CN107651656B - Ni2P4O12Nanoparticle material, preparation method and application thereof - Google Patents
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Abstract
Ni2P4O12A nano-particle material and a preparation method thereof belong to the technical field of catalyst preparation. Ni of the invention2P4O12The nano-particle material has a multistage nano-structure, 5-10 nm of nano-crystals are modified on about 100nm of network-shaped interconnected nano-particles, the structure provides a great active site for oxygen precipitation reaction in electrolyzed water, and is beneficial to adsorption of water molecules, and theoretical research proves that crystal faces of the exposed nano-crystals have low adsorption energy on the water molecules and oxygen intermediates.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to Ni2P4O12A nano-particle material, a preparation method thereof and application thereof in catalyzing oxygen evolution reaction.
Background
Energy and environmental problems caused by rapid economic development increasingly restrict sustainable development of society, and research and development of clean and renewable energy sources capable of replacing traditional fossil energy sources are very important due to environmental problems such as high carbon emission and the like of the traditional fossil energy sources. Among them, hydrogen has the advantages of no pollution, high energy density, abundant sources, etc. and is one of the most potential clean energy sources, and its preparation technology has also been widely paid attention by researchers. Electrolysis of water, as the simplest and mature method of hydrogen production, is considered to be the most suitable means for large-scale application; however, when the hydrogen is produced by electrolyzing water, the hydrogen evolution and oxygen evolution reactions on the double electrodes of the electrolyzed water have higher overpotential, which increases the energy loss of the electrolytic cell, and meanwhile, the high cost brought by the noble metal catalytic electrode is also an important factor restricting the wide application of the electrode.
The anodic oxygen evolution reaction is used as an important reaction in the hydrogen production by water electrolysis, and the energy loss caused by the higher overpotential of the anodic oxygen evolution reaction becomes a bottleneck problem to be solved urgently in water electrolysis. Traditional anode catalytic materials are based on platinum-based precious metal materials, such as ruthenium and iridium oxides and carbon-supported composite materials thereof, and although these materials have good catalytic activity, the scarcity and high price of the precious metals greatly limit the sustainable use of the precious metals on a commercial scale. Therefore, the research and development of a non-noble metal-based anode catalytic material with low cost, high efficiency and low pollution is a problem to be solved at present.
Cui et al (Energy environ. sci.2015,8,1719) report an electrochemical lithium removal regulation lithium iron phosphate material and oxygen evolution activity thereof, wherein an electrochemical lithium removal method needs to package and disassemble a battery, and the operation process is complex; bao et al (ACS appl. Mater. interface 2016,8,22534) reported a carbon-coated Co2P2O7The nanocrystalline has better catalytic activity and stability, but the carbon layer obtained by decomposing the polymer in the preparation process needs high annealing problem (750 ℃), and the cost is increased. In addition, the prepared catalytic material is powdery and needs to be coated on a substrate in a spin mode to form an electrode, so that the time cost and the process complexity are increased.
Disclosure of Invention
Aiming at the defects in the background art, the invention provides Ni2P4O12Nanoparticle materials and methods for their preparation. The loaded Ni provided by the invention2P4O12The electrode of the nano particles shows good catalytic activity and catalytic stability in the oxygen precipitation reaction of the electrolyzed water, and has the advantages of simple process, low cost and easy realization of large-scale production.
The technical scheme of the invention is as follows:
ni2P4O12Nanoparticle material, characterized in that said Ni2P4O12The nano-particle material has a multi-level structure and is formed by modifying 5-10 nm of nano-crystals on network-shaped interconnected nano-particles.
Ni2P4O12A method of preparing a nanoparticle material, comprising the steps of:
step 1: the method comprises the following steps of (3-4): 1, adding the mixture into deionized water, uniformly mixing to obtain a mixed solution A, and then adding ammonia water into the mixed solution A to obtain a mixed solution B; wherein the concentration of the Ni source is 0.2-0.3 mol/L, and the volume ratio of the mixed solution A to the ammonia water is (10-20): 1;
step 2: placing the conductive substrate into the mixed liquid B prepared in the step 1, standing for 15-20 min for Ni (OH)2Growing the nanosheet precursor, then taking out and cleaning, and naturally airing;
and step 3: loading Ni (OH) obtained in step 22The conductive substrate is placed in a quartz tube heating center, and 0.1-1 g of phosphorus source is placed in an upstream area of the quartz tube;
and 4, step 4: vacuumizing the interior of the quartz tube to below 0.1atm, introducing inert gas to keep the pressure in the tube in a normal pressure environment, and introducing carrier gas flow;
and 5: heating the quartz tube at a heating rate of 2-8 ℃/min to enable the temperature of a heating center to reach 280-350 ℃, and then preserving heat at the temperature of 280-350 ℃ for 0-60 min, wherein Ni (OH) is adopted in the process2Nanosheet reaction to produce Ni2P4O12A nanoparticle;
step 6: after the reaction is finished, the quartz tube is naturally cooled to room temperature, the conductive substrate is taken out, and Ni can be obtained on the conductive substrate2P4O12And (3) nanoparticles.
Further, in step 1, the persulfate is ammonium persulfate, sodium persulfate, potassium persulfate or the like.
Further, the Ni source in the step 1 is one or more of nickel chloride hexahydrate, nickel sulfate and nickel nitrate.
Further, the conductive substrate in step 2 is a flexible substrate such as carbon cloth, nickel foam, or the like, or a hard substrate such as FTO, or the like.
Further, the phosphorus source in step 3 is sodium hypophosphite containing crystal water.
Further, in the step 4, the inert gas is argon or nitrogen, the carrier gas flow is argon, nitrogen or a mixed gas of argon and hydrogen, and the flow rate of the carrier gas flow is 20-50 sccm.
The invention also provides the above Ni2P4O12Use of nanoparticles as anode material for electrolysis of water.
The invention has the beneficial effects that:
1. the invention provides Ni2P4O12The nano particle material has a multistage nano structure, 5-10 nm of nano crystals are modified on about 100nm of network-shaped interconnected nano particles, the structure provides a great active site for oxygen precipitation reaction in electrolyzed water, and is beneficial to adsorption of water molecules, and theoretical research proves that the crystal faces of the exposed nano crystals have low adsorption energy on the water molecules and oxygen intermediates.
2. The invention provides Ni2P4O12The preparation method of the nano-particle material regulates and controls the reaction environment in the quartz tube by regulating the amount of the provided phosphorus source and the reaction time, thereby obtaining the Ni with good crystallinity and good dispersibility2P4O12And (3) nanoparticles.
3. The loaded Ni provided by the invention2P4O12The electrode of the nano-particles shows good catalytic activity in the oxygen precipitation reaction, and the loaded Ni can be seen from the electrochemical polarization curve2P4O12The electrode of the nano-particles only needs 280mV to reach 10mA cm in oxygen evolution reaction-2The current density of the catalyst is high, and the catalyst has good catalytic stability.
Drawings
FIG. 1 shows Ni obtained in example 1 of the present invention2P4O12Electron Microscope (SEM) images of nanoparticles;
FIG. 2 shows Ni obtained in example 1 of the present invention2P4O12High Resolution Transmission Electron Microscopy (HRTEM) images of two-level structures of nanoparticles and nanocrystals;
FIG. 3 shows Ni obtained in example 1 of the present invention2P4O12HAADF characterization images of the nanoparticle structures in TEM bright and dark fields, and insets are corresponding selected region electron diffraction SAED characterization images;
FIG. 4 shows Ni obtained from different phosphorus sources and reaction times in examples 1, 2, 3 and 4 of the present invention2P4O12An X-ray diffraction (XRD) pattern of the material;
FIG. 5 shows Ni obtained in example 1 of the present invention2P4O12An electrochemical performance characterization diagram of an oxygen precipitation reaction of the nano-particle material in a 1M KOH solution; (a) ni2P4O12(NPO) and reference material RuO2、Ni(OH)2Comparing with a polarization curve of bare Carbon Cloth (CC); (b) the corresponding tafel slope;
FIG. 6 shows Ni load obtained in example 1 of the present invention2P4O12Continuously testing the electrolytic stability of the carbon cloth electrode of the nano-particle material in a 1M KOH solution for 100 h;
FIG. 7 shows Ni load obtained in example 1 of the present invention2P4O12SEM images of carbon cloth electrodes of nanoparticle materials after 100h of continuous electrolysis in 1M KOH solution.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Example 1
Ni2P4O12A method of preparing a nanoparticle material, comprising the steps of:
step 1: nickel chloride hexahydrate and ammonium persulfate according to a molar ratio of 4: 1, adding the mixture into deionized water, uniformly mixing the mixture by ultrasonic waves to obtain a mixed solution A, and then adding ammonia water into the mixed solution A to obtain a mixed solution B; wherein the concentration of the Ni source is 0.25mol/L, and the volume ratio of the mixed solution A to the ammonia water is 16: 1;
step 2: putting the carbon cloth into the mixed solution B prepared in the step 1, standing for 20min for Ni (OH)2Growing the nanosheet precursor, then taking out and cleaning, and naturally airing;
and step 3: loading Ni (OH) obtained in step 22The carbon cloth is placed in a heating center of a quartz tube, 1g of sodium hypophosphite containing crystal water is placed in an upstream area of the quartz tube, and the distance from the heating center is 15 cm;
and 4, step 4: vacuumizing the interior of quartz tube to below 0.1atm, introducing Ar gas to maintain the pressure in the tube at normal pressure, repeating the process of vacuumizing and introducing argon gas for 3 times, and introducing Ar and H2The mixed gas (the atomic ratio of argon to hydrogen in the mixed gas is 95:5, the flow rate of the mixed gas is 20sccm) is used as a carrier gas flow, so that the pressure in the tube is kept in a normal pressure environment;
and 5: heating the quartz tube at a heating rate of 3 deg.C/min to a heating center temperature of 300 deg.C, and maintaining at 300 deg.C for 30min, in which process Ni (OH)2Nanosheet reaction to produce Ni2P4O12A nanoparticle;
step 6: after the reaction is finished, the carbon cloth is taken out after the quartz tube is naturally cooled to the room temperature, and the Ni load can be obtained2P4O12A carbon cloth electrode of nanoparticles.
Ni obtained in example 12P4O12An electron microscope (SEM) of the nanoparticles is shown in fig. 1, a high-resolution transmission electron microscope (HRTEM) is shown in fig. 2, and a HAADF characterization under TEM bright and dark fields is shown in fig. 3; ni Supported obtained in example 12P4O12The electrochemical performance test curve of the carbon cloth electrode of the nano particles in the 1M KOH solution is shown in figure 5, and the electrolytic stability test curve in the 1M KOH solution is shown in figure 6.
Example 2
Ni preparation according to the procedure of example 12P4O12And (3) adjusting the heat preservation time of the nano particle material in the step (5) to 10min, and keeping other steps unchanged. Example 2 preparation of the resulting Ni2P4O12The XRD diffraction pattern of the nanoparticle material is shown in fig. 4.
Example 3
Ni preparation according to the procedure of example 12P4O12Nano-particle material, only the amount of sodium hypophosphite containing crystal water in step 3 is adjustedThe holding time of step 5 at 300 ℃ was adjusted to 0.1g, and the other steps were not changed. Example 3 preparation of the resulting Ni2P4O12The XRD diffraction pattern of the nanoparticle electrode is shown in fig. 4.
Example 4
Ni preparation according to the procedure of example 12P4O12And (3) adjusting the amount of only sodium hypophosphite containing crystal water in the step (3) to 0.1g, adjusting the heat preservation time of the step (5) at the temperature of 300 ℃ to 10min, and keeping the other steps unchanged. Example 4 preparation of the resulting Ni2P4O12The XRD diffraction pattern of the nanoparticle electrode is shown in fig. 4.
FIG. 1 shows Ni obtained in example 12P4O12Electron Microscope (SEM) images of nanoparticles; FIG. 1 shows Ni obtained in example 12P4O12The surface of the nanoparticles is formed by network-like interconnected nanoparticles with the surface of about 100 nm. FIG. 2 shows Ni obtained in example 12P4O12High Resolution Transmission Electron Microscopy (HRTEM) images of two-level structures of nanoparticles and nanocrystals; as can be seen from FIG. 2, nanocrystals of about 5-10 nm are uniformly distributed on the network-like interconnected nanoparticles of about 100nm, and the rich edge structure of the nanocrystals provides a large number of active sites for the nanoparticles in the catalytic reaction. FIG. 3 shows Ni obtained in example 12P4O12HAADF characterization images of the nanoparticle structures in TEM bright and dark fields, and insets are corresponding selected region electron diffraction SAED characterization images; from FIG. 3, the clear network-like interconnect structure and Ni can be seen2P4O12Polycrystalline nature of the nanocrystals. FIG. 4 shows the results of the reaction of different phosphorus sources and reaction times for Ni in examples 1, 2, 3 and 42P4O12An X-ray diffraction (XRD) pattern of the material; as can be seen from FIG. 4, Ni with different degrees of crystallinity can be obtained by controlling the content of phosphorus source and the phosphorylation time2P4O12And (3) sampling. FIG. 5 shows Ni-loaded samples obtained in example 12P4O12Electrochemical performance of oxygen evolution reaction of carbon cloth electrode of nano particles in 1M KOH solutionA representation; (a) ni2P4O12And reference material RuO2、Ni(OH)2Comparing with the polarization curve of the bare carbon cloth; (b) the corresponding tafel slope; as is clear from FIG. 5, Ni load obtained in example 12P4O12The carbon cloth electrode of the nano-particles only needs 280mV overpotential to reach 10mA cm in the oxygen evolution reaction-2The above current densities indicate that Ni is the present invention2P4O12The nano-particles have good catalytic activity and the performance of the nano-particles is close to that of commercial RuO2. FIG. 6 shows Ni-loaded samples obtained in example 12P4O12Continuously testing the electrolytic stability of the nano-particle carbon cloth electrode in a 1M KOH solution for 100 h; as is clear from FIG. 6, Ni load obtained in example 12P4O12The nano-particle carbon cloth electrode has good stability. FIG. 7 shows Ni-loaded samples obtained in example 12P4O12SEM image of the nano-particle carbon cloth electrode after continuous electrolysis in 1MKOH solution for about 100 h; as is clear from FIG. 7, Ni load obtained in example 12P4O12After the nano-particle carbon cloth electrode is continuously electrolyzed for 100h, the surface of the nano-particle carbon cloth electrode still keeps a network-shaped interconnected structure, which shows that the material has good structural stability.
Claims (9)
1. Ni2P4O12Nanoparticle material, characterized in that said Ni2P4O12The nano-particle material has a multi-level structure and is formed by modifying 5-10 nm of nano-crystals on network-shaped interconnected nano-particles.
2. Ni2P4O12A method of preparing a nanoparticle material, comprising the steps of:
step 1: the method comprises the following steps of (3-4): 1, adding the mixture into deionized water, uniformly mixing to obtain a mixed solution A, and then adding ammonia water into the mixed solution A to obtain a mixed solution B; wherein the concentration of the Ni source is 0.2-0.3 mol/L, and the volume ratio of the mixed solution A to the ammonia water is (10-20): 1;
step 2: placing the conductive substrate into the mixed liquid B prepared in the step 1, standing for 15-20 min, taking out, cleaning and naturally drying;
and step 3: placing the conductive substrate obtained in the step (2) into a quartz tube heating center, and placing 0.1-1 g of phosphorus source in an upstream area of the quartz tube;
and 4, step 4: vacuumizing the interior of the quartz tube to below 0.1atm, introducing inert gas to keep the pressure in the tube in a normal pressure environment, and introducing carrier gas flow;
and 5: heating the quartz tube at a heating rate of 2-8 ℃/min to enable the temperature of a heating center of the quartz tube to reach 280-350 ℃, and then preserving heat for 0-60 min at the temperature of 280-350 ℃;
step 6: after the reaction is finished, the quartz tube is naturally cooled to room temperature, the conductive substrate is taken out, and Ni can be obtained on the conductive substrate2P4O12And (3) nanoparticles.
3. Ni according to claim 22P4O12The preparation method of the nanoparticle material is characterized in that the persulfate in the step 1 is ammonium persulfate, sodium persulfate or potassium persulfate.
4. Ni according to claim 22P4O12The preparation method of the nano-particle material is characterized in that the Ni source in the step 1 is one or more of nickel chloride hexahydrate, nickel sulfate and nickel nitrate.
5. Ni according to claim 22P4O12The preparation method of the nano-particle material is characterized in that the conductive substrate in the step 2 is carbon cloth, foamed nickel or FTO.
6. Ni according to claim 22P4O12The preparation method of the nano-particle material is characterized in that the phosphorus source in the step 3 is sodium hypophosphite containing crystal water.
7. Ni according to claim 22P4O12The preparation method of the nano-particle material is characterized in that in the step 4, the inert gas is argon, the carrier gas flow is argon, nitrogen or a mixed gas of argon and hydrogen, and the flow rate of the carrier gas flow is 20-50 sccm.
8. Ni as defined in claim 12P4O12Use of a nanoparticle material as an anode material for electrolysis of water.
9. Ni obtainable by the process of any of claims 2 to 72P4O12Use of nanoparticles as anode material for electrolysis of water.
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