CN113174608A - Preparation method of double-doped porous cobalt phosphide nanosheet electrocatalytic material - Google Patents
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Abstract
The invention relates to a bimetallic doped porous cobalt phosphide nanosheet electrocatalytic material, and a preparation method and application thereof, and belongs to the technical field of material preparation and electrocatalysis. The invention takes CoP with good stability and good conductivity as a main body, and prepares Cr with high specific surface area and uniformly distributed components by doping and low-temperature calciningxFeyCozP nano-sheet. The prepared material can be used for electrocatalytic hydrogen and oxygen evolution reaction and shows good electrocatalytic performance.
Description
Technical Field
The invention relates to a bimetallic doped porous cobalt phosphide nanosheet electrocatalytic material and a preparation method thereof, and belongs to the technical field of material preparation and electrocatalysis.
Background
Renewable energy sources are developed, environmental pollution is reduced, and the method is vital to the sustainable development of human beings. Hydrogen energy is considered a promising alternative fuel in its clean and sustainable properties. The water decomposition is considered as an environment-friendly and has wide application prospectThe technology for producing high-purity hydrogen. However, in practical applications, water splitting is greatly limited by the slow kinetics of the Oxygen Evolution Reaction (OER) and the Hydrogen Evolution Reaction (HER). In order to obtain practical energy conversion, the development of highly active electrolytic water catalysts is urgently required. At present, is used for (H)2) Release reaction and oxygen (O)2) The highly active electrocatalysts which release the reaction are based on Pt and Ru based materials, respectively. However, the use in practical production is severely limited by the expensive price and the extremely low reserves. Therefore, the design and development of the non-noble metal electrocatalyst material with high activity and low cost have important theoretical and application values.
Transition Metal Phosphides (TMPs) have received much attention from researchers due to their noble metal-like properties, good electronic conductivity and chemical stability. The basic building unit is an isotropic crystal structure, and more active sites are easily exposed. The negatively charged P in TMPs acts as a proton acceptor, which can weaken the strong bond of metal (positively charged, hydride acceptor is M-H), thereby promoting the desorption of hydrogen. In addition, TMPs form amorphous transition metal oxyhydroxide shells on the catalyst surface in the OER reaction, which accelerate the oxidation of-OOH intermediates and act as O2Precipitated catalytically active sites. The combination of these excellent properties results in TMPs suitable for bulk water splitting catalysis. For example, Li et Al report a flower-like Al dispersion2O3CoP/CoP on stents2Nanoparticles, as bifunctional electrocatalysts, have good water splitting properties (nanoscales, 2017,00, 1-9). In addition, heteroatom doping TMPs is considered to be an effective method for improving the intrinsic catalytic performance of the electrocatalyst by adjusting the crystal structure, the conductivity and the charge distribution, and the conductivity of the whole system can be obviously improved and the surface active sites can be increased by element doping, so that the electrocatalytic performance of the material is improved. For example, Li and coworkers prepared Mn-doped porous CoP nanosheets, which could enhance the water splitting performance of CoP by Mn-doping (Dalton Trans.,2018,47, 14679-14685).
Until now, no report is found in the research on the synthesis of chromium and iron bimetal co-doped phosphide nanosheets for integral water cracking, the CoP used in the invention has stable physicochemical properties, cheap and easily available raw materials and no toxicity, the reaction process for preparing the CrFe-CoP nano electro-catalytic material by taking the CoP as a main body is simple, the obtained product has excellent electro-catalytic performance and high stability, and is expected to be produced industrially on a large scale. Meanwhile, compared with a noble metal catalyst, TMPs has low cost and wide raw material source, and is more suitable for commercial production and application.
Disclosure of Invention
The invention aims to provide a novel ferrochrome bimetal co-doped porous cobalt phosphide nano electro-catalytic material and a preparation method thereof.
The invention is realized by the following technical scheme:
step (1): preparation of cobalt hydroxide nanosheets (α -Co (OH)2): weighing a certain amount of CoCl2·6H2O, NaCl and C6H12N4Adding deionized water and anhydrous ethanol into beaker, mixing and stirring for 15min to dissolve, wherein VWater (W)：VEthanolStirring and heating the mixed solution for reaction at a ratio of 9:1, naturally cooling to room temperature, centrifuging to obtain green precipitate, washing with water and alcohol for several times, centrifuging, and vacuum drying to obtain alpha-Co (OH)2(ii) a Reference may be made in particular to J.A.chem.Soc.2005,127,13869-13874.
Step (2): preparation of ferrochrome-codoped cobalt hydroxide nanosheet (CrFe-Co (OH)2): mixing alpha-Co (OH)2、Fe(NO3)3·9H2O and Cr (NO)3)3·9H2Dissolving O in absolute ethanol and ultrasonic treating, alpha-Co (OH)2、Fe(NO3)3·9H2O and Cr (NO)3)3·9H2The molar ratio of O is 20:3:2, the mixed solution is stirred and heated for reaction, and finally the obtained CrFe-Co (OH)2And centrifuging the precipitate, washing with deionized water, washing with absolute ethyl alcohol, and drying.
And (3): preparing a ferrochrome co-doped cobalt phosphide nanosheet (CrFe-CoP): taking out the dried CrFe-Co (OH)2With NaH2PO2·H2Grinding with the mass ratio of 1:5, uniformly mixing, placing in a crucible, transferring the crucible into a temperature-rising tube furnace with automatic program temperature control, and carrying out nitrogen protectionCalcining at 300 deg.C for 2 hr, naturally cooling to room temperature, taking out to obtain black powder CrxFeyCozP nano-sheet.
In the step (1), the heating temperature is 90 ℃, and the reaction time is 1 h; drying means drying in a vacuum oven at 60 ℃ for 12 h.
In the step (1), CoCl2·6H2O, NaCl and C6H12N4The concentrations were 12.2mmol/L, 29mmol/L and 60mmol/L, respectively.
In the step (2), the heating temperature is 50 ℃, and the reaction time is 12 hours; drying means drying in a vacuum oven at 60 ℃ for 12 h.
In the step (2), the power of an ultrasonic machine used for ultrasonic dispersion is 250W, and the ultrasonic treatment time is 0.5 h.
In the step (2), alpha-Co (OH)2The concentration is 0.2 mol/L.
In the step (3), CrxFeyCozP nanosheet, x ═ 0.1 to 0.15; y is 0.1-0.15, and z is 0.7-0.8.
The ferrochrome codoped cobalt phosphide prepared by the method is applied to electrocatalytic full-hydrolysis under alkaline conditions.
The product was analyzed for composition morphology using an X-ray diffractometer (XRD), a Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM). A three-electrode reaction device is adopted, a platinum wire is used as a counter electrode, a silver-silver chloride (Ag/AgCl) electrode is used as a reference electrode, and the electrochemical performance of the product is tested in 1M KOH electrolyte.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method disclosed by the invention is composed of simple solvothermal reaction and low-temperature calcination reaction, and has the advantages of simple steps, short reaction time, convenience in operation, environmental friendliness and strong repeatability;
(2) the porous nanosheet structure of the material increases the specific surface area of the electrode active material, provides more active sites, is beneficial to permeation of electrolyte and release of bubbles after reaction, and improves the electron transmission efficiency due to the synergistic effect of the multi-metal phosphide, so that the electrocatalytic activity can be further improved;
(3) the invention enhances the charge transfer efficiency of the cobalt phosphide catalyst material by doping the ferrochrome bimetal, optimizes the adsorption energy of the intermediate by adjusting the electronic structure, and accelerates the reaction kinetics.
Drawings
FIGS. 1a and b are respectively alpha-Co (OH)2And Cr0.1Fe0.15Co0.75XRD diffraction pattern of P nano sheet electro-catalyst. As can be seen, Co (OH)2And Cr0.1Fe0.15Co0.75The P nano catalytic material has been successfully prepared, and the sample has high crystallinity and no impurity.
FIGS. 2a and b are respectively prepared alpha-Co (OH)2Scanning electron micrographs and transmission electron micrographs of the electrocatalyst; FIG. 2c and d are Cr0.1Fe0.15Co0.75(OH)2Scanning electron micrographs and transmission electron micrographs of the electrocatalyst; FIGS. 2e and f are the prepared Cr0.1Fe0.15Co0.75Scanning electron microscope photographs and transmission electron microscope photographs of the P nanosheet electrocatalyst.
FIGS. 3a and b are the comparison graphs of the polarization curves of hydrogen evolution and oxygen evolution reactions of the prepared precursor and electrocatalytic materials with different doping amount ratios under the condition of 1M KOH, respectively, and the prepared Cr0.1Fe0.15Co0.75The P nanosheet electrocatalytic material has the most excellent electrocatalytic activity.
Detailed Description
COMPARATIVE EXAMPLE 1 alpha-Co (OH)2Preparation of nanosheets
α-Co(OH)2The preparation of the nano-sheet adopts a solvothermal precipitation method: 0.581g of CoCl was weighed2·6H2O, 0.339g NaCl and 1.68g C6H12N4Adding 180mL of deionized water and 20mL of absolute ethyl alcohol into a beaker, magnetically stirring for 15min until the deionized water and the absolute ethyl alcohol are completely dissolved, stirring and heating the mixed solution to 90 ℃ for reaction for 1h, naturally cooling to room temperature, centrifuging to obtain green precipitate, washing with water and alcohol for 3 times, centrifuging, and drying in vacuum at 60 ℃ for 12h to obtain alpha-Co (OH)2。
COMPARATIVE EXAMPLE 2CrFe-Co (OH)2Preparation of nanosheets
CrFe-Co(OH)2The preparation of the nano-sheet adopts a cation exchange method: weigh 0.930g of alpha-Co (OH)2、0.606g Fe(NO3)3·9H2O and 0.400g Cr (NO)3)3·9H2Dispersing O in 50ml absolute ethanol, performing ultrasonic treatment for 0.5h, stirring at 50 deg.C for 12h to obtain uniform and stable suspension, centrifuging to obtain precipitate, washing with water and ethanol for 3 times, centrifuging, placing in a vacuum oven at 60 deg.C, drying for 12h, taking out, grinding into powder to obtain CrFe-Co (OH)2。
Comparative example 3 preparation of CoP nanosheets
The preparation of the CoP nanosheet adopts a low-temperature phosphating method: 0.1g of dried alpha-Co (OH) was weighed2With 0.5g NaH2PO2·H2Grinding, uniformly mixing, placing in a crucible, transferring the crucible to an automatic program temperature control heating tube furnace, calcining for 2h at 300 ℃ under the protection of nitrogen, wherein the heating rate is 2 ℃/min, naturally cooling to room temperature after the reaction is finished, and taking out to obtain black powder which is a CoP nanosheet.
Example 1Cr0.1Fe0.1Co0.8Preparation of P nanosheet electrocatalytic material
The preparation of the nano electro-catalytic material adopts a cation exchange method and a low-temperature phosphating method: weigh 0.930g of alpha-Co (OH)2、0.404g Fe(NO3)3·9H2O and 0.400g Cr (NO)3)3·9H2Dispersing O in 50ml absolute ethanol, ultrasonic treating for 0.5h, stirring at 50 deg.C for 12h to obtain uniform and stable suspension, centrifuging to obtain precipitate, washing with water and ethanol for 3 times, centrifuging, placing in 60 deg.C vacuum oven, drying for 12h, taking out, grinding into powder to obtain Cr0.1Fe0.1Co0.8(OH)2. 0.1g of Cr is weighed0.1Fe0.1Co0.8(OH)2With 0.5g NaH2PO2·H2Grinding O, uniformly mixing, placing in a crucible, transferring the crucible into an automatic program temperature control heating tube furnace, calcining for 2h at 300 ℃ under the protection of nitrogen, wherein the heating rate is 2 ℃/min, naturally cooling to room temperature after the reaction is finished, taking out, and obtaining blackThe color powder is Cr0.1Fe0.1Co0.8P nanosheet electrocatalytic material.
Example 2Cr0.1Fe0.15Co0.75Preparation of P nanosheet electrocatalytic material
The preparation method of the electrocatalytic material is basically the same as that of the example 1, except that: weigh 0.930g of alpha-Co (OH)2、0.606g Fe(NO3)3·9H2O and 0.400g Cr (NO)3)3·9H2O is dispersed in 50ml of absolute ethanol.
Example 3Cr0.15Fe0.1Co0.75Preparation of P nanosheet electrocatalytic material
The preparation method of the electrocatalytic material is basically the same as that of the example 1, except that: weigh 0.930g of alpha-Co (OH)2、0.404g Fe(NO3)3·9H2O and 0.600g Cr (NO)3)3·9H2O is dispersed in 50ml of absolute ethanol.
Example 4Cr0.15Fe0.15Co0.7Preparation of P nanosheet electrocatalytic material
The preparation method of the electrocatalytic material is basically the same as that of the example 1, except that: weigh 0.930g of alpha-Co (OH)2、0.606g Fe(NO3)3·9H2O and 0.600g Cr (NO)3)3·9H2O is dispersed in 50ml of absolute ethanol.
Examples nanomaterial electrocatalytic activity experiments
(1) 1ml of 5 vol% Nafion/ethanol solution was prepared.
(2) 0.004g of electrocatalytic material is weighed and added into the prepared solution in the step (1), and the ultrasonic treatment is continued for 0.5 h.
(3) KOH solution with the concentration of 1 mol per liter is used as electrolyte, a three-electrode reaction device is adopted, a platinum wire is used as a counter electrode, Ag/AgCl is used as a reference electrode, the scanning speed is 5mV/s, and the electrocatalytic water decomposition performance of the ferrochrome bimetallic co-doped cobalt phosphide electrode material is tested.
EXAMPLES characterization analysis of ferrochrome bimetallic codoped CoP catalyst
FIGS. 1a and b are respectively alpha-Co (OH)2And Cr0.1Fe0.15Co0.75XRD diffraction pattern of P nanosheet electrocatalyst, from which alpha-Co (OH) can be seen2The diffraction peak in (A) corresponds well to a-Co (OH)2Standard card (PDF #46-0605) by doping ferrochrome bimetal and in N2Cr formed after phosphating in an atmosphere0.1Fe0.15Co0.75P corresponds well to the CoP standard card (PDF # 29-0497).
FIGS. 2a and b are respectively prepared alpha-Co (OH)2Scanning electron micrographs and Transmission electron micrographs of the electrocatalyst, and the synthesized α -Co (OH) can be seen in FIGS. 2a, b2The electric catalyst is a hexagonal nano sheet; FIG. 2c and d are Cr0.1Fe0.15Co0.75(OH)2Scanning electron microscope photographs and transmission electron microscope photographs of the electrocatalyst, it can be seen from fig. 2c, d that the hexagonal nanosheet structure is not changed but the surface and periphery become rough after element doping, which is caused by ion exchange; FIGS. 2e and f are the prepared Cr0.1Fe0.15Co0.75The scanning electron microscope photo and the transmission electron microscope photo of the P nano sheet electro-catalyst show that the hexagonal nano sheet structure is still kept complete after phosphorization and a large number of micropores are formed, which is beneficial to medium exchange and is beneficial to improvement of electrochemical performance from figures 2e and f.
FIGS. 3a and b are respectively prepared alpha-Co (OH)2、CrFe-Co(OH)2、CoP、Cr0.1Fe0.1Co0.8P、Cr0.1Fe0.15Co0.75P、Cr0.15Fe0.1Co0.75P and Cr0.15Fe0.15Co0.7Polarization curves of P electrocatalyst in 1M KOH reaction are compared. It can be seen from the figure that the monomer alpha-Co (OH) can be improved by doping the element2The activity of the electrocatalyst can also be improved through a phosphating process, wherein the phosphated electrocatalyst Cr is doped by elements with different proportions0.1Fe0.15Co0.75The best P performance is achieved, and the current density is 10mA cm-2Corresponding to hydrogen evolution and oxygen evolutionThe overpotentials were 103mV and 256mV, respectively.
Claims (5)
1. A preparation method of a double-doped porous cobalt phosphide nanosheet electrocatalytic material, wherein the double-doped porous cobalt phosphide nanosheet electrocatalytic material can be used for electrocatalytic full-hydrolysis under an alkaline condition, and is characterized by comprising the following specific steps of:
step (1): preparation of ferrochrome co-doped cobalt hydroxide nanosheet CrFe-Co (OH)2: cobalt hydroxide nanosheet alpha-Co (OH)2、Fe(NO3)3·9H2O and Cr (NO)3)3·9H2Dissolving O in absolute ethyl alcohol for ultrasonic treatment, stirring and heating the mixed solution for reaction, and finally obtaining CrFe-Co (OH)2Centrifuging the precipitate, washing with deionized water, washing with anhydrous ethanol, and drying;
step (2): preparing a ferrochrome co-doped cobalt phosphide nanosheet (CrFe-CoP): taking out the dried CrFe-Co (OH)2With NaH2PO2·H2Grinding O, uniformly mixing, placing in a crucible, transferring the crucible into a temperature-rising tube furnace with automatic program temperature control, calcining for 2h at 300 ℃ under the protection of nitrogen, naturally cooling to room temperature, taking out, and obtaining black powder of CrxFeyCozP nano-sheet.
2. The preparation method of the double-doped porous cobalt phosphide nanosheet electrocatalytic material as set forth in claim 1, wherein in the step (1), the heating temperature is 50 ℃ and the reaction time is 12 hours; drying in a vacuum oven at 60 deg.C for 12 hr; the power of an ultrasonic machine used for ultrasonic dispersion is 250W, and the ultrasonic treatment time is 0.5 h.
3. The preparation method of the double-doped porous cobalt phosphide nanosheet electrocatalytic material as described in claim 1, wherein in step (1), α -Co (OH)2、Fe(NO3)3·9H2O and Cr (NO)3)3·9H2The molar ratio of O is 20:3:2, alpha-Co (OH)2The concentration is 0.2 mol/L.
4. The preparation method of the double-doped porous cobalt phosphide nanosheet electrocatalytic material as described in claim 1, wherein in step (2), CrFe-Co (OH)2With NaH2PO2·H2The mass ratio of O is 1: 5; cr (chromium) componentxFeyCozP nanosheet, x ═ 0.1 to 0.15; y is 0.1-0.15, and z is 0.7-0.8.
5. The preparation method of the double-doped porous cobalt phosphide nanosheet electrocatalytic material as claimed in claim 4, wherein Cr isxFeyCozP nanosheet, x ═ 0.1; y is 0.15 and z is 0.75.
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