CN111822000A - Pt nanoparticle loaded molybdenum dioxide/nickel hydroxide nanosheet array structure material and preparation method and application thereof - Google Patents

Pt nanoparticle loaded molybdenum dioxide/nickel hydroxide nanosheet array structure material and preparation method and application thereof Download PDF

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CN111822000A
CN111822000A CN202010531878.3A CN202010531878A CN111822000A CN 111822000 A CN111822000 A CN 111822000A CN 202010531878 A CN202010531878 A CN 202010531878A CN 111822000 A CN111822000 A CN 111822000A
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吴正翠
张吴正知
高峰
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Anhui Normal University
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Abstract

The invention discloses a Pt nanoparticle loaded molybdenum dioxide/nickel hydroxide nanosheet array structure material and a preparation method and application thereof.A nickel salt, a molybdenum salt, a reducing agent and a platinum source aqueous solution are dissolved in ammonia water, methanol is added, the mixture is uniformly stirred, the platinum source aqueous solution is continuously added and uniformly mixed, the mixed solution is transferred to a reaction kettle, foamed nickel is obliquely placed in the solution for solvothermal reaction, the reaction is cooled to room temperature after the reaction is finished, and a product is washed and dried to prepare a product; MoO in the product2Is metallic in that itPresent as an electron donor in the material, greatly reducing Ni (OH)2With foamed nickel substrate and Ni (OH)2A Schottky barrier between the Pt nano particles and the Schottky barrier accelerates electron transfer in the reaction process; meanwhile, the high-valence Mo ions can well stabilize active Ni on the interface2+Ions are used for further improving the catalytic stability of the material; the catalyst is used as a cathode catalyst material for hydrogen evolution or total moisture decomposition reaction, and has the advantages of high catalytic activity, excellent stability and simple preparation process.

Description

Pt nanoparticle loaded molybdenum dioxide/nickel hydroxide nanosheet array structure material and preparation method and application thereof
Technical Field
The invention belongs to the field of nano material preparation methods and electrocatalysis application, and particularly relates to a Pt nano particle loaded MoO2/Ni(OH)2A nano-sheet array structure material, a preparation method and application thereof.
Background
Hydrogen energy is a pollution-free, sustainable, clean energy source. The hydrogen production by electrolyzing water in alkaline environment is one of the important sources of hydrogen. It is well known that Pt is an excellent hydrogen evolution reaction catalyst. However, the water dissociation efficiency of the Pt surface in an alkaline environment is low and the cost is expensive, which makes it difficult to apply it to industrial production applications on a large scale. Because the performance of the non-noble metal electrocatalyst reported at present is generally lower than that of a Pt-based catalyst, the method for reducing the Pt dosage and improving the overall water dissociation efficiency of the material is a feasible method.
The transition metal hydroxide can effectively break HO-H bonds, and the material with good hydrogen evolution catalytic activity can be obtained by combining the HO-H bonds with platinum. Nevertheless, electron transfer between the material components is greatly hindered due to the weak conductivity of the hydroxide itself and the presence of schottky barriers at the interfaces of the metal hydroxide and the substrate and Pt and metal hydroxide. MoO2The metal semiconductor has a twisted rutile structure, and has obvious metal performance and high conductivity. The Schottky barrier existing in the material can be greatly weakened by introducing the composite material into a Pt/hydroxide composite structure, and the interface charge transmission rate is accelerated. Meanwhile, the expensive Mo ions can also stabilize the active Ni on the interface2+Ions. Thus, Pt and MoO are mixed2And Ni (OH)2The combination of the three substances is expected to design a hydrogen evolution electrocatalyst with low cost, high activity and high stability.
In the prior art, the synthesis method of the Pt nanoparticle supported metal hydroxide catalyst is mostly a complicated two-step reaction, it is difficult to uniformly deposit Pt nanoparticles on a previously prepared support, and the negative effect of the schottky barrier on the material performance is generally not eliminated or reduced.
Disclosure of Invention
The invention aims to provide a Pt nano particle loaded MoO2/Ni(OH)2A nano-sheet array structure material and a preparation method thereof are disclosed, wherein a low-temperature chemical liquid phase method is utilized to directly synthesize Pt nano-particles loaded MoO on a conductive foam nickel substrate in one step2/Ni(OH)2The nano-sheet array structure material has simple synthesis process and low cost.
Another purpose of the invention is to provide a Pt nanoparticle loaded MoO2/Ni(OH)2The nanosheet array structure material is applied as an electrocatalyst for Hydrogen Evolution Reaction (HER) or total moisture decomposition reaction.
The invention provides a Pt nano particle loaded MoO2/Ni(OH)2The preparation method of the nano-sheet array structure material comprises the following steps: dissolving nickel salt, molybdenum salt, a reducing agent and a platinum source aqueous solution in ammonia water, adding methanol, stirring uniformly, continuing to add the platinum source aqueous solution, mixing uniformly, transferring the mixed solution to a reaction kettle, obliquely placing foamed nickel in the solution, carrying out a solvothermal reaction, cooling to room temperature after the reaction is finished, washing and drying a product to obtain the Pt nano-particle loaded MoO2/Ni(OH)2A nanosheet array structure material.
Further, the nickel salt is nickel nitrate hexahydrate; the molybdenum salt is ammonium heptamolybdate tetrahydrate; the reducing agent is sodium borohydride; the platinum source water solution is chloroplatinic acid water solution.
The volume ratio of the ammonia water to the anhydrous methanol is 3: 1.
The ratio of the amounts of the nickel salt, the molybdenum salt, the reducing agent and the platinum source is 0.175-1.225: 0.175:1: 0.00375-0.0075, and preferably 0.7:0.175:1: 0.006.
The concentration of the reducing agent in the mixed solution was 0.05M.
The concentration of the platinum source aqueous solution was 0.03M.
The volume ratio of the platinum source water solution added in the first time to the platinum source water solution added in the second time is 1: 5-9, and the preferred volume ratio is 1: 7.
The solvothermal reaction condition is that the reaction is carried out for 8 hours at 150 ℃.
The foam Nickel (NF) needs to be cleaned before use, and the specific cleaning steps are as follows: soaking in 6M hydrochloric acid for 15min to remove oxide film on the surface, and cleaning with deionized water and anhydrous ethanol for 3-5 times; when in use, the foam nickel is cut into the size of 2 multiplied by 3 cm.
The washing is 3-5 times by using deionized water and absolute ethyl alcohol respectively.
The drying is carried out in a vacuum drying oven at 60 ℃ for 6-12 h.
The invention also provides Pt nano particle loaded MoO prepared by the preparation method2/Ni(OH)2A nanosheet array structure material. The Pt nano-particle loaded MoO2/Ni(OH)2The shape of the nano-sheet array structure material is an array structure formed by crossing nano-sheets with the transverse dimension of 90-120 nm; in MoO2/Ni(OH)2Pt nano particles with the average size of 3.1nm are uniformly distributed on the nano-sheets.
The invention also provides a Pt nanoparticle loaded MoO2/Ni(OH)2The nano-sheet array structure material is applied as a Hydrogen Evolution Reaction (HER) or total moisture decomposition cathode catalyst material.
The Pt nano-particle loaded MoO2/Ni(OH)2When the nano-sheet array structure material is applied as a hydrogen evolution reaction electrocatalyst, the specific method comprises the following steps: MoO loaded Pt nanoparticles prepared on foamed nickel2/Ni(OH)2The nanosheet array structure material is cut into a size of 0.5 multiplied by 0.5cm to be used as a working electrode, 1M KOH solution is used as electrolyte, and a CHI 760E electrochemical workstation is used for testing. Carbon rods and Ag/AgCl electrodes were used as counter and reference electrodes, respectively. Linear Sweep Voltammetry (LSV) at 5.0mV · s-1The polarization curve is obtained at a scanning rate of 90% with ohmic compensation; stability was obtained by measuring the current density time curve at constant voltage. By scanning at different rates (120, 160, 200, 240, 280, 320 and 360 mV. multidot.s) in the absence of significant Faraday regions-1) Measurement of double layer capacitance (C) by Cyclic Voltammetry (CV)dl) Evaluating an electrochemically active area (ECSA); electrochemical Impedance (EIS) in the frequency range of 100kHz to 0.1HzThe test was carried out at an overpotential of 65 mV. MoO on foamed nickel with commercial Pt/C, respectively2/Ni(OH)2The nanosheet array material was used as a working electrode and HER performance was measured for comparison.
The Pt nano-particle loaded MoO2/Ni(OH)2When the nano-sheet array structure material is used as a cathode catalyst material for total hydrolysis reaction, the specific method comprises the following steps: MoO loaded Pt nanoparticles prepared on foamed nickel2/Ni(OH)2Nano-sheet array structure material and self-made NiFe2O4The NiFe LDH nanosheet array structure material is cut into 0.5 multiplied by 0.5cm in size and is assembled in a double-electrode electrolytic cell as a cathode and an anode respectively, and the full-water decomposition performance is tested through an LSV polarization curve compensated by 90% iR. As a comparison, the noble metal RuO supported on nickel foam in a two-electrode electrolyzer was investigated2LSV polarization curves as anode and Pt/C as cathode.
In the present invention, MoO2Mo in (1)4+Mo produced by ion and surface oxidation6+The ions can well stabilize the active Ni on the interface2+Ions. At the same time, MoO2The unique metallic property has high conductivity, greatly reduces Ni (OH)2With foamed nickel substrate and Ni (OH)2Schottky barrier with Pt nanoparticles, thereby accelerating the charge transfer rate. Ni (OH)2The surface hydrophilic hydroxyl groups adsorb water molecules through hydrogen bonds, and then gain electrons from the electrodes, so that the adsorbed water molecules are split into-OH and-H. The adsorbed hydrogen atoms are then recombined on the surface of the Pt nanoparticles to form hydrogen gas, while OH-Ion exchange from MoO2/Ni(OH)2And (5) desorbing the surface of the nanosheet. Thus, Pt nanoparticles, MoO2And Ni (OH)2The three cooperate with each other to promote HER catalytic efficiency. Wherein, MoO2The nano-sheet exists as an electron donor, reduces Schottky barrier existing in the material, accelerates charge transfer rate, and is Ni (OH)2The nanosheet interface catalyzes a Volmer process of water dissociation, and the surface of the Pt nanoparticle optimizes the adsorption energy of H atoms, so that the H atoms are compounded into hydrogen through a Tafel process.
Compared with the prior art, the utility modelThe invention promotes OH by a one-step solvothermal method and utilizing the alkaline environment provided by ammonia water-Ions and Ni2+Ion Generation of Ni (OH)2Nanosheets. Simultaneously, sodium borohydride reduces the + 6-valent molybdenum in the molybdenum salt to + 4-valent molybdenum to form MoO2And Ni (OH)2Forming a mixed phase nanosheet structure. Then, H2PtCl6Reducing the Pt nano particles into Pt nano particles by sodium borohydride, and uniformly loading the Pt nano particles on the nano sheets of the mixed phase. The Pt nano-particle loaded MoO provided by the invention2/Ni(OH)2The catalyst with the nanosheet array structure has excellent catalytic activity and stability on HER in alkaline electrolyte, is simple in preparation process and environment-friendly, and has a great value on the practical application of hydrogen-producing electro-catalytic electrode materials.
Drawings
FIG. 1 shows MoO loaded on Pt nanoparticles prepared in example 12/Ni(OH)2An X-ray powder diffraction (XRD) pattern of the nanoplatelets;
FIG. 2 shows MoO loaded on Pt nanoparticles prepared in example 12/Ni(OH)2A Raman spectrum of the nanosheet;
FIG. 3 shows MoO loaded on Pt nanoparticles prepared in example 12/Ni(OH)2An energy dispersive X-ray spectroscopy (EDX) profile of the nanoplatelets;
FIG. 4 shows MoO loaded on Pt nanoparticles prepared in example 12/Ni(OH)2A Scanning Electron Microscope (SEM) image of the nanoplatelets;
FIG. 5 shows MoO loaded Pt nanoparticles prepared in example 12/Ni(OH)2A Transmission Electron Microscope (TEM) image of the nanoplatelets;
FIG. 6 shows MoO loaded Pt nanoparticles prepared in example 12/Ni(OH)2High Resolution Transmission Electron Microscopy (HRTEM) images of the nanoplates;
FIG. 7 shows MoO loaded Pt nanoparticles prepared in example 12/Ni(OH)2Scanning electron microscope images and corresponding element distribution images of the nanosheets;
FIG. 8 shows MoO loaded Pt nanoparticles prepared in example 12/Ni(OH)2A graph of nanoplatelet contact angle measurements;
FIG. 9 shows MoO loading of Pt nanoparticles with Pt loadings of 0.84% and 1.25% prepared in example 22/Ni(OH)2An energy dispersive X-ray spectroscopy (EDX) profile of the nanoplatelets;
FIG. 10 shows MoO loaded Pt nanoparticles with 0.84% Pt loading prepared in example 22/Ni(OH)2A Scanning Electron Microscope (SEM) image of the nanoplatelets;
FIG. 11 shows MoO loaded Pt nanoparticles with a Pt loading of 1.25% prepared in example 22/Ni(OH)2A Scanning Electron Microscope (SEM) image of the nanoplatelets;
FIG. 12 shows MoO loaded Pt nanoparticles with 0.84% Pt loading prepared in example 22/Ni(OH)2A Transmission Electron Microscope (TEM) image of the nanoplatelets;
FIG. 13 shows MoO loaded Pt nanoparticles with a Pt loading of 1.25% prepared in example 22/Ni(OH)2A Transmission Electron Microscope (TEM) image of the nanoplatelets;
FIG. 14 shows MoO loading of Pt nanoparticles for different Pt loadings (0.84%, 1.07% and 1.25%) prepared in examples 1 and 22/Ni(OH)2LSV profile of nanoplatelet Hydrogen Evolution Reaction (HER);
FIG. 15 shows MoO loading of Pt nanoparticles in example 32/Ni(OH)2Nanosheet material, MoO2/Ni(OH)2LSV plot of nanoplatelet, Hydrogen Evolution Reaction (HER) of Pt/C;
FIG. 16 shows MoO loaded on Pt nanoparticles of example 32/Ni(OH)2Nanoplatelet, current density time profile of Hydrogen Evolution Reaction (HER) of Pt/C;
FIG. 17 shows MoO loaded on Pt nanoparticles in example 32/Ni(OH)2Nanosheet material, MoO2/Ni(OH)2A capacitance current diagram of the nanosheet material at different sweep rates;
FIG. 18 shows MoO supported on Pt nanoparticles of example 32/Ni(OH)2Nanosheet material, MoO2/Ni(OH)2An impedance plot of the nanosheet material;
FIG. 19 shows example 3Pt nanoparticlesLoaded MoO2/Ni(OH)2Nanoplatelet, mass activity plot of Pt/C;
FIG. 20 shows MoO supported on Pt nanoparticles in example 42/Ni(OH)2Polarization curve of the nanosheet material in a two-electrode system for total water splitting (inset is the polarization curve at high current density).
Detailed Description
The invention is described in detail below with reference to the following examples and the accompanying drawings.
Example 1
Pt nanoparticle loaded MoO2/Ni(OH)2The preparation method of the nanosheet array material comprises the following steps:
soaking foamed nickel with the size of 2 multiplied by 3cm in 6M hydrochloric acid solution for 15min, and respectively cleaning the foamed nickel for 3 times by using deionized water and absolute ethyl alcohol;
accurately measure 30mL of ammonia water, add it to a 50mL clean small beaker, then add 1.4mmol of Ni (NO) separately3)2·6H2O,0.35mmol(NH4)6Mo7O24·4H2O, 0.05mL of 0.03M H2PtCl6Solution and 2mmol NaBH4After stirring for 10min, 10mL of anhydrous methanol was added. After stirring for 5min, 0.35mL of 0.03M H was added2PtCl6Continuously stirring the solution for 1-2min to obtain a uniform solution;
transferring the solution to a stainless steel reaction kettle with 50mL of polytetrafluoroethylene as an inner lining, obliquely placing clean foamed nickel into the solution, sealing and reacting in a drying oven at 150 ℃ for 8 hours, naturally cooling to room temperature after the reaction is finished, respectively cleaning the foamed nickel covering the sample by deionized water and absolute ethyl alcohol for 3 times, then placing the foamed nickel in a vacuum drying oven at 60 ℃ for drying for 10 hours to obtain the Pt nano-particle loaded MoO2/Ni(OH)2A nanosheet material.
The phase of the product obtained in example 1 was characterized by an X-ray powder diffractometer (XRD), and the results are shown in FIG. 1. All diffraction peaks are equal to MoO in JCPDS No.78-1069 card2The diffraction peaks of (a) correspond to each other. Due to Ni (OH)2In the amorphous phaseThe existing Pt has low loading, so that the Ni (OH) is not shown in the figure2And diffraction peaks for Pt.
The crystal lattice vibration mode of the product obtained in example 1 was characterized by raman optical system microscopy, and the results are shown in fig. 2. 219. 263, 321 and 360cm-1The peak of (A) belongs to MoO2Bending vibration of 453cm-1The peak at (A) is attributed to the stretching vibration of Ni-OH. Verify the MoO2And Ni (OH)2Is present.
The product was analyzed using energy dispersive X-ray spectroscopy (EDX) as shown in fig. 3. Indicating that the atomic percentages of Ni, Mo and Pt elements were 5.3:1:0.0345, from which the Pt loading was calculated to be 1.07%.
The sample prepared in example 1 was subjected to morphological analysis using a Scanning Electron Microscope (SEM), as shown in fig. 4. The sample is shown to be in an array structure formed by crossing nano sheets, and the transverse size of the nano sheets is 90-120 nm.
The morphology of the sample was further observed using Transmission Electron Microscopy (TEM), as shown in fig. 5. The sample is shown to be composed of nanosheets supported by Pt nanoparticles, with the average size of the Pt nanoparticles being 3.1 nm.
Fig. 6 is a high-resolution transmission electron microscope (HRTEM) picture. The Pt nano particles show clear lattice stripes, the spacing between crystal faces is 0.228nm, and the Pt nano particles are matched with Pt (111) crystal faces; the interplanar spacing of the lattice fringes exhibited on the nanoplatelets was 0.245nm, corresponding to MoO2Is/are as follows
Figure BDA0002535599980000081
A crystal plane.
FIG. 7 is a scanning electron micrograph of a sample and the corresponding elemental distribution. As can be seen from the figure, four elements of Ni, Mo, O and Pt are uniformly distributed in the sample, wherein the distribution density of the Pt element is obviously lower than that of the Ni, Mo and O, which indicates that the product is MoO loaded by Pt nanoparticles2/Ni(OH)2And (4) nano sheets.
Determination of Pt nanoparticle loaded MoO by contact angle method2/Ni(OH)2Surface wettability of the nanosheets. FIG. 8 shows the dropping of water droplets onto Pt nanoparticles loaded with MoO2/Ni(OH)2Typical water drop profile plot of the instant after nanosheet surface. The contact angle is shown to be 26.9 deg., indicating the hydrophilicity of the product.
Example 2
MoO loaded with Pt nanoparticles2/Ni(OH)2The preparation method of the nanosheet array material comprises the following steps:
soaking foamed nickel with the size of 2 multiplied by 3cm in 6M hydrochloric acid solution for 15min, and respectively cleaning the foamed nickel for 3 times by using deionized water and absolute ethyl alcohol;
accurately measure 30mL of ammonia water, add into a 50mL clean small beaker, add 1.4mmol of Ni (NO)3)2·6H2O,0.35mmol(NH4)6Mo7O24·4H2O, 0.05mL of 0.03M H2PtCl6Solution and 2mmol NaBH4After stirring for 10min, 10mL of anhydrous methanol was added. After stirring for an additional 5min, 0.25mL or 0.45mL of 0.03M H was added2PtCl6Continuously stirring the solution for 1-2min to obtain a uniform solution;
transferring the solution to a stainless steel reaction kettle with 50mL of polytetrafluoroethylene as an inner lining, obliquely placing clean foam nickel into the solution, sealing and reacting in a drying oven at 150 ℃ for 8 hours, naturally cooling to room temperature after the reaction is finished, respectively cleaning the foam nickel covering the sample by deionized water and absolute ethyl alcohol for 3 times, then placing the foam nickel in a vacuum drying oven at 60 ℃ for 10 hours, and respectively obtaining Pt nano-particle loaded MoO with the Pt loading of 0.84% and 1.25%2/Ni(OH)2A nanosheet array material.
The product was analyzed using energy dispersive X-ray spectroscopy (EDX) as shown in fig. 9, where the atomic percentages of the Ni, Mo and Pt elements were 5:1:0.0256 and 5.9:1:0.0435, respectively. Pt loadings of 0.84% and 1.25% were calculated accordingly.
Morphology analysis was performed on the sample prepared in example 2 using a Scanning Electron Microscope (SEM), and fig. 10 and 11 are graphs showing Pt nanoparticle-supported MoO with Pt loading of 0.84% and 1.25%, respectively2/Ni(OH)2The SEM image of (A) shows that the sample is an array structure formed by crossing nano sheets.
Use ofThe morphology analysis of the sample prepared in example 2 was performed by Transmission Electron Microscopy (TEM), and fig. 12 and 13 are the Pt nanoparticle-supported MoO with Pt loading of 0.84% and 1.25%, respectively2/Ni(OH)2The TEM image shows that the samples are all composed of nanosheets loaded with Pt nanoparticles. Where the Pt loading was 0.84%, the average size of the Pt nanoparticles on the nanosheets was 2.4nm (fig. 12). At a Pt loading of 1.25%, the average size of the Pt nanoparticles was 4.1nm, and a portion of the nanoparticles were agglomerated (fig. 13).
Example 3
Pt nanoparticle loaded MoO2/Ni(OH)2Use of a nanoplatelet material as a Hydrogen Evolution Reaction (HER) catalyst.
The specific application method comprises the following steps: the Pt nanoparticles obtained in each example with an area of 0.5X 0.5cm were loaded with MoO2/Ni(OH)2The nanosheet material was used as the working electrode, a carbon rod was used as the counter electrode, an Ag/AgCl electrode was used as the reference electrode, and the test was performed in a 1.0M KOH electrolyte solution using the CHI 760E electrochemical workstation. Linear Sweep Voltammetry (LSV) at 5.0mV · s-1At a scan rate of 90% ohm compensation and polarization curves obtained as Pt/C, MoO, respectively2/Ni(OH)2Nanosheet material (MoO)2/Ni(OH)2Nanoplatelet preparation omitting chloroplatinic acid solution from the raw material relative to the preparation method in example 1) was used as a working electrode for comparative testing.
FIG. 14 is a plot of Pt nanoparticle-loaded MoO with different Pt loadings of 0.84%, 1.07%, and 1.25%2/Ni(OH)2Hydrogen Evolution Reaction (HER) polarization curve of the nanoplatelets. It is shown that Pt loading significantly affects the catalyst HER activity, with the sample with Pt loading of 1.07% being optimal.
The LSV plot of FIG. 15 shows that Pt nanoparticles are MoO loaded2/Ni(OH)2Nanosheet material (Pt)1.07%-MoO2/Ni(OH)2) At 10mA cm-2The overpotential of only 18mV under the current density is far less than that of MoO2/Ni(OH)2The overpotential (122mV) of the nanosheet array material is similar to that required for commercial Pt/C (16 mV). In addition, driveDynamic 500mA cm-2And 1000mA · cm-2The high current density only requires an overpotential of 167mV and 256mV, respectively.
The current density time curve of FIG. 16 shows Pt1.07%-MoO2/Ni(OH)2The nanosheet material has excellent stability under low and high current densities, and the current density is kept above 94% after 11h of test. Whereas commercial Pt/C catalysts supported on nickel foam by a binder tended to fall off at 20mA cm-2The overpotential at the current density of (2) is 26mV, and the current density is only maintained at the initial 72.4% after 11h of testing.
The electrochemically active area of the material was evaluated using double layer capacitance, as shown in fig. 17. Pt1.07%-MoO2/Ni(OH)2The electric double layer capacitance of the nano sheet material is 4.08mF cm-2Is greater than MoO2/Ni(OH)2Electric double layer capacitor (1.47 mF. cm)-2) Indicating that Pt loading increases the electrochemically active area of the material.
The Electrochemical Impedance (EIS) plot of FIG. 18 shows Pt1.07%-MoO2/Ni(OH)2The semicircular diameter of the nano sheet material is small, which shows that the resistance is small, and the Pt nano particle load is beneficial to promoting electron transfer.
The mass activity plot of FIG. 19 shows Pt1.07%-MoO2/Ni(OH)2The nanosheet material had higher activity than commercial Pt/C, where the mass activity was 8.24 mA. mu.g at an overpotential of 70mVPt -121.7 times of commercial Pt/C (commercial Pt/C is only 0.38 mA. mu.g)Pt -1)。
Example 4
Pt nanoparticle loaded MoO2/Ni(OH)2The application of the nanosheet material as a cathode catalyst material for total-moisture decomposition reaction.
The specific application method comprises the following steps: the Pt nanoparticles obtained in example 1 having an area of 0.5X 0.5cm were each loaded with MoO2/Ni(OH)2Nano-sheet array structure material and self-made NiFe2O4the/NiFe LDH nano-sheet array structure material is used as a cathode and an anode to be assembled in an electrolytic bath,the test was performed in a 1.0M KOH electrolyte solution using CHI 760E electrochemical workstation. Linear Sweep Voltammetry (LSV) at 5.0mV · s-1At a scanning rate of 90% ohmic compensation, and in Pt/C and RuO, respectively2The cathode and anode compositions were compared electrically.
NiFe2O4NiFe LDH nano-sheet array structure material according to Zhengcui Wu et al2O4Nanoparticles/NiFe Layered Double-Hydroxide Nanosheet HeterostructureArray for Efficient Overall Water Splitting at Large Current Densities.《ACSApplied Materials&The preparation method is disclosed in Interfaces 2018, volume 10, page 26283-26292.
FIG. 20 shows Pt1.07%-MoO2/Ni(OH)2||NiFe2O4The total water decomposition LSV polarization curve of the NiFe-LDH couple can reach 10mA cm under the voltage of 1.481V-2The current density of (2) is only 1.842V required to drive 500mA cm-2The high current density of (2) shows excellent full water cracking catalytic activity. Comparative Pt/C and RuO2The current density of the electric couple can not reach 400mA cm due to the falling of materials-2The above.
MoO loading on Pt nanoparticles as described above with reference to examples2/Ni(OH)2The detailed description of the nanoplatelet array materials, the methods of preparation and the applications are illustrative and not restrictive, and several examples can be cited within the limits defined, and thus variations and modifications without departing from the general inventive concept are intended to be within the scope of the present invention.

Claims (10)

1. Pt nanoparticle loaded MoO2/Ni(OH)2The preparation method of the nano-sheet array structure material is characterized by comprising the following steps:
dissolving nickel salt, molybdenum salt, reducing agent and platinum source aqueous solution in ammonia water, adding methanol, stirring uniformly, continuing to add platinum source aqueous solution, mixing uniformly, transferring the mixed solution to a reaction kettle, and obliquely placing foamed nickel in the reaction kettleCarrying out solvothermal reaction in the solution, cooling to room temperature after the reaction is finished, washing and drying the product to obtain the Pt nano particle loaded MoO2/Ni(OH)2A nanosheet array structure material.
2. The method according to claim 1, wherein the nickel salt is nickel nitrate hexahydrate; the molybdenum salt is ammonium heptamolybdate tetrahydrate; the reducing agent is sodium borohydride; the platinum source water solution is chloroplatinic acid water solution.
3. The method according to claim 1, wherein the volume ratio of the aqueous ammonia to the anhydrous methanol is 3: 1.
4. The method according to claim 1, wherein the ratio of the amounts of the nickel salt, the molybdenum salt, the reducing agent and the platinum source is 0.175 to 1.225:0.175:1:0.00375 to 0.0075.
5. The production method according to any one of claims 1 to 4, wherein the concentration of the reducing agent in the mixed solution is 0.05M.
6. The production method according to claim 1 or 2, characterized in that the concentration of the platinum source aqueous solution is 0.03M; the volume ratio of the platinum source water solution added in the first time to the platinum source water solution added in the second time is 1: 5-9.
7. The method according to claim 1 or 2, wherein the solvothermal reaction is carried out at 150 ℃ for 8 hours.
8. The preparation method of any one of claims 1 to 7, wherein the Pt nano-particle loaded MoO is prepared by the method2/Ni(OH)2A nanosheet array structure material.
9. The Pt nanoparticle-supported MoO of claim 82/Ni(OH)2Nano-sheetApplication of array structure material as Hydrogen Evolution Reaction (HER) electrocatalyst.
10. The Pt nanoparticle-supported MoO of claim 82/Ni(OH)2The nano-sheet array structure material is applied as a full-water decomposition cathode catalyst material.
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