the invention provides a nano molybdenum carbide material and a preparation method thereof, which effectively solve the problems of easy sintering, surface carbon deposition and the like existing in the existing molybdenum carbide-based catalyst and show excellent electrocatalytic hydrogen evolution performance; the preparation method is simple, the reaction condition is mild, and the purity of the obtained product is high, so that the method is suitable for popularization and application.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the nano molybdenum carbide material comprises the following steps:
1) MoO is carried out 3 Uniformly mixing the powder with an inorganic salt mill to obtain a Mo source precursor;
2) The Mo source precursor and the solid-phase carbon source are separately arranged in a reaction device containing a high-temperature area and a low-temperature area; placing a Mo source precursor in a low temperature region, and placing a solid-phase carbon source in a high temperature region;
3) Introducing carrier gas, heating the mixture to a temperature of 800-1100 ℃ in a high temperature area and 400-800 ℃ in a low temperature area in an atmosphere furnace; and cooling, and taking out the product at the high temperature area to obtain the nano molybdenum carbide material.
Preferably, the temperature of the high temperature region is 800-900 ℃.
In the above scheme, the inorganic salt comprises NaCl, KCl, caCl 2 One or more of KBr and NaBr.
In the above scheme, the solid-phase carbon source comprises one or more of carbon nanotubes, graphene, carbon fibers, activated carbon powder and the like.
In the scheme, the diameter and the outer diameter of the carbon nano tube are 20-200 nm, and the inner diameter is 2-50 nm; the diameter of the graphene sheet is 0.5-5 mu m, and the thickness is 0.8-2 nm; the diameter of the carbon fiber is 0.1-10 mu m; the particle size of the activated carbon powder is 5-50 mu m.
In the above scheme, the inorganic salt and MoO 3 The mass ratio of the powder is 1 (0.25-10); solid phase carbon source and MoO 3 The mass ratio of the powder is 1 (10-200).
In the above scheme, the reaction device can be an atmosphere furnace or the like.
In the above scheme, the carrier gas in step 3) is one or more of argon, nitrogen, helium, hydrogen and the like; the flow rate is 20-200 sccm.
In the scheme, the heating rate of the high temperature area in the step 3) is 1-200 ℃/min.
Preferably, the heating rate of the high temperature area is 15-50 ℃/min.
In the scheme, the temperature rising rate of the low temperature area in the step 3) is 1-200 ℃/min.
Preferably, the temperature rising rate of the low temperature area is 10-50 ℃/min.
In the scheme, the temperature of the low-temperature area in the step 3) is controlled to be 450-800 ℃; the temperature is lower than the temperature of the contemporaneous high temperature zone.
Preferably, the temperature of the low temperature zone is 500-600 ℃.
In the scheme, the heat preservation reaction time is 5 min-10 h.
Preferably, the heat preservation time is 0.5-2 h.
According to the scheme, the nano molybdenum carbide material is prepared by taking a solid-phase carbon source as a carbon source and a template, and is obtained by converting elemental carbon in the solid-phase carbon source: the single carbon in the carbon template is converted into molybdenum carbide nanocrystals (the grain diameter is 80-150 nm) through self-propagating reaction, and the molybdenum carbide nanocrystals are further stacked, and the macroscopic morphology is related to the solid-phase carbon source template; the controllable adjustment of the macro morphology of the molybdenum carbide based material can be realized by adopting solid carbon source templates with different morphologies, the problems of carbon deposition on the surface of the molybdenum carbide based material and the like caused by using a gas-phase carbon source can be effectively solved, the high-efficiency preparation of the single-phase molybdenum carbide material (or the high-purity molybdenum carbide material and the carbon composite material) can be synchronously realized, and a new thought can be provided for the preparation of the high-performance molybdenum carbide based material.
The nano molybdenum carbide material prepared according to the scheme is applied to the field of electrocatalysis, and can be used as a hydrogen evolution catalyst to be coated on the surface of an electrode to prepare an electrocatalysis hydrogen evolution electrode.
Compared with the prior art, the invention has the beneficial effects that:
1) Adopts solid-phase carbon source as carbon template and utilizes MoO simultaneously 3 And NaCl-forming gas-phase intermediate (MoO) 2 Cl 2 ) As a molybdenum source, the rapid conversion from the carbon simple substance in the carbon template to the molybdenum carbide can be realized, and the reaction time is obviously shortened; meanwhile, the prepared molybdenum carbide material has no impurity and does not need further purification; the problems of easy sintering and agglomeration of the nano molybdenum carbide material at high temperature and the like can be effectively solved, and the problems of carbon deposition on the surface of the molybdenum carbide material and the like caused by using a gas-phase carbon source are effectively avoided; meanwhile, the controllable adjustment of the shape of the molybdenum carbide base material can be realized by adopting simple means of solid carbon source templates with different shapes;
2) The preparation method is simple and convenient, the used raw materials are simple and easy to obtain, the byproducts are few, the purity of the product is high (single-phase molybdenum carbide), and the method is suitable for large-scale production;
3) The nano molybdenum carbide material prepared by the method has good electrocatalytic hydrogen evolution performance, is superior to most molybdenum carbide electrocatalysts, and has very wide application prospect in the field of water electrolysis hydrogen production.
Drawings
FIG. 1 is a schematic diagram of a preparation flow of a nano molybdenum carbide material according to the present invention;
FIG. 2 is an XRD pattern of the nano molybdenum carbide material prepared in examples 1 to 4 of the present invention;
FIG. 3 is a scanning electron microscope image of the nano molybdenum carbide material prepared in example 1 of the present invention;
FIG. 4 is a scanning electron microscope image of the nano molybdenum carbide material prepared in example 2 of the present invention;
FIG. 5 is a transmission electron microscope image and an element distribution diagram of the nano molybdenum carbide material prepared in example 2 of the present invention;
FIG. 6 is a scanning electron microscope image of the nano molybdenum carbide material prepared in example 3 of the present invention;
FIG. 7 is a scanning electron microscope image of the nano molybdenum carbide material prepared in example 4 of the present invention;
FIG. 8 is a polarization diagram of electrocatalytic hydrogen evolution reaction of nano molybdenum carbide materials prepared in examples 1, 3 and 4 in 1M KOH solution;
FIG. 9 is a Tafel slope diagram of the nano molybdenum carbide material prepared in examples 1, 3 and 4 in 1M KOH solution;
FIG. 10 is an XRD pattern of the material prepared in comparative example 1 of the present invention;
fig. 11 is an XRD pattern of the molybdenum carbide material prepared in comparative example 2 of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation process of the nano molybdenum carbide material is schematically shown in fig. 1, and specifically comprises the following steps:
1) Grinding and uniformly mixing 700mg of molybdenum trioxide and 300mg of sodium chloride to obtain a Mo source precursor;
2) Placing a Mo source precursor and 10mg whisker carbon nanotubes (with the outer diameter of 80-150 nm and the inner diameter of 5-10 nm) in a crucible shown in figure 1 respectively, then placing the crucible in a tube furnace, placing the Mo source precursor in a non-heating zone positioned in the upwind direction (the position is calibrated by a thermometer, when the temperature of a central heating zone is 900 ℃, the temperature is just 500-600 ℃), and placing the whisker carbon nanotubes in a central heating zone in the downwind direction;
3) After argon with the flow of 80sccm is introduced, the temperature of the tube furnace is raised to 900 ℃ in a high temperature area at the heating rate of 15 ℃/min, and the heat preservation time is 1h; and naturally cooling to room temperature, and taking out the product of the central heating zone of the tube furnace after the reaction to obtain a final product.
The XRD pattern of the product obtained in this example is shown in FIG. 2; the results show that the obtained product is pure-phase molybdenum carbide.
FIG. 3 is a scanning electron microscope image of the product obtained in this example, and the result shows that, unlike the smoother surface of the original whisker carbon nanotube, the prepared molybdenum carbide whisker carbon nanotube is formed by stacking small nanocrystals, the surface is rough, the diameter (outer diameter) of the whisker carbon nanotube is 80-200 nm, and the size of the nanocrystals is 80-150 nm.
5mg of the product obtained in the embodiment is weighed and dispersed in 1mL of isopropanol, 20 mu LNafion solution is dripped into the isopropanol, the solution is dripped onto carbon cloth after ultrasonic treatment for 30min, the carbon cloth is dried to prepare a hydrogen evolution electrode, the hydrogen evolution electrode is placed into 1M KOH for testing, and the measured polarization curve of the electrocatalytic hydrogen evolution reaction and a Tafel slope chart are respectively shown in fig. 8 and 9. The results show that: when the current density is 10mAcm -2 When the hydrogen evolution reaction has an overpotential of only 99mV, the Tafel slope of only 56mV dec -1 Proved to have good electrocatalytic hydrogen evolution performance.
Example 2
A nano molybdenum carbide material was prepared in the same manner as in example 1, except that the temperature in the high temperature region in example 1 was changed to 800℃and the temperature in the low temperature region was maintained.
The XRD pattern in FIG. 2 shows that the product prepared in this example is a composite material of graphitic carbon and molybdenum carbide, and the scanning electron microscope in FIG. 4 shows that the product almost maintains the original morphology of whisker carbon nanotubes.
The TEM images (a-c) in fig. 5 are the reaction states of three whisker carbon nanotubes with complete morphology observed at different positions in the product (after 1h of incubation) obtained in this example, and it can be seen that the originally smooth surface of the whisker carbon nanotube becomes rough gradually along the axial direction. FIG. 5d is a graph of the elemental distribution of the product of FIG. 5b, showing that molybdenum carbide is present at only the rough end of the carbon nanotubes of the whisker; indicating that the formation of molybdenum carbide exists in the reaction process from one end of the self-propagating reaction to the other end along the axial direction of the whisker carbon nano tube.
Example 3
A nano molybdenum carbide material was prepared in substantially the same manner as in example 1, except that 10mg of whisker carbon nanotubes in example 1 were replaced with 16mg of carbon fiber (diameter 4 to 8 μm).
The XRD pattern shown in FIG. 2 shows that the product obtained in this example is a composite phase of graphitic carbon and molybdenum carbide; the scanning electron microscope image in fig. 6 shows that the carbon fiber is wrapped by a layer of porous molybdenum carbide, the grain size is 80-200 nm, and the hole size is 100-200 nm.
The polarization curve and Tafel slope of the electrocatalytic hydrogen evolution reaction of the product obtained according to the present invention were measured as described in example 1 and are shown in FIGS. 8 and 9, respectively. The results show that: when the current density is 10mAcm -2 When the hydrogen evolution reaction has an overpotential of only 115mV, the Tafel slope of only 62mV dec -1 。
Example 4
A nano molybdenum carbide material is prepared in the same way as in example 1, except that 10mg of whisker carbon nanotube solid phase carbon source in example 1 is changed into 10mg of graphene (sheet diameter 1-5 μm).
The XRD pattern in figure 2 shows that the product obtained in this example is pure phase molybdenum carbide; the scanning electron microscope image in fig. 7 shows that the molybdenum carbide nanocrystals grown along the graphene are stacked into a sheet shape, and the size of the nanocrystals is 80-150 nm.
The polarization curve and Tafel slope of the electrocatalytic hydrogen evolution reaction of the product obtained according to the present invention were measured as described in example 1 and are shown in FIGS. 8 and 9, respectively. The results show that: when the current density is 10mAcm -2 When the hydrogen evolution reaction overpotential is only 150mV, the Tafel slope is only 63mV dec -1 。
Comparative example 1
A molybdenum carbide material was prepared in substantially the same manner as in example 1, except that the temperature in the high temperature region was controlled to 700 c and the temperature in the low temperature region was maintained.
The XRD patterns of the products obtained in this comparative example are shown in FIG. 10, and the results indicate that the material prepared at this temperature is MoO 2 The molybdenum carbide material cannot be prepared.
Comparative example 2
The preparation method of the molybdenum carbide material is almost the same as that of the embodiment 1, except that the whisker carbon nanotube solid phase carbon source and the Mo source precursor in the embodiment 1 are mixed and then placed in a high temperature area together.
Fig. 11 is an XRD pattern of the product obtained in this comparative example, which shows that: the obtained product medium phase is free of Mo 2 C contains NaCl, mo, moO 2 And (5) waiting for mixed phases.
The above examples are presented for clarity of illustration only and are not limiting of the embodiments. Other variations and modifications of the above description will be apparent to those of ordinary skill in the art, and it is not necessary or exhaustive of all embodiments, and thus all obvious variations or modifications that come within the scope of the invention are desired to be protected.
Claims (5)
1. The preparation method of the nano molybdenum carbide material is characterized by comprising the following steps of:
1) MoO is carried out 3 The powder and the inorganic salt are uniformly mixed,obtaining a Mo source precursor;
2) The Mo source precursor and the solid-phase carbon source are separately arranged in a reaction device, wherein the Mo source precursor is arranged in a low-temperature area, and the solid-phase carbon source is arranged in a high-temperature area; the Mo source precursor is arranged in an upwind direction, and the solid carbon source is arranged in a downwind direction;
3) Introducing carrier gas, heating to 800-1100 ℃ in a high temperature area, and carrying out heat preservation reaction; cooling, and taking out the product at the high temperature area to obtain the nano molybdenum carbide material;
the temperature of the low temperature area is controlled to be 400-800 ℃; the temperature is lower than the temperature of the synchronous high temperature zone;
the inorganic salt is NaCl, KCl, caCl 2 One or more of KBr and NaBr; inorganic salt and MoO 3 The mass ratio of the powder is 1 (0.25-10);
the solid-phase carbon source is one or more of carbon nano tube, graphene, carbon fiber and active carbon powder; solid phase carbon source and MoO 3 The mass ratio of the powder is 1 (10-200).
2. The method according to claim 1, wherein the carrier gas is one or more of argon, nitrogen, helium, and hydrogen; the flow rate is 20-200 sccm.
3. The preparation method of claim 1, wherein the incubation time is 5 min-10 h.
4. The nano molybdenum carbide material prepared by the preparation method according to any one of claims 1 to 3, which is characterized in that the nano molybdenum carbide material is formed by stacking molybdenum carbide nanocrystals.
5. Use of the nano molybdenum carbide material according to claim 4 in the field of electrocatalytic technology.
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| CN110878418A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Self-supporting molybdenum carbide and preparation method and application thereof |
| CN110575840A (en) * | 2019-09-10 | 2019-12-17 | 太原理工大学 | Preparation method of two-dimensional molybdenum carbide/graphene nanosheet composite material |
| CN113832446A (en) * | 2020-06-24 | 2021-12-24 | Asm Ip私人控股有限公司 | Vapor deposition of films comprising molybdenum |
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