CN109622044B - Efficient hydrogen evolution catalyst material, preparation method and application - Google Patents
Efficient hydrogen evolution catalyst material, preparation method and application Download PDFInfo
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- CN109622044B CN109622044B CN201811557659.1A CN201811557659A CN109622044B CN 109622044 B CN109622044 B CN 109622044B CN 201811557659 A CN201811557659 A CN 201811557659A CN 109622044 B CN109622044 B CN 109622044B
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Abstract
The invention relates to a preparation method of a high-efficiency hydrogen evolution catalyst material, which comprises the following steps: 1) preparation of palladium ammonium complex: adding palladium chloride and ethylenediamine into deionized water for ultrasonic treatment; 2) dispersing ammonium tetrathiomolybdate and urea in N, N-dimethylformamide to form a homogeneous solution; transferring the palladium-ammonium complex into the solution, carrying out ultrasonic treatment, adding hydrazine hydrate, and continuing ultrasonic treatment; 3) adding the obtained solution into a reaction kettle and reacting for 4 hours at the temperature of 160-; 4) and after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining the obtained sample at 400 ℃ for 2h in a hydrogen environment to obtain the material. The high-efficiency hydrogen evolution catalyst material can obviously improve the Hydrogen Evolution (HER) performance of the catalyst.
Description
Technical Field
The invention belongs to the technical field of inorganic nano material chemistry and electrochemistry, and particularly relates to a high-efficiency hydrogen evolution catalyst material, a preparation method and application thereof in improving the hydrogen evolution performance of a catalyst.
Background
Since the 21 st century, energy and environmental problems have been highlighted, and hydrogen is considered as a clean energy carrier without environmental problems. In actual life, hydrogen can be used as an environment-friendly fuel cell, liquid hydrogen can be used as a high-energy fuel for launching rockets and spacecrafts, and the liquid hydrogen can be used for smelting metals and preparing high-purity silicon and the like industrially. The challenge in commercializing this technology is how to achieve minimization of power consumption and cost, which requires low-cost and durable electrocatalysts for efficient Hydrogen Evolution Reactions (HER).
In recent years, two-dimensional transition metal oxide and sulfide lamellar structures, particularly molybdenum oxide (MoO)3) And molybdenum disulfide (MoS)2) And the like are deeply concerned by researchers due to excellent HER catalytic performance and low cost. Meanwhile, the research on the participation of noble metals in catalysis is endless. For example, Huang et al (LB Huang, LZHao, Y Zhang, et al. adv. Energy Mater. 2018, 1800734) utilize in situ decomposition adsorption and calcination in a sulfur vapor environment by passing MoO through a solid phase catalyst3Nanodots converted into vertically oriented ultra-small layer MoS2To realize the high-efficiency hydrogen evolution reaction, the obtained hydrogen evolution catalyst is 10 mA cm-2The overpotential was 126 mV. However, the conductivity is low, the cycling stability is weak, and if the hydrogen evolution performance is further improved, the combination with other active materials brings new opportunities. Qi et al (K Qi, SS Yu, QY Wang, et al. journal of materials Chemistry A, 2016, 4, 4025) by applying a composition to a defect-rich MoS2Assembling Pd nanosheets on the base surface of the nanosheets, and modifying MoS by using the Pb nanosheets2Strives to obtain hydrogen evolution performance similar to Pt/C.
The noble metal such as Pb, Au, Pt and the like has extremely high electrochemical catalytic activity. Sun et al (XL Sun, DGLi, Y Ding, et al.J. Am. chem. Soc, 2014, 136, 5745-. Guo et al (SJGuo, X Zhuang, W L Zhu, et al.J. Am. chem. Soc, 2014, 136, 15026-15033) prepared 0.75 and 1.1 nm nanoshells of Ag/Cu by co-reducing palladium acetylacetonate and copper acetylacetonate with nano noble metals (Ag and Au) and CuPb37Pd63And Au/Cu40Pd60To obtain oxygen reduction performance superior to Pt/C. However, when noble metal nanoparticles are used as catalysts, the size of the noble metal nanoparticles is generally 1-4 nm, so that the noble metal nanoparticles can show ideal activity, and thus the material synthesis conditions are severe and are not easy to control. In addition, the cost of the noble metal is high, and how to efficiently utilize the noble metal is an important challenge. Therefore, the Pd nano-particles and the MoO can be prepared under the conditions of mild conditions and simple synthetic method3The composite catalyst utilizes the synergistic effect of the composite catalyst to improve the hydrogen evolution performance of the catalyst, so that the size requirement on Pb nano particles is reduced, and a better catalytic effect is achieved.
Disclosure of Invention
The invention aims to open up a new way and provide a high-efficiency hydrogen evolution catalyst material, a preparation method and application thereof in improving the hydrogen evolution performance of the catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-efficiency hydrogen evolution catalyst material specifically comprises the following steps:
1) adding palladium chloride and ethylenediamine into deionized water, and performing ultrasonic treatment for 10-30 min to obtain a palladium-ammonium complex;
2) dispersing ammonium tetrathiomolybdate and urea in N, N-dimethylformamide to form a homogeneous solution, adding a palladium-ammonium complex, performing ultrasonic treatment for 40-70 min, adding hydrazine hydrate, and continuing ultrasonic treatment for 30-40 min;
3) after the ultrasonic treatment is finished, performing hydrothermal reaction on the product obtained in the step 2) in a reaction kettle at 160-240 ℃ for 6-10 h;
4) after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining for 1.5-3 h at the temperature of 380-420 ℃ in a hydrogen atmosphere to obtain the hydrogen evolution catalyst.
Specifically, in step 1), 180. mu.l of palladium chloride was added per 22mg of ammonium tetrathiomolybdate. The palladium chloride and ethylenediamine are mainly used for forming the palladium ammonium complex, the ethylenediamine is relatively excessive, and the molar ratio of the two is suitably 0.05-0.07: 1.
specifically, in the step 2), the mass ratio of ammonium tetrathiomolybdate to urea is 1: 1-1.5; urea is an organic compound consisting of carbon, nitrogen, oxygen and hydrogen and having the molecular formula H2NCONH2(ii) a Also known as urea, carbamide. Preferably, 0.05 to 0.2ml of hydrazine hydrate is added per 22mg of ammonium tetrathiomolybdate. Too much or too little hydrazine hydrate can affect the internal structure of the nano material product. N, N-dimethylformamide is used as a dispersing solvent for ammonium tetrathiomolybdate and urea so as to be uniformly dispersed. Generally, 30 to 40ml of N, N-dimethylformamide per 22mg of ammonium tetrathiomolybdate is preferably added.
In the reaction in step 3), the reaction temperature is preferably 200 ℃ and the reaction time is preferably 10 hours.
In the step 4), centrifugal separation can be selected for solid-liquid separation, the centrifugal rotation speed is 9000-10000 rpm, and the centrifugal time is 5-10 min.
The invention provides the high-efficiency hydrogen evolution catalyst material prepared by the method.
The invention also provides application of the high-efficiency hydrogen evolution catalyst material in improving the hydrogen evolution performance of the catalyst.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention provides a new way for preparing a high-efficiency hydrogen evolution catalyst material. Compared with methods such as a chemical vapor deposition method, a template method and the like, the method provided by the invention obtains a target product by simple hydrothermal and calcination;
2) the invention has simple preparation process, small environmental pollution and easy batch preparation. Meanwhile, the high-efficiency hydrogen evolution catalyst material obtained by the invention has excellent electrochemical performance;
3) the invention adopts ammonium tetrathiomolybdate as a raw material, and the ammonium tetrathiomolybdate can be directly synthesized at high temperature. Meanwhile, the size problem of noble metal participating in catalytic reaction is solved, and the possibility for developing other catalysts is provided.
Drawings
FIG. 1 is a TEM image of the high efficiency hydrogen evolution catalyst material prepared in example 1;
FIG. 2 is an X-ray photoelectron spectrum of the high efficiency hydrogen evolution catalyst material prepared in example 1;
FIG. 3 is an X-ray diffraction pattern of the high efficiency hydrogen evolution catalyst material prepared in example 1;
FIG. 4 is a polarization curve (a) and corresponding Tafel slope (b) of an electrochemical test of the high efficiency hydrogen evolution catalyst material prepared in example 1;
FIG. 5 is a polarization curve (a) and corresponding Tafel slopes (b) of electrochemical tests of the high efficiency hydrogen evolution catalyst materials prepared in example 1 (200. mu.l palladium chloride), 2 (100. mu.l palladium chloride) and 3 (300. mu.l palladium chloride);
FIG. 6 shows the polarization curve (a) and the corresponding Tafel slope (b) of the electrochemical test of the high efficiency hydrogen evolution catalyst material prepared in example 1 (calcination at 400 ℃ for 2 h), 4 (calcination at 300 ℃ for 2 h), and 5 (calcination at 500 ℃ for 2 h).
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited thereto.
In the examples described below, ammonium tetrathiomolybdate (analytically pure) was obtained from Sigma Aldrich trade, Inc., urea (analytically pure) was obtained from the research and development center for fine chemical engineering, Guangdong province, and other compounds were obtained as commonly commercially available products.
Example 1
A preparation method of a high-efficiency hydrogen evolution catalyst material specifically comprises the following steps:
1) preparation of palladium ammonium complex: adding 200 mu l (0.056 mmol) of palladium chloride and 63 mu l (0.943 mol) of ethylenediamine into 10 ml of deionized water for ultrasonic treatment for 15min to obtain a palladium-ammonium complex;
2) dispersing 22mg of ammonium tetrathiomolybdate and 22mg of urea in 35ml of N, N-dimethylformamide to form a homogeneous solution; transferring the palladium-ammonium complex into the solution, carrying out ultrasonic treatment for 50min, then adding 100 mu l of hydrazine hydrate, and continuing ultrasonic treatment for 35 min;
3) after the ultrasonic treatment is finished, adding the obtained solution into a reaction kettle, and carrying out hydrothermal reaction for 10 hours at 200 ℃;
4) and after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining for 2 hours at 400 ℃ in a hydrogen atmosphere to obtain the high-efficiency hydrogen evolution catalyst material.
Comparative example 1
MoO (MoO)3A method of making nanoplatelets comprising the steps of:
1) dispersing 22mg of ammonium tetrathiomolybdate and 22mg of urea in 35ml of N, N-dimethylformamide to form a homogeneous solution, carrying out ultrasonic treatment for 50min, then adding 100 mu l of hydrazine hydrate, and continuing ultrasonic treatment for 35 min;
2) adding the obtained solution into a reaction kettle, and reacting for 10 hours at 200 ℃;
3) and after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining for 2 hours at 400 ℃ in a hydrogen atmosphere to obtain the catalyst material.
A Transmission Electron Microscope (TEM) image of the target product high-efficiency hydrogen evolution catalyst material obtained in example 1 is shown in FIG. 1, and an X-ray photoelectron spectroscopy (XPS) image is shown in FIG. 2. The X-ray diffraction pattern (XRD) is shown in FIG. 3. The polarization curve for the electrochemical hydrogen evolution reaction is shown in a in fig. 4, and the corresponding tafel slope is shown in b in fig. 4. The polarization curves of the reaction and the corresponding tafel slopes for different amounts of palladium chloride are shown in a and b of fig. 5. The corresponding polarization curves of the reaction and the corresponding tafel slopes at different calcination temperatures are shown in a and b of fig. 6.
The above characterization results show that: the hydrogen evolution catalyst is prepared by adopting ammonium tetrathiomolybdate as a raw material and calcining the ammonium tetrathiomolybdate under the condition of solvothermal reaction in a hydrogen atmosphere and is assembled by a series of nanosheets (see figure 1). X-ray diffraction (XRD) pattern (FIG. 3) demonstrates the interaction of elemental Pd and MoO3Compared with the XRD standard card, MoO exists in the XRD pattern of the sample3And diffraction peaks of elemental Pd.
The prepared product material MoO3The performance of the three-electrode system is tested by loading Pd on a glassy carbon electrode, and the electrolyte is 0.5M H2SO4. For HER, the catalyst was at 10 mA cm-2A low overpotential of 71mV was exhibited. Compared with other structures of nano materials, the small overpotential makes the material of the invention more advantageous in practical application.
MoO3The nanosheet electrochemical test pattern is shown in fig. 4 (a), and can be seen as follows: compared with example 1, the overpotential is significantly greater than that of example 1 and the cathode current density is significantly smaller. This can result in: after palladium chloride is added, the electrochemical hydrogen evolution performance is obviously improved.
As a control, the invention also measured the MoO prepared in control 13Nanosheet, 10 mA cm-2Exhibit a high overpotential of 300mV, showing poor HER activity. To further understand the MoO of the present invention3Hydrogen evolution performance of the/Pd material, the application investigated the tafel plot (fig. 4 b) for various catalysts. Among them, the MoO of the invention3Pd nano-scaleThe slope of the Tafel plot for the material was 42.8mV/dec, which is close to the currently accepted commercial Pt/C catalyst, whereas the MoO prepared in comparative example 13The nano-sheet product has a higher Tafel slope of 79.2 mV/dec. The small tafel slope of such nanomaterials is advantageous for practical applications. As it will result in a faster increase in HER rate with increasing overpotential.
Examples 2 to 3
A preparation method of a high-efficiency hydrogen evolution catalyst material comprises the following steps:
1) preparation of palladium ammonium complex: adding 63 mul of palladium chloride and ethylenediamine into 10 ml of deionized water for ultrasonic treatment for 15min, wherein the difference is that the amount of the palladium chloride is 100 mul and the amount of the palladium chloride is 300 mul;
2) dispersing 22mg of ammonium tetrathiomolybdate and 22mg of urea in 35ml of N, N-dimethylformamide to form a homogeneous solution; transferring the palladium-ammonium complex into the solution, carrying out ultrasonic treatment for 50min, then adding 100 mu l of hydrazine hydrate, and continuing ultrasonic treatment for 35 min;
3) after the ultrasonic treatment is finished, adding the obtained solution into a reaction kettle, and carrying out hydrothermal reaction for 10 hours at 200 ℃;
4) and after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining for 2 hours at 400 ℃ in a hydrogen atmosphere to obtain the high-efficiency hydrogen evolution catalyst material.
The polarization curves of the hydrogen evolution catalysts prepared in examples 2 to 3 and the corresponding tafel slopes are shown in a and b of fig. 5, as is evident from the following figures: 200 μ l of palladium chloride showed the best performance, both in HER performance and in tafel slope.
Examples 4 to 5
A preparation method of a high-efficiency hydrogen evolution catalyst nano material comprises the following steps:
1) preparation of palladium ammonium complex: adding 200 mu L of palladium chloride and 63 mu L of ethylenediamine into 10 ml of deionized water for ultrasonic treatment for 15 min;
2) dispersing 22mg of ammonium tetrathiomolybdate and 22mg of urea in 35ml of N, N-dimethylformamide to form a homogeneous solution; transferring the palladium-ammonium complex into the solution, carrying out ultrasonic treatment for 50min, then adding 100 mu l of hydrazine hydrate, and continuing ultrasonic treatment for 35 min;
3) after the ultrasonic treatment is finished, adding the obtained solution into a reaction kettle, and carrying out hydrothermal reaction for 10 hours at 200 ℃;
4) after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining for 2 hours in a hydrogen atmosphere to obtain the high-efficiency hydrogen evolution catalyst material, wherein the difference is that the calcining temperature is 300 ℃ and 500 ℃ respectively.
The polarization curves of the hydrogen evolution catalysts prepared in examples 4 to 5 and the corresponding tafel slopes are shown in a and b of fig. 6, as can be clearly seen: the best performance was shown at 400 ℃ calcination temperature, both in HER performance and in tafel slope.
Claims (5)
1. A preparation method of a high-efficiency hydrogen evolution catalyst material is characterized by comprising the following steps:
1) adding palladium chloride and ethylenediamine into deionized water, and performing ultrasonic treatment for 10-30 min to obtain a palladium-ammonium complex;
2) dispersing ammonium tetrathiomolybdate and urea in N, N-dimethylformamide to form a homogeneous solution, adding a palladium-ammonium complex, performing ultrasonic treatment for 40-70 min, adding hydrazine hydrate, and continuing ultrasonic treatment for 30-40 min;
3) after the ultrasonic treatment is finished, carrying out hydrothermal reaction on the product obtained in the step 2) at the temperature of 160-240 ℃ for 6-10 h;
4) after the reaction is finished, naturally cooling to room temperature, carrying out solid-liquid separation, washing and drying the precipitate, and calcining at the temperature of 380-420 ℃ for 1.5-3 h in a hydrogen atmosphere to obtain the hydrogen evolution catalyst;
in the step 1), 180-;
in the step 2), the mass ratio of ammonium tetrathiomolybdate to urea is 1: 1-1.5; 0.05-0.2 ml of hydrazine hydrate is added per 22mg of ammonium tetrathiomolybdate.
2. The method for preparing the high efficiency hydrogen evolution catalyst material according to claim 1, wherein the reaction temperature in the step 3) is 200 ℃ and the reaction time is 10 h.
3. The method for preparing the high efficiency hydrogen evolution catalyst material as claimed in claim 1, wherein in the step 4), the solid-liquid separation is performed by centrifugal separation, the centrifugal rotation speed is 9000-10000 rpm, and the centrifugal time is 5-10 min.
4. The high-efficiency hydrogen evolution catalyst material prepared by the method of any one of claims 1 to 3.
5. The use of the high efficiency hydrogen evolution catalyst material of claim 4 to improve the hydrogen evolution performance of the catalyst.
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