CN115029727A - confined-Fe-doped CoSe 2 /MXene composite material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a limited-domain Fe-doped CoSe 2 A/MXene composite material and a preparation method and application thereof belong to the field of electrocatalytic oxygen evolution. The composite material is prepared according to the following steps: a. uniformly growing and assembling a metal zeolite imidazole framework compound on the surface of two-dimensional MXene containing negative charge groups by using a room temperature liquid phase electrostatic assembly method to serve as a precursor; b. the precursor and potassium ferricyanide are subjected to room temperature ion exchange reaction, and fine Prussian blue crystals containing Fe are further loaded to synthesize [ ZIFs @ PBA]a/MXene "sandwich" precursor; c. in a hydrogen/argon mixed gas, carrying out high-temperature annealing in a quartz tube furnace to generate a porous carbon layer confinement FeCo metal/MXene sandwich composite structure; d. finally, the crystal selenium powder is used as a selenium source, and the limited domain type Fe-doped CoSe is obtained through high-temperature annealing reaction 2 the/MXene composite material. The composite material shows excellent electrolytic water oxygen evolution reaction performance under alkaline conditions, provides a new idea for developing an electrocatalyst with ultrahigh efficiency, stability and low cost, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of electrocatalytic oxygen evolution, and particularly relates to an oxygen evolution electrocatalytic composite material and a preparation method and application thereof.
Background
Electrocatalytic decomposition of water is a process that produces clean hydrogen fuel with zero carbon emissions and has received much attention from researchers. However, the slow, multi-step electron transfer involved Oxygen Evolution Reaction (OER) of the electrolyzed water anode results in a high energy barrier, making it require a tremendous energy input, so a low overpotential OER electrocatalyst is of critical importance. Currently, commercial ruthenium dioxide (RuO) 2 ) And iridium dioxide (IrO) 2 ) The OER electrocatalysts considered to be the most advanced, but their high cost and poor stability severely hamper their large-scale practical application. Therefore, there is a strong need to design advanced non-noble metal based materials to reduce the barrier of the OER process.
For decades, researchers have developed numerous transition metal-based catalysts, of which cobalt-based selenides have received much attention due to their advantages of inherently high electrical conductivity, rapid charge transfer properties, and good catalytic activity. It is known that by metal doping or compounding with low dimensional materials (such as carbon nanotubes, graphene, MXene), the electronic structure can be modulated and more active sites can be exposed, thereby significantly improving the OER activity. However, the transition metal-based material is not ideal for maintaining the durability of the OER for a long time because it is in direct contact with the corrosive electrolyte.
Disclosure of Invention
The invention aims to provide a limited-domain Fe-doped CoSe 2 A/MXene composite material and a preparation method and application thereof.
The invention provides a limited-domain Fe-doped CoSe 2 The preparation method of the/MXene composite material specifically comprises the following steps:
(1) adding Zn (NO) 3 ) 2 And Co (NO) 3 ) 2 Sequentially mixing the methanol solution, the methanol solution of 2-methylimidazole and the water/methanol mixed solution of MXene, stirring for reaction, washing and drying after the reaction to obtain ZIFs/MXene (namely the zeolite imidazole framework compound/MXene) powder;
(2) will K 3 [Fe(CN) 6 ]The aqueous solution is mixed with an ethanol solution of ZIFs/MXene, stirred for reaction, and after the reaction, precipitate is separated, washed and dried to obtain [ ZIFs @ PBA ]]/MXene (i.e. [ Zeolite imidazole framework compound @ Prussian blue)]MXene) powder;
(3) will [ ZIFs @ PBA]/MXene in H 2 Carrying out high-temperature annealing treatment in the atmosphere of mixed gas of Ar to obtain FeCo @ PNC/MXene (namely a porous nitrogen-doped carbon layer limited-area FeCo metal/MXene sandwich composite structure) powder;
(4) FeCo @ PNC/MXene and elemental selenium powder are respectively placed at two separation positions in a tube furnace, the selenium powder is positioned at the upstream, the FeCo @ PNC/MXene is positioned in an intermediate heating zone, and H is continuously introduced from the upstream 2 And carrying out high-temperature selenization treatment on the mixed gas of Ar to obtain the limited-area Fe-doped CoSe 2 /MXene composite (i.e. Fe-CoSe) 2 @PNC/MXene）。
Preferably, the MXene is Ti 3 C 2 T x 。
Preferably, the Zn (NO) 3 ) 2 And Co (NO) 3 ) 2 Zn (NO) in methanol solution of (2) 3 ) 2 Has a mass concentration of 10 to 30 mg/mL –1 ，Co(NO 3 ) 2 Has a mass concentration of 10 to 30 mg/mL –1 (ii) a The mass concentration of the methanol solution of the 2-methylimidazole is 30-50 mg/mL –1 (ii) a The mass concentration of the MXene water/methanol mixed solution is 1-3 mg/mL –1 。
Preferably, said K 3 [Fe(CN) 6 ]The mass concentration of the aqueous solution of (3) is 4 to 6 mg/mL –1 。
Preferably, the high-temperature annealing treatment is to keep the temperature of the alloy at 700-900 ℃ for 1-3 h and then cool the alloy to room temperature.
Preferably, the high-temperature selenization treatment is performed at 400-500 ℃ for 0.5-1.5 h.
Preferably, said H 2 H in mixed gas with Ar 2 And Ar in a volume ratio of 1: 9.
The invention provides a limited-domain Fe-doped CoSe 2 the/MXene composite material is prepared by the method. The confinement type Fe-doped CoSe 2 the/MXene composite material has a sandwich structure, can be used as an electrolytic water catalyst and is used for electrocatalytic oxygen evolution reaction.
The invention has the advantages and beneficial effects that: (1) a unique multi-dimensional heterostructure construction strategy is provided, and double MOFs are loaded on two sides of a two-dimensional MXene nanosheet, so that the two-dimensional MXene nanosheet is carbonized and selenized to form a limited-domain Fe-doped CoSe 2 the/MXene sandwich structure composite material has simple operation and strong repeatability; (2) based on limited-area type Fe doped CoSe 2 The design of the/MXene sandwich structure can efficiently modulate an electronic structure, enhance charge transfer and improve an active site; (3) the resulting Fe-CoSe 2 The @ PNC/MXene material can reduce the potential barrier of the OER process, shows super-strong OER performance and can obtain the current density of 10 mA-cm –2 Only the over-potential is 244 mV and the Tafel slope is only 41.1 mV dec –1 (ii) a (4) The method combines the multidimensional heterostructure and the metal element doping to synergistically enhance the OER process, and has wide prospects in the fields of designing efficient and low-cost electrocatalysts, promoting the practical application of electrocatalysis systems and the like.
Drawings
FIG. 1 is a confined Fe doped CoSe of example 1 2 XRD pattern of/MXene composite material. By comparison with a standard card, it was confirmed that the resulting composite material contained orthorhombic CoSe 2 Crystalline phase, whereas doped Fe element, amorphous carbon and a small amount of MXene were not detectable by XRD instrument.
FIG. 2 is the confined type Fe doped CoSe of example 1 2 EDX-Mapping diagram of/MXene composite material. This analysis reveals a relatively uniform distribution of elements such as Ti, N and C in the composite, while the Co, Se and Fe elements are mainly concentrated in the central confinement region.
FIG. 3 is the confined type Fe doped CoSe of example 1 2 /MXene compositeSEM image of material. The material presents a two-dimensional composite structure, and the surface of the material is rich in rough porous and nanoparticle structures.
FIG. 4 is a confined Fe doped CoSe of example 1 2 TEM image of/MXene composite. The picture shows that "gauze" -shaped two-dimensional MXene is observed, and rich spherical Fe-CoSe is obtained 2 The grain structure is coated by a porous nitrogen-doped carbon layer in a limited domain mode, and the grain structure is uniformly attached to MXene to form the multi-dimensional heterogeneous Fe-CoSe 2 @ PNC/MXene composite material.
FIG. 5 is the confined Fe doped CoSe of example 2 2 the/MXene composite material is used as an electrocatalyst and has a linear sweep voltammetry polarization curve in 1M KOH. Tests show that the limited-domain type Fe is doped with CoSe 2 the/MXene composite material has excellent OER electrocatalytic activity and generates 10 mA-cm –2 The reference current density (equivalent to the current density produced by a 12.3% efficient solar water splitting plant) requires only 244 mV overpotential.
FIG. 6 is the confined Fe doped CoSe of example 2 2 the/MXene composite material is used as an electrocatalyst, and a Tafel slope curve is fitted by a polarization curve. In-picture confined-type Fe-doped CoSe 2 The Tafel slope of the/MXene composite material is only 41.1 mV dec –1 The very low slope indicates that the composite demonstrates the highly efficient reaction kinetic efficiency of the composite.
FIG. 7 is the confined Fe doped CoSe of example 2 2 The constant 10 mA cm of the/MXene composite material as the electrocatalyst –2 The chronopotentiometric curve was tested for 20 h at current density. The test shows that the composite material still has stable potential without obvious rising after 20 hours of OER test.
FIG. 8 is the confined type Fe doped CoSe of example 2 2 SEM image of/MXene composite as electrocatalyst after 20 h chronopotentiometric stability test. The picture shows that the shape of the composite material after stability test is not obviously changed, which shows that the material not only has excellent catalytic activity, but also has good structural and performance stability in the OER test process.
Detailed Description
The nano confinement structure can not only prevent the inner active material from being corroded by electrolyte, but also improve the catalytic activity by virtue of the electron penetration; the heterogeneous metal atoms are doped with the inner active material, so that the electronic structure can be modulated and the activity of reaction sites can be enhanced; the support of the two-dimensional MXene material avoids the aggregation of nano-confinement particles and ensures the rapid transmission of ions/electrons. The advantages of the three are combined with CoSe 2 Combined, a porous nitrogen-doped carbon layer is utilized, and a limited-area Fe element is doped with CoSe 2 Particles of Ti in two dimensions simultaneously 3 C 2 T x The MXene is used as a carrier, so that the doped nano confinement structure is uniformly distributed on two sides of the MXene to form a sandwich structure, and the oxygen evolution electrocatalytic activity and stability of the catalyst are comprehensively improved by combining the MXene and the nano confinement structure.
Based on the above, the invention provides a limited-domain Fe-doped CoSe 2 The preparation method of the/MXene composite material specifically comprises the following steps:
(1) zn (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving O in methanol under stirring; dissolving 2-methylimidazole in methanol under stirring; mixing MXene (i.e. Ti) 3 C 2 T x ) Ultrasonic mixing of the water solution and methanol; then, stirring and mixing the three solutions in sequence in a certain order, and continuously stirring for reaction; centrifugally cleaning by using a water/methanol mixed solution, re-dispersing in deionized water, and carrying out vacuum freeze drying to obtain ZIFs/MXene (namely a zeolite imidazole framework compound/MXene) powder;
(2) will K 3 [Fe(CN) 6 ]Dropwise adding the aqueous solution into ethanol containing ZIFs/MXene, continuously stirring for reaction, centrifugally cleaning and precipitating by using a water/ethanol mixed solvent, and carrying out vacuum freeze drying to obtain [ ZIFs @ PBA]/MXene (i.e. [ Zeolite imidazole framework compound @ Prussian blue)]MXene) powder;
(3) will contain [ ZIFs @ PBA]The ceramic boat of/MXene is put into a quartz tube furnace, and H is continuously introduced 2 Performing high-temperature annealing treatment in a/Ar mixed atmosphere by setting a temperature program, and naturally cooling to obtain FeCo @ PNC/MXene (namely porous nitrogen-doped carbon layer confinement FeCo metal/MXene sandwich composite structure) powder；
(4) FeCo @ PNC/MXene and elemental selenium powder are respectively placed at two separation positions in a quartz tube furnace, the selenium powder is positioned at the upstream, the FeCo @ PNC/MXene is positioned in an intermediate heating zone, and H is continuously introduced 2 Performing high-temperature selenization treatment in a temperature program under the/Ar mixed atmosphere to obtain the limited-range Fe-doped CoSe 2 /MXene composite (i.e. Fe-CoSe) 2 @PNC/MXene）。
Wherein, the operation procedures of stirring and mixing the three solutions in a certain sequence are as follows: the metal salt methanol solution is poured quickly into the stirred 2-methylimidazole methanol solution for 10 s and then into the water/methanol mixed solution containing MXene. Said Zn (NO) 3 ) 2 And Co (NO) 3 ) 2 Zn (NO) in methanol solution of (2) 3 ) 2 Has a mass concentration of 10 to 30 mg/mL –1 ，Co(NO 3 ) 2 Has a mass concentration of 10 to 30 mg/mL –1 The dosage can be 12 mL; the mass concentration of the methanol solution of the 2-methylimidazole is 30-50 mg/mL –1 The dosage can be 20 mL; the mass concentration of the MXene water/methanol mixed solution is 1-3 mg/mL –1 The amount may be 8 mL. Said K 3 [Fe(CN) 6 ]The volume of the aqueous solution is 3-5 mL, and the mass concentration is 4-6 mg/mL –1 . The mass ratio of FeCo @ PNC/MXene to elemental selenium powder is 1: 20. The parameters of the high-temperature annealing treatment carried out by the set temperature program are as follows: at 2 ℃ min –1 Raising the temperature from room temperature to 700-900 ℃, and then keeping for 1-3 h. The parameters of the set temperature program for high-temperature selenization treatment are as follows: at 5 ℃ min –1 Raising the temperature from room temperature to 400-500 ℃, and then keeping for 0.5-1.5 h.
The invention is further illustrated by the following examples.
The morphology and structure of the product of the invention are determined by a field emission Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM); its crystalline phase is determined by X-ray diffractometry (XRD); the element composition is measured by imaging (EDX-mapping) of an energy dispersion X-ray spectrometer matched with the TEM; the electrocatalytic oxygen evolution reaction performance of the product is measured on the Shanghai Chenghua electrochemical workstation.
Example 1: preparation of confined Fe-doped CoSe 2 /MXene composite material
The confined-Fe-doped CoSe in this example 2 The preparation process and the steps of the/MXene composite material are as follows:
(1) 0.183 g of Zn (NO) 3 ) 2 ·6H 2 O and 0.183 g Co (NO) 3 ) 2 ·6H 2 Dissolving O in 12 mL of methanol under stirring; 0.811 g of 2-methylimidazole was dissolved in 20mL of methanol with stirring; 1.6 mL of 10 mg. multidot.mL –1 MXene (i.e. Ti) 3 C 2 T x ) Ultrasonically mixing the aqueous solution with 6.4 mL of methanol; then, quickly pouring a metal salt methanol solution into the stirred 2-methylimidazole methanol solution for 10 seconds, quickly pouring a water/methanol mixed solution containing MXene, and continuously stirring for reacting for 3 hours; centrifugally cleaning with a water/methanol mixed solution (volume ratio of 1: 24) for 3 times, re-dispersing in 20mL of deionized water, and carrying out vacuum freeze drying for 24 h to obtain zeolite imidazole framework compound/MXene (ZIFs/MXene) powder;
(2) 4 mL of 5 mg/mL –1 Concentration of K 3 [Fe(CN) 6 ]Dropwise adding the aqueous solution into 36 mL of ethanol containing 40 mg of ZIFs/MXene, continuously stirring for reaction for 2 h, centrifugally cleaning and precipitating for 6 times by using a water/ethanol mixed solvent, and carrying out vacuum freeze drying for 24 h to obtain the [ zeolite imidazole framework compound @ Prussian blue]/MXene (i.e., [ ZIFs @ PBA)]MXene) powder;
(3) will contain 100 mg of [ ZIFs @ PBA ]]The ceramic boat of/MXene is put into a quartz tube furnace, and H is continuously introduced 2 (10%)/Ar (90%) mixed atmosphere, setting a temperature program and carrying out high-temperature annealing treatment parameters as follows: at 2 ℃ min –1 Raising the temperature from room temperature to 800 ℃, then keeping the temperature for 2 hours, and naturally cooling to obtain the powder with the porous nitrogen-doped carbon layer confinement FeCo metal/MXene sandwich composite structure (namely FeCo @ PNC/MXene);
(4) FeCo @ PNC/MXene and elemental selenium powder with the mass ratio of 1:20 are weighed and respectively placed at two separation positions in a quartz tube furnace, the selenium powder is positioned at the upstream, the FeCo @ PNC/MXene is positioned in an intermediate heating zone, and H is continuously introduced 2 A mixed atmosphere of (10%)/Ar (90%), and a temperature program is set for the operationThe parameters of the high-temperature selenization treatment are as follows: at 5 ℃ min –1 The temperature is raised from room temperature to 450 ℃ at the speed, and then the temperature is kept for 1 h, thus obtaining the limited-area Fe-doped CoSe 2 /MXene composite (i.e. Fe-CoSe) 2 @PNC/MXene）。
Example 2: confined-Fe-doped CoSe 2 Performance testing of/MXene composite materials
confined-Fe-doped CoSe 2 The performance of the/MXene composite material as the catalyst for the electrolytic water oxygen evolution reaction is tested:
(1) preparing an electrocatalyst working electrode:
weighing 5 mg of confinement type Fe-doped CoSe 2 Adding the/MXene composite material powder into 1 ml of mixed solution (comprising 40 mul of 5 wt% nafion solution and 960 mul of ethanol), and performing ultrasonic treatment for 30 min to form relatively uniform ink-shaped catalyst dispersion liquid; and (3) dripping 8 mul of dispersion liquid on the surface of a glassy carbon electrode with the diameter of 3 mm for 5 times by using a liquid transfer gun, and carrying out an electrochemical performance test after the surface of the electrode is naturally dried.
(2) Electrochemical performance study:
using the prepared electrocatalyst working electrode, electrochemical characteristics were tested on CHI 760E electrochemical workstation (Chenhua apparatus, Shanghai, China), using 1 mol. L –1 Aqueous KOH was used as the electrolyte for OER testing. A standard three-electrode system, namely a graphite electrode as a counter electrode, a Saturated Calomel Electrode (SCE) as a reference electrode and a prepared electrocatalyst modified glassy carbon electrode as a working electrode, is adopted. The potentials in the test were each converted to a reversible hydrogen electrode potential according to the Nernst equation (E RHE ) Will beE RHE Subtracting 1.23V to obtain the overpotentialη. The linear volt-ampere scanning technology is adopted to carry out the polarization curve test, and the scanning speed is 2 mV –1 (ii) a Based onE RHE And log | Current Density: (j, mA cm –2 ) Linear regression between | can calculate the tafel slope from the polarization curve data; adopting a timing potential testing technology to carry out 10 mA cm of prepared electrocatalyst working electrode –2 And (5) testing the stability under constant current density.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. Limited-domain Fe-doped CoSe 2 The preparation method of the/MXene composite material specifically comprises the following steps:
(1) adding Zn (NO) 3 ) 2 And Co (NO) 3 ) 2 Sequentially mixing the methanol solution, the methanol solution of 2-methylimidazole and the water/methanol mixed solution of MXene, stirring for reaction, washing and drying after the reaction to obtain ZIFs/MXene powder;
(2) will K 3 [Fe(CN) 6 ]The aqueous solution is mixed with an ethanol solution of ZIFs/MXene, stirred for reaction, and after the reaction, precipitate is separated, washed and dried to obtain [ ZIFs @ PBA ]]MXene powder;
(3) will [ ZIFs @ PBA]/MXene in H 2 Carrying out high-temperature annealing treatment in the atmosphere of mixed gas of Ar to obtain FeCo @ PNC/MXene powder;
(4) FeCo @ PNC/MXene and elemental selenium powder are respectively placed at two separation positions in a tube furnace, the selenium powder is positioned at the upstream, the FeCo @ PNC/MXene is positioned in an intermediate heating zone, and H is continuously introduced from the upstream 2 And carrying out high-temperature selenization treatment on the mixed gas of Ar to obtain the limited-area Fe-doped CoSe 2 the/MXene composite material.
2. The method of claim 1, wherein the MXene is Ti 3 C 2 T x 。
3. Method according to claim 1, characterized in that said Zn (NO) 3 ) 2 And Co (NO) 3 ) 2 Zn (NO) in methanol solution of (2) 3 ) 2 Has a mass concentration of 10 to 30 mg/mL –1 ，Co(NO 3 ) 2 Has a mass concentration of 10 to 30 mg/mL –1 (ii) a The 2-methylimidazoleThe methanol solution (2) has a mass concentration of 30 to 50 mg/mL –1 (ii) a The mass concentration of the MXene water/methanol mixed solution is 1-3 mg/mL –1 。
4. The method of claim 1, wherein K is 3 [Fe(CN) 6 ]The mass concentration of the aqueous solution of (3) is 4 to 6 mg/mL –1 。
5. The method of claim 1, wherein the high temperature annealing treatment is performed by maintaining at 700-900 ℃ for 1-3 hours and then cooling to room temperature.
6. The method of claim 1, wherein the high temperature selenization process is performed at 400-500 ℃ for 0.5-1.5 h.
7. The method of claim 1, wherein the H is 2 H in mixed gas with Ar 2 And Ar in a volume ratio of 1: 9.
8. The confined-domain Fe-doped CoSe obtained by the method of any one of claims 1 to 7 2 the/MXene composite material.
9. The confined-domain Fe-doped CoSe of claim 8 2 The application of the/MXene composite material as a water electrolysis catalyst.
10. The use of claim 9, wherein the confined-Fe doped CoSe 2 the/MXene composite material is used for electrocatalytic oxygen evolution reaction.
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