CN113174608B - 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 calcining x Fe y Co z P nanosheet. 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, belonging 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. Water splitting is considered as a green and environmentally friendly technology for producing high-purity hydrogen with a wide application prospect. 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, 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, so that more active sites are easily exposed. The P with negative charge in TMPs is used as a proton acceptor, which can weaken the strong bond of metal (with positive charge, hydride acceptor is M-H), thereby promoting the desorption of hydrogen. In addition, TMPs form amorphous transition metal hydroxyls on the catalyst surface during OER reactionsAn oxide shell which accelerates the oxidation of the-OOH intermediate, acting as O 2 Precipitated catalytically active sites. The combination of these excellent properties has led to TMPs suitable for bulk water splitting catalysis. For example, li et Al report a dispersion in flower-like Al 2 O 3 CoP/CoP on stents 2 Nanoparticles, 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 nanoplates, by which CoP decomposition water performance was enhanced (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, the 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 nanosheet (alpha-Co (OH) 2 ): weighing a certain amount of CoCl 2 ·6H 2 O, naCl and C 6 H 12 N 4 Adding deionized water and anhydrous ethanol into beaker, mixing and stirring for 15min to dissolve, wherein V Water (W) ：V Ethanol And (9) stirring and heating the mixed solution for reaction, naturally cooling to room temperature, centrifuging to obtain a green precipitate, washing with water and alcohol for a plurality of times, centrifuging, and performing true washingAir 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(NO 3 ) 3 ·9H 2 O and Cr (NO) 3 ) 3 ·9H 2 Dissolving O in absolute ethyl alcohol, ultrasonic, alpha-Co (OH) 2 、Fe(NO 3 ) 3 ·9H 2 O and Cr (NO) 3 ) 3 ·9H 2 And the molar ratio of O is 20 2 And centrifuging the precipitate, washing with deionized water, washing with absolute ethyl alcohol, and drying.
And (3): preparing ferrochrome co-doped cobalt phosphide nanosheets (CrFe-CoP): taking out the dried CrFe-Co (OH) 2 With NaH 2 PO 2 ·H 2 Grinding O, wherein the mass ratio of the powder to the powder is 1 x Fe y Co z P nanosheet.
In the step (1), the heating temperature is 90 ℃, and the reaction time is 1h; drying means drying in a vacuum oven at 60 ℃ for 12h.
In the step (1), coCl 2 ·6H 2 O, naCl and C 6 H 12 N 4 The 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 12h; drying means drying in a vacuum oven at 60 ℃ for 12h.
In the step (2), the power of an ultrasonic machine used for ultrasonic dispersion is 250W, and the ultrasonic treatment time is 0.5h.
In the step (2), alpha-Co (OH) 2 The concentration was 0.2mol/L.
In the step (3), cr x Fe y Co z P nanoplatelets, x =0.1-0.15; y =0.1-0.15, z =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 each alpha-Co (OH) 2 And Cr 0.1 Fe 0.15 Co 0.75 XRD diffraction pattern of P nanometer slice electric catalyst. As can be seen from the figure, co (OH) 2 And Cr 0.1 Fe 0.15 Co 0.75 The 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) 2 Scanning electron micrographs and transmission electron micrographs of the electrocatalyst; FIG. 2c and d are each Cr 0.1 Fe 0.15 Co 0.75 (OH) 2 Scanning electron micrographs and transmission electron micrographs of the electrocatalyst; FIGS. 2e and f are the prepared Cr 0.1 Fe 0.15 Co 0.75 Scanning electron micrographs and transmission electron micrographs of the P nanosheet electrocatalyst.
FIGS. 3a and b are the comparison graphs of the polarization curves of hydrogen evolution reaction and oxygen evolution reaction of the prepared precursor and electrocatalytic materials with different doping amount ratios under the condition of 1M KOH, and the prepared Cr 0.1 Fe 0.15 Co 0.75 The P nanosheet electrocatalytic material has the most excellent electrocatalytic activity.
Detailed Description
COMPARATIVE EXAMPLE 1 alpha-Co (OH) 2 Preparation of nanosheets
α-Co(OH) 2 The preparation of the nano-sheet adopts a solvothermal precipitation method: 0.581g of CoCl was weighed out 2 ·6H 2 O, 0.339g NaCl and 1.68g C 6 H 12 N 4 Adding 180mL of deionized water and 20mL of absolute ethyl alcohol into a beaker, stirring for 15min by magnetic force until the deionized water and 20mL of 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) 2 Preparation of nanosheets
CrFe-Co(OH) 2 The preparation of the nano-sheet adopts a cation exchange method: 0.930g of alpha-Co (OH) is weighed 2 、0.606g Fe(NO 3 ) 3 ·9H 2 O and 0.400g Cr (NO) 3 ) 3 ·9H 2 Dispersing O in 50ml absolute ethanol, performing ultrasonic treatment for 0.5h, stirring at 50 ℃ 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 ℃, 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 dry alpha-Co (OH) is weighed 2 With 0.5g NaH 2 PO 2 ·H 2 Grinding, 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 1Cr 0.1 Fe 0.1 Co 0.8 Preparation of P nanosheet electrocatalytic material
The preparation of the nano electro-catalytic material adopts a cation exchange method and a low-temperature phosphating method: 0.930g of alpha-Co (OH) was weighed 2 、0.404g Fe(NO 3 ) 3 ·9H 2 O and 0.400g Cr (NO) 3 ) 3 ·9H 2 Dispersing O in 50ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 0.5h, stirring at 50 ℃ for 12h to react to obtain uniform and stable suspension, centrifuging to obtain precipitate, washing with water and alcohol for 3 times, centrifuging, placing in a vacuum oven at 60 ℃, drying for 12h, taking out, grinding into powder to obtain Cr 0.1 Fe 0.1 Co 0.8 (OH) 2 . 0.1g of Cr is weighed 0.1 Fe 0.1 Co 0.8 (OH) 2 With 0.5g NaH 2 PO 2 ·H 2 Grinding 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 black powder which is Cr 0.1 Fe 0.1 Co 0.8 P nanosheet electrocatalytic material.
Example 2Cr 0.1 Fe 0.15 Co 0.75 Preparation of P nanosheet electrocatalytic material
The preparation method of the electrocatalytic material is basically the same as that of the example 1, except that: 0.930g of alpha-Co (OH) was weighed 2 、0.606g Fe(NO 3 ) 3 ·9H 2 O and 0.400g Cr (NO) 3 ) 3 ·9H 2 O is dispersed in 50ml of absolute ethanol.
Example 3Cr 0.15 Fe 0.1 Co 0.75 Preparation of P nanosheet electrocatalytic material
The preparation method of the electrocatalytic material is basically the same as that of the example 1, except that: 0.930g of alpha-Co (OH) is weighed 2 、0.404g Fe(NO 3 ) 3 ·9H 2 O and 0.600g Cr (NO) 3 ) 3 ·9H 2 O is dispersed in 50ml of absolute ethanol.
Example 4Cr 0.15 Fe 0.15 Co 0.7 Preparation of P nano-sheet electro-catalytic materialPrepare for
The preparation method of the electrocatalytic material is basically the same as that of the example 1, except that: 0.930g of alpha-Co (OH) is weighed 2 、0.606g Fe(NO 3 ) 3 ·9H 2 O and 0.600g Cr (NO) 3 ) 3 ·9H 2 O is dispersed in 50ml of absolute ethanol.
Examples nanomaterial electrocatalytic activity experiments
(1) 1ml of a 5vol% 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 0.5h.
(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 electro-catalytic water decomposition performance of the ferrochrome bimetal co-doped cobalt phosphide electrode material is tested.
EXAMPLES characterization and analysis of ferrochrome bimetal co-doped cobalt phosphide catalyst
FIGS. 1a and b are respectively alpha-Co (OH) 2 And Cr 0.1 Fe 0.15 Co 0.75 XRD diffraction pattern of P nano-sheet electrocatalyst, alpha-Co (OH) can be seen from the pattern 2 The diffraction peak in (1) corresponds well to alpha-Co (OH) 2 Standard cards (PDF # 46-0605) by doping ferrochrome bimetal and in N 2 Cr formed after phosphating in atmosphere 0.1 Fe 0.15 Co 0.75 P corresponds well to the CoP standard card (PDF # 29-0497).
FIGS. 2a and b are prepared alpha-Co (OH) 2 Scanning electron micrographs and Transmission Electron micrographs of the electrocatalyst, it can be seen from FIGS. 2a, b that the synthesized α -Co (OH) 2 The electric catalyst is a hexagonal nano thin sheet; FIG. 2c and d are Cr 0.1 Fe 0.15 Co 0.75 (OH) 2 In the scanning electron microscope photos and the transmission electron microscope photos of the electrocatalyst, as can be seen from fig. 2c and d, the hexagonal nanosheet structure is not changed but the surface and the periphery become rough after element doping, which is caused by ion exchange; FIGS. 2e and f are the prepared Cr respectively 0.1 Fe 0.15 Co 0.75 P nano sheetIn the scanning electron microscope photos and the transmission electron microscope photos of the electrocatalyst, as can be seen from fig. 2e and f, the hexagonal nanosheet structure remains intact after the phosphating, and a large number of micropores are formed, which is beneficial to medium exchange and improvement of electrochemical performance.
FIGS. 3a and b are respectively prepared alpha-Co (OH) 2 、CrFe-Co(OH) 2 、CoP、Cr 0.1 Fe 0.1 Co 0.8 P、Cr 0.1 Fe 0.15 Co 0.75 P、Cr 0.15 Fe 0.1 Co 0.75 P and Cr 0.15 Fe 0.15 Co 0.7 Polarization 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 increased by doping with an element 2 The activity of the electrocatalyst can also be improved by a phosphating process, wherein the phosphated electrocatalyst Cr is doped by elements with different proportions 0.1 Fe 0.15 Co 0.75 The best P performance is achieved, and the current density is 10mA cm -2 The overpotential for hydrogen evolution and oxygen evolution is 103mV and 256mV respectively.
Claims (4)
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 codoped cobalt hydroxide nanosheet CrFe-Co (OH) 2 : cobalt hydroxide nanosheet alpha-Co (OH) 2 、Fe(NO 3 ) 3 ·9H 2 O and Cr (NO) 3 ) 3 ·9H 2 Dissolving O in absolute ethyl alcohol, performing ultrasonic treatment, stirring the mixed solution, heating for reaction, and finally obtaining the CrFe-Co (OH) 2 Centrifuging 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) 2 With NaH 2 PO 2 ·H 2 Grinding, uniformly mixing, placing in a crucible, transferring the crucible into an automatic program temperature control heating tube furnaceCalcining at 300 deg.C for 2h under nitrogen protection, naturally cooling to room temperature, taking out to obtain black powder of Cr x Fe y Co z P nanosheet;
in step (2), crFe-Co (OH) 2 With NaH 2 PO 2 ·H 2 The mass ratio of O is 1; cr (chromium) component x Fe y Co z P nanoplatelet, x =0.1-0.15; y =0.1-0.15, z =0.7-0.8.
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; the drying refers to placing in a vacuum oven at 60 ℃ for drying for 12h; the power of an ultrasonic machine used for ultrasonic dispersion is 250W, and the ultrasonic treatment time is 0.5h.
3. The method for preparing the double-doped porous cobalt phosphide nanosheet electrocatalytic material as described in claim 1, wherein in step (1), α -Co (OH) 2 、Fe(NO 3 ) 3 ·9H 2 O and Cr (NO) 3 ) 3 ·9H 2 The molar ratio of O is 20:3:2, alpha-Co (OH) 2 The concentration was 0.2mol/L.
4. The preparation method of the double-doped porous cobalt phosphide nanosheet electrocatalytic material as set forth in claim 1, wherein Cr is x Fe y Co z P nanoplatelets, x =0.1; y =0.15, z =0.75.
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