CN114622220A - Co3S4Doping SnSxPreparation method and application of heterogeneous nanosheet - Google Patents
Co3S4Doping SnSxPreparation method and application of heterogeneous nanosheet Download PDFInfo
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Abstract
The invention provides a Co3S4Doping SnSxA method of preparing heterogeneous nanoplates comprising the steps of: mixing the Co, Sn-thiourea complex with the dodecylamine solution, heating to 245 ℃ and 250 ℃, and carrying out heat preservation reaction for 50-60min to obtain Co3S4Doping SnSxA heterogeneous nanosheet electrocatalyst. The invention also discloses Co prepared by the preparation method3S4Doping SnSxApplication of the heterogeneous nanosheet as an OER catalyst in a 0.1M KOH alkaline medium. The invention has simple processThe method has the advantages of being novel, efficient, low in cost and the like, and has potential industrial value.
Description
Technical Field
The invention relates to the technical field of electrocatalysts, in particular to Co3S4Doping SnSxA preparation method and application of the heterogeneous nanosheet.
Background
The electrolyzed water can generate clean energy, is a hotspot of energy storage and conversion research, is beneficial to solving the problems of energy crisis and environmental pollution caused by over consumption of fossil fuel, but is restricted by high cost and large reaction energy barrier, and cannot be used on a large scale all the time. The key point is that the OER reaction process is well improved in dynamics, so a high-activity oxygen evolution reaction electrocatalyst is needed to accelerate the reaction.
Currently, noble metal Ru/Ir oxides are still considered to be efficient oxygen evolution catalysts, but the commercial application of electrolytic water technology is seriously hampered by the problems of high cost and low reserves, and therefore, the design of efficient non-noble metal water cracking catalysts has attracted extensive attention. In recent years, the development of catalysts for transition metal compounds and their oxides, sulfides, phosphides, nitrides and carbon nanomaterials, which are abundant, inexpensive, corrosion-resistant and highly active, has been greatly advanced. Among these catalysts, metal sulfide electrocatalysts not only have costLow, high catalytic activity and stable operation, and is approaching or even surpassing RuO in the aspects of oxygen evolution electrocatalytic performance, catalytic durability and the like2、IrO2And the like, and has great application potential.
Among many binary metal sulfides, stannous sulfide has received wide attention due to its advantages such as narrow bandwidth, good optical properties, and non-toxicity. However, it is noteworthy that these catalysts tend to form large particles during the synthesis process, and have poor dispersibility, which inevitably results in a decrease in surface active sites. Most importantly, the catalytic activity of stannous sulfide is much lower than that of commercial catalysts, and therefore, how to optimize the catalytic performance of stannous sulfide is a great challenge.
Literature studies have shown that lattice expansion strategies can alter the intrinsic interatomic distance and thus the lattice spacing, influence the geometry and electronic structure of the active centers, allow the microstructure to be tuned, and ultimately optimize the electrocatalytic activity of the material. For example, Jiang et al demonstrated that lattice strain can enhance the synergy between sulfur vacancies and Ru sites, thereby altering the catalytic performance of the active sites. However, the materials studied are small molecules, the strain generated during the preparation process of the materials is randomly formed, and although the controllable induced lattice expansion is a good method, the research needs to be carried out on how to efficiently and controllably induce the lattice expansion.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides Co3S4Doping SnSxA preparation method of heterogeneous nano-sheets.
The technical scheme adopted by the invention for overcoming the technical problems is as follows: co3S4Doping SnSxThe preparation method of the heterogeneous nanosheet electrocatalyst comprises the following steps: mixing the Co, Sn-thiourea complex with the dodecylamine solution, heating to 245 ℃ and 250 ℃, and carrying out heat preservation reaction for 50-60min to obtain Co3S4Doping SnSxA heterogeneous nanosheet electrocatalyst.
Preferably, the mass volume ratio of the Co, Sn-thiourea complex to the dodecylamine solution is 25 mg: 1 ml.
Preferably, the rate of temperature rise is 4 ℃/min.
Preferably, the product obtained by the incubation reaction is subjected to dispersion sedimentation by using n-heptane and ethanol solution.
Preferably, the volume ratio of the n-heptane to the ethanol solution is 3.5: 1.
preferably, the preparation method of the Co, Sn-thiourea complex comprises the following steps: heating the mixed solution of stannous chloride dihydrate, cobalt chloride hexahydrate, thiourea and deionized water to 110 ℃, and drying after heat preservation reaction to obtain the Co, Sn-thiourea complex.
Preferably, the molar ratio of the cobalt chloride dihydrate to the stannous chloride hexahydrate to the thiourea is 1: 1: 5, the molar volume ratio of the cobalt chloride dihydrate to the deionized water is 1 mmol: 5 ml.
The invention also discloses Co prepared by the preparation method3S4Doping SnSxApplication of the heterogeneous nanosheet as an OER catalyst in a 0.1M KOH alkaline medium.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a Co3S4Doping SnSxThe preparation method of the heterogeneous nanosheet is characterized in that the ratio of cobalt chloride dihydrate to stannous chloride hexahydrate is controlled to be 1: 1, preparing Co and Sn-thiourea complex serving as a precursor, and then directly preparing Co by adopting a one-pot pyrolysis method3S4Doping SnSxHeterogeneous nanosheets in SnSxCo is formed on the surface of the nano sheet3S4Nanosheet layer, and Co3S4Incorporation to cause SnSxLattice expansion is beneficial to the reconstruction and activation of the surface of a Co site, the adsorption free energy of water and oxygen is optimized, and the OER reaction is promoted. In addition, the reserves of Co, Sn and S are rich, and the price of the salts is far lower than that of the salts of noble metals such as Ru, Pt and the like, so that the preparation cost is greatly reduced.
Drawings
FIG. 1 is a comparison graph of the IR spectrum of a Co, Sn-thiourea complex in the example of the present invention.
FIG. 2Is Co in the examples of the invention3S4Doping SnSxAnd (3) heterogeneous nanosheet TEM, HRTEM and Mapping images.
FIG. 3 shows Co, Sn-Thiourea complexes and Co3S4Doping SnSxXRD contrast pattern of heterogeneous nanoplates.
FIG. 4 shows Co in an embodiment of the present invention3S4Doping SnSxXPS plot of heterogeneous nanoplates.
FIG. 5 shows Co, Sn-Thiourea complexes and Co3S4Doping SnSxAnd (3) an electrochemical performance test chart of the heterogeneous nanosheets.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings.
Examples
Co3S4Doping SnSxThe preparation method of the heterogeneous nano-sheet comprises the steps of preparing precursor Co, Sn-thiourea complex and Co3S4Doping SnSxAnd (3) heterogeneous nanosheet.
Step 1: preparation of Co, Sn-Thiourea complexes: at room temperature, sequentially adding 0.2256g of stannous chloride dihydrate, 0.2379g of cobalt chloride hexahydrate, 0.3805g of thiourea and 5ml of deionized water into a dry beaker with the capacity of 100ml to obtain a mixed solution, placing the beaker into an oil bath pot, setting the temperature to be 110 ℃, continuously stirring by using a glass rod during a reaction process, accelerating dissolution and preventing a sample from being condensed on the wall of the beaker, stopping heating when a large amount of solid is separated out and the water is not much, evaporating the residual water by using waste heat, then transferring a product to a culture dish by using a medicine spoon, uniformly spreading, setting the temperature to be 45 ℃, drying for 4h, and grinding the product into powder by using a mortar to obtain light blue precursors of Co and Sn-thiourea complex for analysis and characterization.
The infrared spectrum was characterized as shown in FIG. 1 at 3391.65 and 3300.85cm-1The double peak of (A) is attributed to NH stretching vibration, 1622.81cm-1Is attributed to NH flexural vibration, 1388.64cm-1Peak of (2)Ascribed to C-N stretching vibration, 1096.57cm-1The peak of (A) is attributed to Sn2+,567.74cm-1The peak of (A) is attributed to Co2+And the integral infrared spectrogram is almost consistent with the thiourea standard infrared spectrogram, so that the precursor is inferred to be a Co and Sn-thiourea complex.
Step 2: preparation of Co3S4Doping SnSxHeterogeneous nanosheets: weighing 250mg of the obtained precursor Co, Sn-thiourea complex at room temperature, adding the precursor Co, Sn-thiourea complex into a dry three-neck flask with the capacity of 250ml, then transferring 10ml of dodecylamine solution by using a 10ml rubber head dropper, plugging two sides of the three-neck flask by using glass stoppers, plugging the middle by using a spherical condensation pipe, then placing the three-neck flask into a marmite, raising the temperature to 250 ℃ at the speed of 4 ℃/min under the programmed temperature control, and then carrying out heat preservation reaction for 60 min. After the reaction is finished, naturally cooling the reaction device to 48 ℃, and mixing the components in a volume ratio of 3.5: 1, washing with a mixed solution of n-heptane and absolute ethyl alcohol, and drying the obtained product in a vacuum drying oven at 60 ℃ for 12h to obtain Co3S4Doping SnSxAnd (3) heterogeneous nanosheets for analytical characterization.
As can be seen from the low power TEM of FIGS. 2a and 2b, Co prepared3S4Doping SnSxThe morphology of the heterogeneous nano-sheet is SnSxCo is doped on the nano-sheet substrate3S4Small nanosheet particles, Co can be seen by high resolution TEM of FIG. 2c3S4Doping SnSxThe heterogeneous nano-sheets are mainly made of Co3S4The (311) type crystal plane and the (111) type crystal plane of SnS, the lattice spacing of the normal SnS (111) type crystal plane should be 0.284nm, since Co3S4The lattice of the nano-film is expanded to 0.315nm by doping, and the mapping graph of figure 2d shows that the prepared heterogeneous nano-film mainly comprises three elements of Co, Sn and S, namely Co grows on the SnS nano-film3S4And (3) nano-sheet small particles. The same conclusion is also obtained from the characterization result of XRD powder diffraction of figure 3, and the prepared heterogeneous nanosheet is made of Co3S4(JCPDS # 47-1738) and SnS (JCPDS # 73-1859). Co can be known from the XPS survey in FIG. 4a3S4Doping SnSxThe heterogeneous nano-sheet mainly comprises Co, Sn, S and C elements; the Co 2p peak of FIG. 4b is mainly composed of three groups of peaks, the first group is the main peak at the binding energy 777.63, 792.80 eV, which represents the Co-containing sample3+The second set of peaks is the main peak at the binding energies 779.13, 795.32 eV, which represents the Co-containing content in the sample2+The third set of peaks is satellite peaks at binding energies 783.00, 802.38 eV; the Sn 3d peak of FIG. 4c is mainly composed of two groups of peaks, the first group is the main peak at 484.65, 493.05 eV, which represents that the sample contains Sn2+The second set of peaks are the main peaks at 485.89, 494.28 eV, which represent Sn in the sample4+(ii) a The S2 p peak of FIG. 4d is mainly composed of C = S peak at binding energy 160.13 eV, C-S peak at 160.74 eV, S peak at 161.33 eVn 2-Peak and S at 162.15 eV2-Peak composition. As can be seen, the characterization results of XPS also indicate that Co is present3S4Doping SnSxThe heterogeneous nano-sheets are mainly made of Co3S4And SnSxAnd (4) forming.
Test examples
Co, Sn-Thiourea complexes and Co obtained in the examples3S4Doping SnSxAnd (3) respectively carrying out electrochemical performance test on the heterogeneous nanosheets, wherein the test method comprises the following steps: before testing, 5mg of the substance to be tested is weighed and dispersed into 250 mul of absolute ethyl alcohol and 50 mul of 1% naphthol solution, after ultrasonic treatment is carried out for 30min to be uniform, 700 mul of secondary distilled water is added, and then ultrasonic treatment is carried out to be uniform, so as to obtain 5mg/ml suspension. The glassy carbon electrode with the diameter of 5mm adopts Al2O3Grinding to a smooth mirror surface, washing with secondary distilled water, and drying in a 45 ℃ oven after the electrode is successfully activated. Dripping 10 mu l of the suspension on the surface of the electrode in one time, then putting the electrode into an oven for drying, dripping 5 mu l of 0.1% naphthol solution on the surface of the glassy carbon electrode after drying, and drying in the oven to obtain the modified electrode.
Before OER test, high-purity O is firstly introduced into 0.1M KOH solution for 30min2To remove dissolved other gases from the solution and continue to pass O during the test2To remove dissolved oxygen. Mercury oxide is used as reference electrode, Pt sheet is used as counter electrode and drippingThe glassy carbon electrode of the sample formed the test loop. The CV (rotation speed: 400 r) is swept for 15 circles until coincidence is achieved, and then the LSV (rotation speed: 1600 r) is tested until coincidence is achieved, wherein the corresponding electrochemical scanning rate is 10 mV/s, and the scanning range is 0V to 1.2V.
OER performance testing with reference to FIG. 5a can result in a current density of 10mA/cm in 0.1M KOH solution2When is Co3S4/SnSxThe overpotential of the heterogeneous nano-sheet is 321.67mV, which is lower than that of commercial IrO2380.29mV, slightly higher than commercial RuO, of the catalyst at the same current density2297.06mV of catalyst. From FIG. 5b, Co can be seen3S4/SnSxThe Tafel slope of the heterogeneous nanosheets is 77mV/dec, which is lower than that of commercial IrO 290 mV/dec of catalyst, slightly higher than commercial RuO268mV/dec of catalyst. The results of electrochemical tests show that the performance of the product in 0.1M KOH is better than that of commercial IrO2Catalyst, slightly lower than commercial RuO2Catalyst, indicating its substituted commercial IrO2Potential of the catalyst.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. Co3S4Doping SnSxThe preparation method of the heterogeneous nanosheet is characterized by comprising the following steps: mixing the Co, Sn-thiourea complex with a dodecylamine solution, heating to 245-250 ℃, and carrying out heat preservation reaction for 50-60min to obtain Co3S4Doping SnSxA heterogeneous nanosheet electrocatalyst.
2. The method according to claim 1, wherein the mass-to-volume ratio of the Co, Sn-thiourea complex to the dodecylamine solution is 25 mg: 1 ml.
3. The method according to claim 1, wherein the rate of temperature rise is 4 ℃/min.
4. The preparation method according to claim 1, wherein the product obtained by the incubation reaction is subjected to dispersion sedimentation by using n-heptane and ethanol solution.
5. The method according to claim 4, wherein the volume ratio of n-heptane to ethanol solution is 3.5: 1.
6. the method of claim 1, wherein the Co, Sn-thiourea complex is prepared by the method comprising the steps of: heating the mixed solution of stannous chloride dihydrate, cobalt chloride hexahydrate, thiourea and deionized water to 110 ℃, and drying after heat preservation reaction to obtain the Co, Sn-thiourea complex.
7. The preparation method according to claim 6, wherein the molar ratio of the cobalt chloride dihydrate to the stannous chloride hexahydrate is 1: 1.
8. co prepared by the preparation method according to any one of claims 1 to 73S4Doping SnSxApplication of the heterogeneous nanosheet as an OER catalyst in a 0.1M KOH alkaline medium.
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