CN113235126B - Molybdenum disulfide nanoflower loaded zinc oxide quantum dot and application thereof in synthesizing ammonia electrocatalyst - Google Patents
Molybdenum disulfide nanoflower loaded zinc oxide quantum dot and application thereof in synthesizing ammonia electrocatalyst Download PDFInfo
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Abstract
The invention provides a preparation method of molybdenum disulfide nanoflower loaded zinc oxide quantum dots, which comprises the steps of adding ammonium molybdate and thiourea into a certain amount of deionized water, uniformly stirring to obtain a clear solution, then adding a proper amount of hydrochloric acid solution, and carrying out hydrothermal reaction to obtain molybdenum disulfide nanoflowers; adding the molybdenum disulfide nanoflower into absolute ethyl alcohol containing a certain amount of zinc acetate for ice bath, stirring while ice bath, dropwise adding an absolute ethyl alcohol solution dissolved with a certain amount of strong base into the solution while stirring, standing after dropwise adding is finished, preserving heat at the temperature of 80-100 ℃, washing, drying, introducing argon gas for ignition, and obtaining an ignition sample, namely the molybdenum disulfide nanoflower loaded zinc oxide quantum dot. The prepared synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide increases catalytic active sites by utilizing the incomplete coordination property of atoms on the surface of the black zinc oxide, so that the synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide is applied to the room-temperature electrocatalytic synthesis of ammonia.
Description
Technical Field
The invention belongs to the field of preparation of an electro-catalytic synthetic ammonia material, and particularly relates to a method for growing white zinc oxide on the surface of a flaky molybdenum disulfide nanoflower, and changing the white zinc oxide into black zinc oxide through high-temperature annealing treatment, namely, molybdenum disulfide nanoflower loaded zinc oxide quantum dots.
Background
Mo and S elements in the azotase play an important role in nitrogen fixation, molybdenum disulfide is an important member of transition metal disulfide, has many properties of semiconductors, has a typical hexagonal structure, a unique lamellar structure, a special valence band and good physicochemical properties, so that the molybdenum disulfide is an electrode material with great potential, has attracted various interests in the field of electrocatalysis in recent years, and is widely applied to the fields of electrochemical synthesis of ammonia and the like.
However, recent studies have found that MoS2The band gap is wider than 1.73 (ev), the inherent conductivity is poor, and the promotion of the catalytic activity is severely limited. To improve this deficiency, zinc oxide with better properties was introduced as a composite material. The zinc oxide has wide band gap and high exciton binding energy, and has very low resistance on the C axis due to high crystallinity, thereby being beneficial to the conduction of current carriers. The introduction of zinc oxide is beneficial to the current carrier on the molybdenum disulfide and promotes electronsSeparation of the hole pairs, while being N-type semiconductors due to their band matching, enables the formation of a heterojunction with molybdenum disulfide. Research shows that the construction of the heterojunction can promote charge transfer among the components, enhance conductivity and improve MoS2An efficient way of catalytic activity. Compared with a pure molybdenum disulfide material, the heterojunction formed by growing black zinc oxide particles on the surface of molybdenum disulfide is remarkably improved in the efficiency of synthesizing ammonia through electrocatalysis, and the method shows that the heterojunction material has great potential in the field of synthesizing ammonia through electrochemistry and has very important significance.
Disclosure of Invention
The invention provides a composite material with heterojunction, which is prepared by growing zinc oxide particles on the surface of a flaky molybdenum disulfide nanoflower under a liquid phase condition by using flaky molybdenum disulfide as a substrate, and changing white zinc oxide into black after high-temperature annealing treatment. Compared with the pure molybdenum disulfide, the prepared catalyst has the advantages that the synthetic ammonia yield and the Faraday efficiency are greatly improved. The invention discloses a preparation method of molybdenum disulfide nanoflower-loaded zinc oxide quantum dots, in particular to a preparation method of a synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide, aiming at changing white zinc oxide into black zinc oxide by utilizing a high-temperature flame-fading technology, and improving the electrocatalytic activity through electrocatalytic performance test. The catalyst is a composite structure constructed by flaky molybdenum disulfide nanoflowers and black zinc oxide particles. According to the invention, the flaky molybdenum disulfide nanoflower is used as a substrate, zinc oxide grows in situ, and then white zinc oxide is changed into black, so that the high-activity composite catalyst is prepared.
The above object of the present invention is achieved by the following means:
firstly preparing flaky molybdenum disulfide nanoflowers, then adding molybdenum disulfide into a liquid phase, growing zinc oxide particles on the surface of the molybdenum disulfide nanoflowers, and then placing a sample in a tubular furnace for high-temperature annealing treatment to prepare the black zinc oxide which grows on the surface of the molybdenum disulfide to synthesize the ammonia electrocatalyst.
The obtained black zinc oxide grows on the surface of molybdenum disulfide to synthesize the ammonia electrocatalyst, and is characterized in that: the zinc oxide is black in color, and a heterojunction exists between the two materials.
The invention relates to a preparation method of a synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide, which comprises the following steps:
(1) preparing molybdenum disulfide nanoflowers: adding ammonium molybdate and thiourea into a certain amount of deionized water, uniformly stirring to obtain a clear solution, then adding a proper amount of hydrochloric acid solution, and carrying out hydrothermal reaction to obtain molybdenum disulfide nanoflowers; the mass ratio of ammonium molybdate to thiourea is 1: 1-1: 5. The concentration of the hydrochloric acid solution is 2-4 mol/L. The temperature of the hydrothermal reaction is 150-200 ℃, and the reaction time is 10-24 h.
(2) The preparation of the white zinc oxide growing in the molybdenum disulfide nanoflower: adding the molybdenum disulfide nanoflower into absolute ethyl alcohol containing a certain amount of zinc acetate for ice bath, stirring while ice bath, dropwise adding an absolute ethyl alcohol solution dissolved with a certain amount of strong base into the solution while stirring, standing after dropwise adding is finished, preserving heat for 1 hour at the temperature of 80-100 ℃, washing the obtained sample with absolute ethyl alcohol for multiple times, and centrifugally drying to obtain white zinc oxide growing in the molybdenum disulfide nanoflower; the mass ratio of the molybdenum disulfide nanoflower to the zinc acetate is 3: 1-30. The strong base is KOH, and the mass concentration of the absolute ethyl alcohol solution of the strong base is 0.001-0.07 g/ml.
(3) Preparing the molybdenum disulfide nanoflower loaded zinc oxide quantum dots: and (3) putting the white zinc oxide growing in the molybdenum disulfide nanoflower into a tubular furnace, introducing argon gas for ignition, and obtaining an ignited sample, namely the molybdenum disulfide nanoflower loaded zinc oxide quantum dots. The burning temperature is 700-1000 ℃, the heating rate is 2-3 ℃/min, and the heat preservation time is 2-3 h.
The preparation method of the synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide comprises the following steps: the 10mg catalyst and 1mL nafion aqueous solution are ultrasonically homogenized, 20 mu L of mixed solution is dripped on hydrophobic carbon paper to be used as a working electrode, a Pt electrode is a counter electrode, an Ag/AgCl electrode is a reference electrode, and a three-electrode reaction device is adopted to carry out electrochemical reaction to synthesize ammonia gas.
The invention provides a preparation method capable of greatly improving the activity of electrocatalytic synthesis of ammonia, compared with the synthesis of molybdenum disulfideAmmonia yield 3.067 μ gh-1mgcat-1The Faraday efficiency is 3.34 percent, and the synthetic ammonia yield of the prepared novel catalyst reaches 14.544 mu gh-1mgcat-1The Faraday efficiency reaches 15.1 percent and is almost improved by 5 times. The preparation method is simple, zinc oxide grows on the surface of the molybdenum disulfide by an in-situ growth method, white zinc oxide is changed into black zinc oxide by high-temperature annealing, the electron transmission rate is increased, and the catalytic activity is improved. The prepared synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide increases catalytic active sites by utilizing the incomplete coordination property of atoms on the surface of the black zinc oxide, and has multifunctional reaction sites by utilizing a heterostructure, so that the synthetic ammonia electrocatalyst with black zinc oxide growing on the surface of molybdenum disulfide is applied to the room-temperature electrocatalytic synthesis of ammonia, and the field of material preparation of electrocatalytic synthesis of ammonia is widened.
Drawings
Fig. 1 is an SEM image of the flaky molybdenum disulfide nanoflower of example 1.
Fig. 2 is an SEM image of the surface of the molybdenum disulfide nanoflower loaded with zinc oxide quantum dots of example 1.
Fig. 3 is a performance test chart of the catalyst of example 1, in which the molybdenum disulfide nanoflowers load zinc oxide quantum dots.
Fig. 4 is an SEM picture of white zinc oxide grown on the surface of molybdenum disulfide in example 2.
Figure 5 is the XRD chart of the catalyst with molybdenum disulfide nanoflowers loaded with zinc oxide quantum dots of example 2.
Fig. 6 is a performance test chart of the catalyst on the surface of the molybdenum disulfide nanoflower loaded with the zinc oxide quantum dots in example 2.
Figure 7 is a picture of the performance test of the molybdenum disulfide nanoflower catalyst in example 3.
FIG. 8 is a graph comparing the improvement in the performance of catalysts grown on the surface of molybdenum disulfide for white zinc oxide of example 3.
Detailed Description
Example 1
Dissolving 1.24g ammonium molybdate in 50mL deionized water to form a transparent solution, adding 2.28g thiourea, stirring to dissolve, adding 1mL 3mol/L hydrochloric acid to dissolveStirring the solution for half an hour and performing ultrasonic dispersion uniformly, finally adding the obtained liquid into a 50ml reaction kettle containing a polytetrafluoroethylene lining, performing hydrothermal reaction for 24 hours at 200 ℃, centrifuging, washing and drying in a vacuum drying oven. The sample is molybdenum disulfide nanoflower (see attached figure 1). Adding 0.3g of sample molybdenum disulfide nanoflower into 50ml of absolute ethyl alcohol containing 2.36g of zinc acetate, carrying out ice bath for 1 hour while stirring, then dropwise adding 35ml of absolute ethyl alcohol solution dissolved with 1g of KOH into the obtained solution while stirring for two hours, standing for one hour, and finally carrying out heat preservation for one hour at 80 ℃. And (4) centrifugal vacuum drying, wherein the sample is the synthetic ammonia electrocatalyst with white zinc oxide growing on the surface of molybdenum disulfide. Putting the dried solid into a tubular furnace, introducing argon gas, and igniting, wherein the ignition temperature is 750 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 2 h. The burned sample is the molybdenum disulfide nanoflower loaded zinc oxide quantum dots, and black zinc oxide can be seen to grow on the surface of the molybdenum disulfide from the sample (see attached figure 2). Test of synthetic Ammonia yield and Faraday efficiency Performance (see FIG. 3) As can be seen in FIG. 3, the combined efficiency is best at-0.1V, where the Faraday efficiency for electrochemically synthesizing ammonia is 6.29% and the ammonia yield is 5.19. mu.g.h-1·mg-1 cat. The preparation method of the electro-catalyst for synthesizing ammonia by using the molybdenum disulfide nanoflower loaded with the zinc oxide quantum dot catalyst, the white zinc oxide catalyst growing on the surface of the molybdenum disulfide and the molybdenum disulfide nanoflower catalyst comprises the following steps: 10mg of catalyst, 950 mu L of absolute ethyl alcohol and 50 mu L of nafion aqueous solution are ultrasonically and uniformly mixed, 20 mu L of mixed solution is dripped on hydrophobic carbon paper to be used as a working electrode, a Pt electrode is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and a three-electrode reaction device is adopted to carry out electrochemical reaction to synthesize ammonia gas.
Example 2
Dissolving 1.24g of ammonium molybdate in 30mL of deionized water to form a transparent solution, adding 2.28g of thiourea into the solution, stirring for dissolving, adding 1mL of 3mol/L hydrochloric acid solution into the solution, stirring for half an hour and ultrasonically dispersing uniformly, finally adding the obtained liquid into a 50mL reaction kettle containing a polytetrafluoroethylene lining, and performing hydrothermal reaction at 160 DEG CIt should be washed by centrifugation for 18h and dried in a vacuum drying oven. The sample is molybdenum disulfide nanoflower. Adding 0.3g of sample molybdenum disulfide nanoflower into 50ml of absolute ethyl alcohol containing 1g of zinc acetate, carrying out ice bath for 1 hour, stirring while carrying out ice bath, then dropwise adding 50ml of absolute ethyl alcohol solution dissolved with 0.1g of KOH into the obtained solution, stirring while carrying out dropwise addition for two hours, standing for one hour, finally carrying out heat preservation at 80 ℃ for one hour, centrifuging, and drying in vacuum, thus obtaining a sample, namely the synthetic ammonia electrocatalyst with white zinc oxide growing on the surface of molybdenum disulfide (shown in figure 4). Putting the dried solid into a tubular furnace, introducing argon gas, and igniting at 900 ℃, wherein the heating rate is 3 ℃/min, and the heat preservation time is 2 h. The sample after firing is the molybdenum disulfide nanoflower loaded zinc oxide quantum dot, namely the molybdenum disulfide nanoflower loaded zinc oxide quantum dot synthetic ammonia electrocatalyst, an XRD analysis chart (shown in figure 5) is adopted, and the synthetic ammonia yield and Faraday efficiency performance are tested (shown in figure 6), and as can be seen from figure 6, the comprehensive efficiency is the best at-0.1V, the Faraday efficiency of the electrochemical synthetic ammonia is 15.1%, and the ammonia yield is 10.51 mug.h-1·mg-1 cat. The preparation method of the synthetic ammonia electrocatalyst with the molybdenum disulfide nanoflowers loaded with the zinc oxide quantum dots comprises the following steps of: 10mg of catalyst, 950 mu L of absolute ethyl alcohol and 50 mu L of nafion aqueous solution are ultrasonically and uniformly mixed, 20 mu L of mixed solution is dripped on hydrophobic carbon paper to be used as a working electrode, a Pt electrode is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and a three-electrode reaction device is adopted to carry out electrochemical reaction to synthesize ammonia gas.
Example 3
1.24g of ammonium molybdate is added into 40mL of deionized water to be dissolved to form a transparent solution, 2.28g of thiourea is added into the solution, the solution is stirred and dissolved, 10mL of 3mol/L hydrochloric acid solution is added into the solution, the solution is stirred for half an hour and is uniformly dispersed by ultrasonic, finally, the obtained liquid is added into a 50mL reaction kettle with a polytetrafluoroethylene lining, hydrothermal reaction is carried out for 20h at 170 ℃, centrifugal washing is carried out, and drying is carried out in a vacuum drying oven. The sample is molybdenum disulfide nanoflower, the synthetic ammonia yield and Faraday efficiency (see attached figure 7) can be seen from figure 7 that the comprehensive efficiency is best at-0.1V, and the Faraday efficiency of the electrochemical synthesis of ammonia at the momentThe first efficiency was 3.34% and the ammonia yield was 3.06. mu.g.h-1·mg-1 cat. Adding 0.3g of sample molybdenum disulfide nanoflower into 50ml of absolute ethyl alcohol containing 1g of zinc acetate, carrying out ice bath for 1 hour, stirring while carrying out ice bath, then dropwise adding 40ml of absolute ethyl alcohol solution dissolved with 0.5g of KOH into the obtained solution, stirring for two hours while carrying out dropwise addition, standing for one hour, finally carrying out heat preservation for one hour at 80 ℃, centrifuging, and carrying out vacuum drying to obtain a sample, namely the synthetic ammonia electrocatalyst with white zinc oxide growing on the surface of molybdenum disulfide. The performance of the catalyst is improved by growing white zinc oxide on the surface of molybdenum disulfide (see attached figure 8). It can be seen from fig. 8 that the white zinc oxide is grown on the molybdenum disulfide catalyst, and the catalytic performance of the white zinc oxide is obviously improved compared with that of the single molybdenum disulfide. Putting the dried solid into a tubular furnace, introducing argon gas, and igniting, wherein the ignition temperature is 800 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 2 h. The burned sample is the molybdenum disulfide nanoflower loaded zinc oxide quantum dots. The method for testing the performance of the synthetic ammonia by using the zinc oxide quantum dots loaded on the molybdenum disulfide nanoflowers comprises the following steps: 10mg of catalyst, 950 mu L of absolute ethyl alcohol and 50 mu L of nafion aqueous solution are ultrasonically and uniformly mixed, 20 mu L of mixed solution is dripped on hydrophobic carbon paper to be used as a working electrode, a Pt electrode is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and a three-electrode reaction device is adopted to carry out electrochemical reaction to synthesize ammonia gas.
Claims (7)
1. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing molybdenum disulfide nanoflowers: adding ammonium molybdate and thiourea into a certain amount of deionized water, uniformly stirring to obtain a clear solution, then adding a proper amount of hydrochloric acid solution, and carrying out hydrothermal reaction to obtain molybdenum disulfide nanoflowers;
(2) the preparation of the white zinc oxide growing in the molybdenum disulfide nanoflower: adding the molybdenum disulfide nanoflower into absolute ethyl alcohol containing a certain amount of zinc acetate for ice bath, stirring while ice bath, dropwise adding an absolute ethyl alcohol solution dissolved with a certain amount of strong base into the solution while stirring, standing after dropwise adding is finished, preserving heat for 1 hour at the temperature of 80-100 ℃, washing the obtained sample with absolute ethyl alcohol for multiple times, and centrifugally drying to obtain white zinc oxide growing in the molybdenum disulfide nanoflower;
(3) preparing the molybdenum disulfide nanoflower loaded zinc oxide quantum dots: and (3) putting the white zinc oxide growing in the molybdenum disulfide nanoflower into a tubular furnace, introducing argon gas for ignition, and obtaining an ignited sample, namely the molybdenum disulfide nanoflower loaded zinc oxide quantum dots.
2. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot as claimed in claim 1, which is characterized in that: the mass ratio of ammonium molybdate to thiourea in the step (1) is 1: 1-1: 5.
3. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot as claimed in claim 1, which is characterized in that: the concentration of the hydrochloric acid solution in the step (1) is 2-4 mol/L.
4. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot as claimed in claim 1, which is characterized in that: the temperature of the hydrothermal reaction in the step (1) is 150-200 ℃, and the reaction time is 10-24 h.
5. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot as claimed in claim 1, which is characterized in that: in the step (2), the mass ratio of the molybdenum disulfide nanoflowers to the zinc acetate is 3: 1-30.
6. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot as claimed in claim 1, which is characterized in that: in the step (2), the strong base is KOH, and the mass concentration of the absolute ethyl alcohol solution of the strong base is 0.001-0.07 g/ml.
7. The preparation method of the molybdenum disulfide nanoflower-loaded zinc oxide quantum dot as claimed in claim 1, which is characterized in that: in the step (3), the burning temperature is 700-1000 ℃, the heating rate is 2-3 ℃/min, and the heat preservation time is 2-3 h.
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