CN113737216B - FeSe/FeSe 2 Nano flower heterojunction catalyst and preparation method and application thereof - Google Patents
FeSe/FeSe 2 Nano flower heterojunction catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a FeSe/FeSe 2 The preparation method of the nanoflower heterojunction catalyst comprises the following steps: s101, dissolving selenium powder in an organic solvent under an inert atmosphere, uniformly mixing, then dropwise adding pentacarbonyl iron, and uniformly mixing at room temperature to obtain a reddish brown mixed solution; s102, placing the reddish brown mixed solution into a high-pressure reaction kettle to fully react at 100-250 ℃ to obtain a mixture; s103, after the high-pressure reaction kettle after the reaction is cooled to room temperature, centrifuging the mixture to obtain a black precipitate; purifying the black precipitate to obtain the final product. The invention also provides FeSe/FeSe 2 The nanometer flower heterojunction catalyst and the application thereof. The invention obtains the nano flower cluster FeSe/FeSe with controllable shape, uniform size and high specific surface area by regulating and controlling the feeding ratio of the selenium powder and the iron source precursor before the reaction 2 A nanoflower heterojunction catalyst.
Description
Technical Field
The invention relates to the technical field of electrocatalytic materials, in particular to FeSe/FeSe 2 A preparation method and application of a nano flower heterojunction catalyst.
Background
The massive combustion of traditional fossil fuels makes environmental pollution more serious, so that people search for other renewable energy sources. Oxygen is considered to be one of the most potential clean energy sources in the 21 st century. However, at present, more than 90% of oxygen energy is obtained by industrial cooling and liquefying, and water splitting is a low-cost and environment-friendly oxygen obtaining mode from the aspects of cleaning and sustainable development. In general, electrolysis of water involves two half reactions. 1) Oxidation of water and 2) proton reduction. The upper half of the reaction is generally considered to be an inherent slow kinetics of OER, a key bottleneck in the development of efficient electrolysis of water. Therefore, the development of highly efficient electrocatalysts for OER is highly desirable and has attracted worldwide attention in recent years. To date, irO 2 And RuO (Ruo) 2 Are generally considered to be the most industrially effective OER catalysts. Therefore, it is important to design and develop OER electrocatalysts with high abundance, low cost and high durability to enhance catalytic performance.
In recent years, by continuous research on electrocatalyst materials, moS-based 2 、FeSe 2 And transition metal based dihalides (LTMDs) of FeSe have become alternatives to noble metal catalysts. FeSe and FeSe 2 All have special structures, are favorable for electron transfer and can provide more active sites for OER processes. Through composition control, the heterojunction structure of the iron selenide and the ferrous selenide shows excellent water splitting catalysis performance.
In recent years, along with development of technology, iron-based catalysts are increasingly widely applied in the fields of electrocatalytic decomposition of water and the like, and the prior art discloses that the rate can be remarkably improved when ferrous selenide nano materials are used as oxygen evolution materials, and also discloses that the catalytic performance of Oxygen Evolution Reaction (OER) can be remarkably enhanced when iron selenide grows on nanotubes in a layered mode. Related applicability tests of the heterojunction formed by two substances also appear successively, and the heterojunction is reported to be capable of effectively accelerating oxygen evolution reaction under alkaline conditions, so that low-cost and high-efficiency electrochemical oxygen evolution catalysts can be produced by extension. In the Chinese patent application with application number 202010177065.9, a heterojunction of ferrous selenide/ferric oxide nano-particles is disclosed, and the preparation method is specifically disclosed as follows: feSe prepared 2 /Fe 2 O 3 Nanoparticle heterojunction will FeSe 2 The nano particles are oxidized in air at high temperature to obtain FeSe 2 /Fe 2 O 3 A nanoparticle heterojunction; the high-temperature oxidation temperature is 250-300 ℃ and the time is 1-3 hours to finally form FeSe 2 /Fe 2 O 3 Nanoparticle heterojunction. The nanoparticle heterojunction prepared by the patent needs a complex preparation process, needs to be divided into multiple steps, and is difficult to ensure the consistency of the product quality in large-scale production. Although there are many heterojunction studies in the prior art, feSe is not yet known 2 And research on FeSe heterojunction, feSe has a specific FeSe in some aspects 2 More outstanding characteristics, feSe and the catalytic properties of the heterostructure are worth going deep. Nor is it true for FeSe 2 And the related disclosure of the quality of the electrocatalytic performance of FeSe heterojunction.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a FeSe/FeSe 2 A preparation method and application of a nano flower heterojunction catalyst.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the invention firstly provides a FeSe/FeSe 2 The preparation method of the nanoflower heterojunction catalyst comprises the following steps:
s101, dissolving selenium powder in an organic solvent under an inert atmosphere, uniformly mixing, then dropwise adding pentacarbonyl iron, and uniformly mixing at room temperature to obtain a reddish brown mixed solution;
s102, placing the reddish brown mixed solution into a high-pressure reaction kettle to fully react at 100-250 ℃ to obtain a mixture; preferably, the reddish brown mixed liquor is fully reacted for 10-24 hours.
S103, after the high-pressure reaction kettle after the reaction is cooled to room temperature, centrifuging the mixture, and taking a precipitation part to obtain a black precipitate; purifying the black precipitate to obtain FeSe/FeSe 2 A nanoflower heterojunction catalyst.
In one embodiment according to the present invention, in step S101, the ratio of selenium powder, iron pentacarbonyl and organic solvent is 0.1 to 5 in g/mL: 10:30-100;
preferably 0.3 to 0.75 to 35.
In one embodiment according to the invention, in S101, the inert atmosphere is achieved by introducing one of nitrogen, xenon, neon, helium, argon or krypton into the operating environment.
In one embodiment according to the invention, in S102, the purification treatment is achieved by a method comprising the steps of: and carrying out ultrasonic treatment on the black precipitate, then sequentially washing with acetone and water for a plurality of times, and finally drying.
In one embodiment according to the present invention, in S103, the drying process is drying or freeze-drying with a vacuum dryer.
In one embodiment according to the invention, in S103, the centrifugation speed is 10000r/min and the centrifugation time is 10min.
The invention also provides FeSe/FeSe prepared by the preparation method 2 A nanoflower heterojunction catalyst.
Preferably, the FeSe/FeSe 2 FeSe in nanoflower heterojunction catalyst 2 The molar ratio to FeSe is 1:1.
the invention further provides the FeSe/FeSe 2 The application of the nanoflower heterojunction catalyst in the electrochemical reaction of catalyzing and decomposing water to separate oxygen.
In another aspect, the invention also provides an oxygen evolution electrode for a fuel cell, comprising the FeSe/FeSe 2 A nanoflower heterojunction catalyst.
The technical scheme of the invention has the following beneficial effects:
the invention uses the organic reagent as the solvent, and obtains the nano flower cluster FeSe/FeSe with controllable morphology, uniform size and high specific surface area by regulating and controlling the feeding ratio of the selenium powder and the iron source precursor before the reaction 2 The nano flower heterojunction catalyst is expected to play an important role in a wider emerging field, such as the field of electrocatalysis.
The invention is simple solvothermal synthesis of FeSe/FeSe 2 Dissolving selenium powder in an organic solvent, stirring for a plurality of minutes, adding pentacarbonyl iron, performing solvothermal reaction, and centrifugally washing the obtained product to obtain black precipitate, namely FeSe/FeSe 2 A nanoflower catalyst. The invention can obtain FeSe/FeSe through one-pot solvothermal reaction 2 The nano flower heterojunction catalyst simplifies the preparation process, provides a large number of active sites for the catalytic reaction due to the unique morphology, ensures the rapid transmission of electrons and ions, and ensures the rapid release of generated oxygen bubbles, thus having low cost and simple operation.
The FeSe/FeSe provided by the invention 2 Nanoflower catalyst and preparation method thereofIs expected to play an important role in a wider emerging field.
Drawings
FIG. 1 shows FeSe/FeSe according to an embodiment of the present invention 2 A preparation method flow chart of the nano flower heterojunction catalyst.
FIG. 2 is a schematic illustration of FeSe/FeSe prepared in example 1 according to an embodiment of the present invention 2 Scanning Electron Microscope (SEM) map of the nanoflower heterojunction catalyst, and the sample is in the shape of nanoflower.
FIG. 3 is a sample of FeSe/FeSe of different proportions prepared in example 1 provided in the examples of the present invention 2 SEM (scanning electron microscope) spectrum of the nano flower heterojunction catalyst and controllable sample morphology.
Fig. 4 is a scanning electron microscope mapping (SEM mapping) chart provided in example 1 of the present invention, and it can be seen that the two elements are uniformly distributed.
FIG. 5 is a FeSe/FeSe prepared in example 1 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst.
FIG. 6 is a FeSe/FeSe prepared in example 2 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst.
FIG. 7 is a FeSe/FeSe prepared in example 3 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst.
FIG. 8 is a FeSe/FeSe prepared in example 4 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst.
FIG. 9 is a FeSe/FeSe prepared in example 5 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
The invention provides a FeSe/FeSe 2 The invention relates to a preparation method and application of a nano flower heterojunction catalyst, and the preparation method and application are described in detail below with reference to the accompanying drawings.
As shown in FIG. 1, the FeSe/FeSe provided by the invention 2 The preparation method of the nanoflower heterojunction catalyst comprises the following steps:
s101: dissolving selenium powder in an organic solvent under an inert atmosphere, stirring for a plurality of minutes, and dropwise adding pentacarbonyl iron;
s102: continuously stirring the mixture at room temperature for a period of time, transferring the mixture into a stainless steel high-pressure reaction kettle, putting the reaction kettle into an oven, preserving heat for a period of time, and cooling;
s103: after the reaction kettle is cooled to room temperature, performing centrifugal washing on the mixture to obtain black precipitate, and performing ultrasonic treatment and washing for a plurality of times by adopting deionized water and acetone; drying in a freeze dryer to obtain FeSe/FeSe 2 A nanoflower heterojunction catalyst.
In a preferred embodiment of the present invention, the organic solvent is selected from any one of toluene, para-xylene or azomethine formamide.
In a preferred embodiment of the invention, wherein during the centrifugation and collection in the third step, the centrifugation speed is 3000-12000r/min and the centrifugation time is 1-10min.
In a preferred embodiment of the present invention, wherein the magnetic stirring speed in the first step is 7000-10000r/min.
The FeSe/FeSe provided by the invention 2 The preparation method of the nanoflower heterojunction catalyst can also be implemented by other steps by one of ordinary skill in the art, and the FeSe/FeSe provided by the invention of the figure 1 2 The preparation method of the nanoflower heterojunction catalyst is only one specific example.
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1: preparation of FeSe/FeSe according to the invention 2 Nano flower heterojunction catalyst
First, 0.30g of selenium powder was dissolved in three portions of 35mL of organic solvent under nitrogen protection, respectively, and stirred well. Then 0.50mL, 0.75mL and 1.00mL of iron pentacarbonyl are added dropwise under nitrogen protection. Then, the mixture was rapidly magnetically stirred at room temperature for 20min, and then the mixture was transferred to a stainless steel autoclave, and the autoclave was placed in an oven at 230 ℃ and maintained for 24h; finally, after the temperature of the high-pressure reaction kettle is cooled to room temperature, centrifugally washing the mixture to obtain black precipitate, carrying out ultrasonic dispersion treatment on the black precipitate, adopting deionized water and acetone to wash for a plurality of times alternately, and finally centrifugally collecting, and drying in a vacuum freeze dryer for 2h to obtain a black product.
The properties of the obtained end product were observed, as shown in particular in fig. 2, 3 and 4.
FIG. 2 is a schematic illustration of FeSe/FeSe prepared in example 1 according to an embodiment of the present invention 2 Scanning Electron Microscope (SEM) map of the nanoflower heterojunction catalyst, and the sample is in the shape of nanoflower.
FIG. 3 is a sample of FeSe/FeSe of different proportions prepared in example 1 provided in the examples of the present invention 2 As can be seen from a Scanning Electron Microscope (SEM) map of the nanoflower heterojunction catalyst, the method obtains the nanoflower cluster FeSe/FeSe with controllable morphology, uniform size and high specific surface area by regulating and controlling the feeding ratio of the selenium powder and the iron source precursor before the reaction as shown in FIG. 3 2 A nanoflower heterojunction catalyst.
Fig. 4 is a scanning electron microscope mapping (SEM mapping) chart provided in example 1 of the present invention, and it can be seen that the two elements are uniformly distributed.
Example 2: the FeSe/FeSe provided by the embodiment of the invention 2 The nanoflower heterojunction catalyst comprises the following steps:
first, 0.15g of selenium powder was dissolved in three portions of 35mL of organic solvent under nitrogen protection, and stirred well. Then 0.50mL, 0.75mL and 1.00mL of iron pentacarbonyl are added dropwise under nitrogen protection. Then, the mixture was rapidly magnetically stirred at room temperature for 20min, and then the mixture was transferred to a stainless steel autoclave, and the autoclave was placed in an oven at 230 ℃ and maintained for 24h; finally, after the temperature of the high-pressure reaction kettle is cooled to room temperature, centrifugally washing the mixture to obtain black precipitate, carrying out ultrasonic dispersion treatment on the black precipitate, adopting deionized water and acetone to wash for a plurality of times alternately, and finally centrifugally collecting, and drying in a vacuum freeze dryer for 2h to obtain a black product.
Example 3: the FeSe/FeSe provided by the embodiment of the invention 2 Nano flower heterojunction catalyst
First, 0.60g of selenium powder was dissolved in three portions of 35mL of organic solvent under nitrogen protection, and stirred well. Then 0.50mL, 0.75mL and 1.00mL of iron pentacarbonyl are added dropwise under nitrogen protection. Then, the mixture was rapidly magnetically stirred at room temperature for 20min, and then the mixture was transferred to a stainless steel autoclave, and the autoclave was placed in an oven at 230 ℃ and maintained for 24h; finally, after the temperature of the high-pressure reaction kettle is cooled to room temperature, centrifugally washing the mixture to obtain black precipitate, carrying out ultrasonic dispersion treatment on the black precipitate, adopting deionized water and acetone to wash for a plurality of times alternately, and finally centrifugally collecting, and drying in a vacuum freeze dryer for 2h to obtain a black product.
Example 4: the FeSe/FeSe provided by the embodiment of the invention 2 Nano flower heterojunction catalyst
First, 0.30g of selenium powder was dissolved in three portions of 35mL of organic solvent under nitrogen protection, respectively, and stirred well. Then 0.50mL, 0.75mL and 1.00mL of iron pentacarbonyl are added dropwise under nitrogen protection. Then, the mixture is quickly stirred magnetically for 20min at room temperature, and then the mixture is transferred into a stainless steel high-pressure reaction kettle, and the high-pressure reaction kettle is put into a baking oven at 250 ℃ and kept for 24h; finally, after the temperature of the high-pressure reaction kettle is cooled to room temperature, centrifugally washing the mixture to obtain black precipitate, carrying out ultrasonic dispersion treatment on the black precipitate, adopting deionized water and acetone to wash for a plurality of times alternately, and finally centrifugally collecting, and drying in a vacuum freeze dryer for 2h to obtain a black product.
Example 5: the FeSe/FeSe provided by the embodiment of the invention 2 Nano flower heterojunction catalyst
First, 0.30g of selenium powder was dissolved in three portions of 35mL of organic solvent under nitrogen protection, and stirred well. Then 0.50mL, 0.75mL and 1.00mL of iron pentacarbonyl are added dropwise under nitrogen protection. Then, the mixture is rapidly stirred magnetically for 20min at room temperature, and then the mixture is transferred into a stainless steel high-pressure reaction kettle, and the high-pressure reaction kettle is put into a 180 ℃ oven and kept for 24h; finally, after the temperature of the high-pressure reaction kettle is cooled to room temperature, centrifugally washing the mixture to obtain black precipitate, carrying out ultrasonic dispersion treatment on the black precipitate, adopting deionized water and acetone to wash for a plurality of times alternately, and finally centrifugally collecting, and drying in a vacuum freeze dryer for 2h to obtain a black product.
Example 6: performance testing
Electrochemical testing of all samples was performed in 1.0m koh at room temperature using an electrochemical workstation with a standard three electrode system. Working electrode on Carbon Fiber Paper (CFP) is made of FeSe/FeSe 2 The catalyst is prepared. To a mixture of 750 μl deionized water and 250 μl ethanol and 40 μl ethanol in solution (5 wt%) was added 5mg of sample catalyst and 5mg of carbon powder, followed by sonication for 40 minutes to obtain a uniform suspension. Then 70 mu LFASe/FeSe is added 2 The catalyst was dropped onto a clean CFP sheet (1 cm). Calibration is performed with reference to the reference and is converted to a reversible oxygen electrode (RHE) by the formula.
E RHE ＝E (Hg/HgO) +0.89
The three electrode system was bubbled with high purity nitrogen for 30 minutes prior to each OER test. To explore OER activity, linear sweep voltammetry testing was performed at a rate of 5mV/s at a sweep rate of 0V to 1.8V. Electrochemical Impedance Spectroscopy (EIS) measurements were obtained at a frequency range of 0.01 to 105Hz and fitted by Zview software. An Hg/HgO electrode in 1M KOH aqueous solution was used as a reference electrode.
The heterojunction catalysts prepared in examples 1-5 were tested for performance according to the methods described above, respectively, as shown in fig. 5-9.
FIG. 5 is a FeSe/FeSe prepared in example 1 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst. Comparison shows that FeSe/FeSe at the same current density 2 The overpotential of =1:1 is the smallest and performs best.
FIG. 6 is a FeSe/FeSe prepared in example 2 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst. Also by comparison, it was found that FeSe: feSe at the same current density 2 The overpotential of =1:1 is the smallest and performs best.
FIG. 7 is a FeSe/FeSe prepared in example 3 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst. Also by comparison, it was found that FeSe: feSe at the same current density 2 The overpotential of =1:1 is the smallest and performs best.
FIG. 8 is a FeSe/FeSe prepared in example 4 according to an embodiment of the present invention 2 Nanoflower heterojunction catalyst and non-heterojunction FeSe 2 Electrochemical performance of the catalyst and of the non-heterojunction FeSe catalyst. Also by comparison, it was found that FeSe: feSe at the same current density 2 The overpotential of =1:1 is the smallest and performs best.
FIG. 9 is a FeSe/FeSe prepared in example 5 according to an embodiment of the present invention 2 Nanoflower hybrid catalyst and non-hybrid FeSe 2 Electrochemical performance of the catalyst and the non-hybridized FeSe catalyst are compared. Also by comparison, it was found that FeSe: feSe at the same current density 2 The overpotential of =1:1 is the smallest and performs best.
Thus proving that the experimental conditions are changed anyway, feSe: feSe 2 The performance of =1:1 is excellent.
Compared with the prior art, the invention uses selenium powder and iron pentacarbonyl to co-heat in the p-xylene solvent for one stepSynthesis of FeSe/FeSe 2 A nanoflower heterojunction catalyst. The results presented in this invention may provide new opportunities for the discovery of efficient and low cost oxygen evolution reaction electrocatalyst materials.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (10)
1. FeSe/FeSe 2 The preparation method of the nanoflower heterojunction catalyst is characterized by comprising the following steps:
s101, dissolving selenium powder in an organic solvent under an inert atmosphere, uniformly mixing, then dropwise adding pentacarbonyl iron, and uniformly mixing at room temperature to obtain a reddish brown mixed solution;
s102, placing the reddish brown mixed solution into a high-pressure reaction kettle to fully react at 100-250 ℃ to obtain a mixture;
s103, after the high-pressure reaction kettle after the reaction is cooled to room temperature, centrifuging the mixture, and taking a precipitation part to obtain a black precipitate; purifying the black precipitate to obtain FeSe/FeSe 2 A nanoflower heterojunction catalyst.
2. The method according to claim 1, wherein in the step S101, the ratio of selenium powder, iron pentacarbonyl and organic solvent is 0.1 to 5 in g/mL: 10:30-100.
3. The method of claim 1, wherein in S101, the inert atmosphere is achieved by introducing one of nitrogen, xenon, neon, helium, argon, or krypton into the operating environment.
4. The method of claim 1, wherein in S103, the purification treatment is performed by a method comprising the steps of: and carrying out ultrasonic treatment on the black precipitate, then sequentially washing with acetone and water for a plurality of times, and finally drying.
5. The method according to claim 4, wherein in S103, the drying treatment is drying or freeze-drying with a vacuum dryer.
6. The method according to claim 1, wherein in S103, the centrifugal speed is 10000r/min and the centrifugal time is 10min.
7. FeSe/FeSe prepared by the preparation method of any one of claims 1-6 2 A nanoflower heterojunction catalyst.
8. FeSe/FeSe according to claim 7 2 The nano flower heterojunction catalyst is characterized in that FeSe and FeSe 2 The molar ratio of (2) is 1:1.
9. FeSe/FeSe according to claim 7 or 8 2 The application of the nanoflower heterojunction catalyst in the electrochemical reaction of catalyzing and decomposing water to separate oxygen.
10. An oxygen evolution electrode for a fuel cell comprising the FeSe/FeSe according to claim 7 or 8 2 A nanoflower heterojunction catalyst.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977827A (en) * | 2018-08-01 | 2018-12-11 | 兰州大学 | Include FeSe2-Co3O4Composite material and preparation method and catalyst and application |
| CN111320212A (en) * | 2020-03-13 | 2020-06-23 | 西安交通大学 | Ferrous selenide/ferric oxide nanoparticle heterojunction, preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977827A (en) * | 2018-08-01 | 2018-12-11 | 兰州大学 | Include FeSe2-Co3O4Composite material and preparation method and catalyst and application |
| CN111320212A (en) * | 2020-03-13 | 2020-06-23 | 西安交通大学 | Ferrous selenide/ferric oxide nanoparticle heterojunction, preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| Thanh-Tung Le et al..Carbon-Decorated Fe3S4-Fe7Se8 Hetero-Nanowires: Interfacial Engineering for Bifunctional Electrocatalysis Toward Hydrogen and Oxygen Evolution Reactions.《Journal of the Electrochemical Society》.2020,第167卷(第8期),086501. * |
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