CN110655066A - Method for preparing platinum-graphene-molybdenum sulfide composite material by low-temperature plasma - Google Patents
Method for preparing platinum-graphene-molybdenum sulfide composite material by low-temperature plasma Download PDFInfo
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Abstract
The invention provides a method for preparing a platinum-graphene-molybdenum sulfide composite material by using low-temperature plasma, which comprises the steps of mixing 24.09mmol/L potassium chloroplatinate, molybdenum sulfide and graphene oxide solution with the same concentration according to the volume ratio of 1:5:5 to obtain a mixed solution; performing ultrasonic treatment on the mixed solution for 20-40min to obtain a dispersion solution; centrifuging the dispersion, and freeze-drying the separated precipitate; and carrying out low-temperature plasma discharge on the powder under a hydrogen atmosphere to obtain the platinum-graphene-molybdenum sulfide compound. Compared with the prior art, the method is simpler, has low requirement on conditions, is suitable for large-scale production, and can improve the benefit and reduce the cost.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a method for preparing a platinum-graphene-molybdenum sulfide composite material by using low-temperature plasma.
Background
Graphene has many excellent physicochemical properties such as high conductivity, high specific surface area, and high specific strength, and thus is widely used as an electrode material for fuel cell catalysts, adsorbents, and supercapacitors. The molybdenum sulfide can effectively regulate the graphene structure and has an important effect on improving the performance of the material, for example, when the nitrogen-doped graphene is used as an electrode material of a super capacitor, the specific capacity of the electrode material is related to the nitrogen doping capacity and the type of nitrogen doping, namely graphitized nitrogen can effectively reduce the charge transfer resistance under high current density, and pyridine nitrogen and pyrrole nitrogen can provide higher specific capacitance. The nitrogen-doped graphene is used as a catalyst for the oxygen reduction reaction of the fuel cell, the active site of the nitrogen-doped graphene is a carbon atom adjacent to pyridine nitrogen, and the nitrogen-doped graphene has Lewis alkalinity and can effectively adsorb oxygen molecules in the initial stage of the oxygen reduction reaction. However, the methods for synthesizing nitrogen-doped graphene up to now mainly include hydrothermal synthesis methods, vapor deposition methods, radiation synthesis methods, arc discharge methods, and the like, but such methods are relatively harsh in synthesis conditions, and are not conducive to mass production, and at the same time, the type of nitrogen doping is not convenient to regulate.
To date, noble metal Pt-based catalysts have been considered as the most effective catalysts for electrocatalytic hydrogen production, and have been widely coated on the surface of electrodes for hydrogen production reactions. However, the expensive price of the noble metal Pt seriously hinders its large-scale industrial application. Therefore, the search for a platinum catalyst electrode with low cost and high and durable performance is the key of hydrogen energy utilization. In recent years, the layered molybdenum disulfide (MoS2) two-dimensional crystal material has become a research hotspot in the field of electrocatalytic hydrogen production due to the advantages of high abundance, low price and the like. The literature and theoretical research results show that the electrocatalytic hydrogen production activity of the MoS2 is related to the catalytic active sites at the edges of the two-dimensional layered structure, and the design of the two-dimensional MoS2 thin layer of the nano structure and the maximum exposure of the number of the catalytic active sites at the edges are effective ways for improving the electrocatalytic hydrogen production activity. The two-dimensional MoS2 thin layer is effectively compounded in the graphene material, so that the interface resistance of molybdenum sulfide and a graphene nano structure can be obviously reduced, the electrocatalytic reaction efficiency is obviously improved, on one hand, a plurality of tiny pores can be formed on the surface of a MoS2 nano sheet in the graphene material, and the edge catalytic active sites of the material are effectively increased; on the other hand, the planar structure of the graphene can ensure the efficient transmission of electrons, so that the catalytic product hydrogen is easy to diffuse out of the electrode.
The preparation method of the molybdenum disulfide/carbon nitride composite material mainly comprises an in-situ mixing method, a physical method and the like. The method is mainly prepared by adopting a two-step method or a multi-step method, the synthetic method is relatively complex, the process is complicated, the time consumption is long, the yield is low, and the composite material does not have a certain 3D structure configuration. At the present stage, a controllable and good-repeatability method is necessary to be developed, and the prepared composite material can keep a good nano configuration.
Disclosure of Invention
The invention aims to: aiming at the problems in the prior art, the method for preparing the platinum-graphene-molybdenum sulfide composite material by using the low-temperature plasma is provided, the existing complex method and harsh condition requirements are simplified, the problem that the synthetic process in the prior art cannot regulate and control the nitrogen doping type at low temperature and low pressure is solved, and the large-scale production is facilitated.
The invention aims to be realized by the following technical scheme:
a method for preparing a platinum-graphene-molybdenum sulfide composite material by low-temperature plasma comprises the following steps:
mixing 24.09mmol/L potassium chloroplatinate, molybdenum sulfide and graphene oxide solution according to the volume ratio of 1:5:5 to obtain a mixed solution;
performing ultrasonic treatment on the mixed solution for 20-40min to obtain a dispersion solution;
centrifuging the dispersion, and freeze-drying the separated precipitate;
and carrying out low-temperature plasma discharge on the powder under a hydrogen atmosphere to obtain the platinum-graphene-molybdenum sulfide compound.
Furthermore, when the dispersion is centrifuged, the rotational speed of centrifugation is 5000-12000rbm for 5-30 min.
Further, when freeze-drying the separated precipitated compound, the freeze-drying temperature is from-20 ℃ to-50 ℃.
Further, when the powder is subjected to low-temperature plasma discharge in a hydrogen atmosphere, the temperature of the low-temperature plasma discharge is 30-50 ℃, the pressure is 70Pa, and the discharge power is 100W.
Further, the powder is subjected to low-temperature plasma discharge in a hydrogen atmosphere, the discharge time is 20-30min, and the hydrogen flow is 20-30 sccm.
Further, the mass ratio of the graphene to the molybdenum sulfide is 1: 1.
Compared with the prior art, the method has the advantages that the reaction activity of the plasma is utilized to realize the normal-temperature low-pressure reduction of the platinum precursor and the graphene oxide, the high-temperature high-pressure synthesis process is avoided, the method is simpler than the prior art, the condition requirement is low, and the method is suitable for large-scale production to improve the benefit and reduce the cost. The dispersion of the platinum in the product can be regulated and controlled by regulating parameters such as discharge power, discharge time and the like. The catalyst with different catalytic activities can be prepared by utilizing the graphene and molybdenum sulfide precursors with different mass ratios, wherein the ratio of 1:1 has the best methanol catalytic oxidation performance, the process is simple, the reaction process is easy to control, and the method is suitable for industrial large-scale production.
Drawings
Fig. 1 is a schematic diagram of the preparation of platinum/graphene-molybdenum sulfide.
Figure 2 is a raman plot of example platinumdiplatin graphene-molybdenum sulfide.
FIG. 3 is a transmission electron microscopy characterization of the platinum/graphene-molybdenum sulfide samples of the examples.
Fig. 4 is an XRD pattern of tetraplatin/graphene-molybdenum sulfide of example.
Fig. 5 is an XPS plot of the pentaplatinum/graphene-molybdenum sulfide of the example.
Fig. 6 is a graph of CV of the example hexaplatinum/graphene-molybdenum sulfide in 1M sulfuric acid.
Fig. 7 is a graph of CV of the heptaplatinum/graphene-molybdenum sulfide of the example in 0.5M sulfuric acid and 1M methanol solution.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The invention provides a novel preparation method of a platinum/molybdenum sulfide-graphene composite material, which can be used for preparing a molybdenum sulfide material with a 3D dendritic structure, can be effectively compounded with a carbon nitride substrate to form a specific heterojunction structure, and has a wide application prospect in the field of electrocatalytic hydrogen production.
As shown in fig. 1, the present invention includes a method comprising: mixing 1mL of 24.09mmol/L potassium chloroplatinate, 5mL of molybdenum sulfide with the same concentration and 5mL of graphene oxide solution to obtain a mixed solution; performing ultrasonic treatment on the mixed solution for 20-40min and 30min to obtain a dispersion liquid; the dispersion liquid is centrifugally separated, the rotational speed of the centrifugal separation is 5000-12000rbm, and the time is 5-30 min. Freeze drying the separated precipitated compound at-20 deg.C to-50 deg.C; and then, carrying out low-temperature plasma discharge on the dried powder in a hydrogen atmosphere, wherein the temperature of the low-temperature plasma discharge is 30-50 ℃, the pressure is 70Pa, the discharge power is 100W, the discharge time is 20-30min, and the hydrogen flow is 20-30 sccm. The mass ratio of the graphene to the molybdenum sulfide is 1: 1.
Example 2
The method comprises the following steps: mixing 1mL of 24.09mmol/L potassium chloroplatinate, 5mL of 2mg/mL molybdenum sulfide and 5mL of 2mg/mL graphene oxide solution to obtain a mixed solution; performing ultrasonic treatment on the mixed solution for 30min to obtain a dispersion liquid; the dispersion liquid is centrifugally separated, the rotational speed of the centrifugal separation is 5000-12000rbm, and the time is 5-30 min. Freeze drying the separated precipitated compound at-20 deg.C to-50 deg.C; and then, carrying out low-temperature plasma discharge on the dried powder under a hydrogen atmosphere, wherein the temperature of the low-temperature plasma discharge is 30-50 ℃, the pressure is 70Pa, the discharge power is 100W, the discharge time is 40min, and the hydrogen flow is 25 sccm. The mass ratio of the graphene to the molybdenum sulfide is 1: 1.
In this embodiment, various data also verify that the product obtained by the present invention indeed has a good effect:
as shown in fig. 2, raman characterization proves that graphene and molybdenum sulfide are successfully compounded, and respective characteristic peaks appear at corresponding positions. D, G and 2D characteristic peaks of graphene are obvious.
As shown in fig. 3, the transmission electron micrograph demonstrates that platinum is uniformly dispersed on the graphene-molybdenum sulfide support.
As shown in fig. 4, XRD also proves that graphene and molybdenum sulfide are successfully compounded, and respective characteristic peaks appear at corresponding positions.
As shown in fig. 5, XPS also proves that graphene and molybdenum sulfide are successfully compounded, and respective characteristic peaks appear at corresponding positions. The specific positions are respectively as follows: mo3d 229.5, S2p 164, Pt4d1314.5, Pt4d3331.2, Pt4f771.0, Pt4f574.4eV, Mo3d3231.1.0.
As shown in fig. 6, CV curves were tested in sulfuric acid solution, which proves that platinum-graphene-molybdenum sulfide has better electrochemical activity and active area of 104.3m2 g-1.
As shown in FIG. 7, a CV curve is tested in a methanol sulfate solution, which proves that the platinum/graphene-molybdenum sulfide has better electrocatalytic methanol oxidation activity and the mass current density is 737.8mA m g < -1 >.
Therefore, the invention utilizes the reaction activity of the plasma to realize the normal temperature and normal pressure doping and synthesis of the platinum, the graphene oxide and the molybdenum sulfide, avoids the synthesis process of high temperature and high pressure, is simpler than the prior art, has the advantages of simple process, easy control of the reaction process and the like, and is suitable for industrial large-scale production.
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, it should be noted that any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A method for preparing a platinum-graphene-molybdenum sulfide composite material by using low-temperature plasma is characterized by comprising the following steps:
mixing 24.09mmol/L potassium chloroplatinate, molybdenum sulfide and graphene oxide solution according to the volume ratio of 1:5:5 to obtain a mixed solution;
performing ultrasonic treatment on the mixed solution for 20-40min to obtain a dispersion solution;
centrifuging the dispersion, and freeze-drying the separated precipitate;
and carrying out low-temperature plasma discharge on the powder under a hydrogen atmosphere to obtain the platinum-graphene-molybdenum sulfide compound.
2. The method for preparing platinum-graphene-molybdenum sulfide composite material according to claim 1, wherein the centrifugal separation is performed at a rotation speed of 5000-12000rbm for 5-30 min.
3. The method for preparing the platinum-graphene-molybdenum sulfide composite material according to claim 1, wherein the freeze-drying temperature is from-20 ℃ to-50 ℃ when the separated precipitated compound is freeze-dried.
4. The method for preparing the platinum-graphene-molybdenum sulfide composite material according to claim 1, wherein when the powder is subjected to low-temperature plasma discharge in a hydrogen atmosphere, the temperature of the low-temperature plasma discharge is 30-50 ℃, the pressure is 70Pa, and the discharge power is 100W.
5. The method for preparing the platinum-graphene-molybdenum sulfide composite material through low-temperature plasma according to claim 4, wherein the powder is subjected to low-temperature plasma discharge in a hydrogen atmosphere, the discharge time is 30-50min, and the hydrogen flow is 20-30 sccm.
6. The method for preparing the platinum-graphene-molybdenum sulfide composite material through low-temperature plasma according to claim 1, wherein the mass ratio of graphene to molybdenum sulfide is 1: 1.
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Cited By (3)
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| CN111268732A (en) * | 2020-03-09 | 2020-06-12 | 常熟理工学院 | Method for preparing molybdenum disulfide graphene aerogel by using low-temperature plasma and product thereof |
| CN111933958A (en) * | 2020-07-28 | 2020-11-13 | 航天科工智慧产业发展有限公司 | Catalyst for anode of methanol fuel cell and preparation method thereof |
| CN114369848A (en) * | 2022-02-11 | 2022-04-19 | 苏州阳池科技有限公司 | Preparation and application of heteroatom-doped molybdenum disulfide nanocomposite |
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Application publication date: 20200107 |