CN114622220B - Co 3 S 4 Doping SnS x Preparation method and application of heterogeneous nanosheet - Google Patents
Co 3 S 4 Doping SnS x Preparation method and application of heterogeneous nanosheet Download PDFInfo
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Abstract
The invention provides a Co 3 S 4 Doping SnS x A method of preparing heterogeneous nanoplates, comprising the steps of: mixing the Co, sn-thiourea complex with the dodecylamine solution, heating to 245-250 ℃, and reacting for 50-60min under the condition of heat preservation to obtain Co 3 S 4 Doping SnS x A heterogeneous nanosheet electrocatalyst. The invention also discloses Co prepared by the preparation method 3 S 4 Doping SnS x The heterogeneous nanosheet is used as an OER catalyst in a 0.1M KOH alkaline medium. The method has the advantages of simple process, novelty, high efficiency, low cost and the like, and has potential industrial value.
Description
Technical Field
The invention relates to the technical field of electrocatalysts, in particular to a catalystCo seed 3 S 4 Doping SnS x A 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 the catalysts, the metal sulfide electrocatalyst has the characteristics of low cost, high catalytic activity and stable operation, and is approaching or even exceeding RuO in the aspects of oxygen evolution electrocatalytic performance, catalytic durability and the like 2 、IrO 2 And 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 Co 3 S 4 Doping SnS x A preparation method of heterogeneous nano-sheets.
The technical scheme adopted by the invention for overcoming the technical problems is as follows: co 3 S 4 Doping SnS x The preparation method of the heterogeneous nanosheet electrocatalyst comprises the following steps: mixing the Co, sn-thiourea complex with a dodecylamine solution, heating to 245-250 ℃, and reacting for 50-60min under the condition of heat preservation to obtain Co 3 S 4 Doping SnS x A heterogeneous nanosheet electrocatalyst.
Preferably, the mass volume ratio of the Co, sn-thiourea complex to the dodecylamine solution is 25mg:1ml.
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 stannous chloride dihydrate to the cobalt chloride hexahydrate to the thiourea is 1:1:5, the molar volume ratio of the stannous chloride dihydrate to the deionized water is 1mmol:5ml.
The invention also discloses a preparation method according to the methodMethod for preparing Co 3 S 4 Doping SnS x Application 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 Co 3 S 4 Doping SnS x The 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 method 3 S 4 Doping SnS x Heterogeneous nanosheets in SnS x Co is formed on the surface of the nano sheet 3 S 4 Nanosheet layer, and Co 3 S 4 Incorporation to cause SnS x Lattice 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. 2 shows Co in an embodiment of the present invention 3 S 4 Doping SnS x And (3) heterogeneous nanosheet TEM, HRTEM and Mapping images.
FIG. 3 shows the Co, sn-thiourea complex and Co in the example of the present invention 3 S 4 Doping SnS x XRD contrast pattern of heterogeneous nanoplates.
FIG. 4 shows Co in an embodiment of the present invention 3 S 4 Doping SnS x XPS plot of heterogeneous nanoplates.
FIG. 5 shows Co, sn-Thiourea complexes and Co 3 S 4 Doping SnS x And (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
Co 3 S 4 Doping SnS x The preparation method of the heterogeneous nano-sheet comprises the steps of preparing precursor Co, sn-thiourea complex and Co 3 S 4 Doping SnS x 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 in the 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 content is not large, 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 4 hours, and then grinding the product into powder by using a mortar to obtain light blue precursor Co, sn-thiourea complex for analysis and characterization.
The infrared spectrum is characterized as shown in figure 1, and is at 3391.65 and 3300.85cm -1 The double peak of (A) is attributed to NH stretching vibration, 1622.81cm -1 Is due to NH flexural vibration, 1388.64cm -1 The peak is attributed to C-N stretching vibration, 1096.57cm -1 The peak of (A) is attributed to Sn 2+ ,567.74cm -1 The peak of (A) is attributed to Co 2+ 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 Co 3 S 4 Doping SnS x Heterogeneous 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 60min. After the reaction is finished, naturally cooling the reaction device to 48 ℃, and mixing the components in a volume ratio of 3.5:1 with a mixed solution of n-heptane and absolute ethanol, and vacuum drying at 60 deg.CDrying in a drying oven for 12h to obtain Co 3 S 4 Doping SnS x Heterogeneous nanoplatelets for analytical characterization.
As can be seen from the low power TEM of FIGS. 2a and 2b, the prepared Co 3 S 4 Doping SnS x The morphology of the heterogeneous nano-sheet is SnS x Co is doped on the nano-sheet substrate 3 S 4 Small nanosheet particle, co as can be seen by high resolution TEM of FIG. 2c 3 S 4 Doping SnS x The heterogeneous nano-sheets are mainly made of Co 3 S 4 The (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 Co 3 S 4 The 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-film 3 S 4 And (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 Co 3 S 4 (JCPDS # 47-1738) and SnS (JCPDS # 73-1859). Co can be known from the XPS survey of FIG. 4a 3 S 4 Doping SnS x The heterogeneous nano-sheet mainly comprises Co, sn, S and C elements; the Co 2p peak of FIG. 4b consists essentially of three sets of peaks, the first set of peaks being the main peaks at binding energies 777.63, 792.80 eV, which represent the Co-containing sample 3+ The second set of peaks is the main peak at 779.13, 795.32 eV binding energy, which represents the Co-containing sample 2+ 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 located at 484.65, 493.05 eV, which represents that the sample contains Sn 2+ The second set of peaks is the main peak at 485.89,494.28 eV, which represents Sn in the sample 4+ (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 eV n 2- Peak and S at 162.15 eV 2- Peak composition. As can be seen, the characterization results of XPS also indicate Co 3 S 4 Doping SnS x The heterogeneous nanosheets are mainlyFrom Co 3 S 4 And SnS x And (4) forming.
Test examples
Co, sn-Thiourea complexes and Co obtained in the examples 3 S 4 Doping SnS x And (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 Al 2 O 3 Grinding to a smooth mirror surface, washing with secondary distilled water, and drying in a 45 ℃ oven after successful electrode activation for later use. 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 30min 2 To remove dissolved other gases from the solution and continue to pass O during the test 2 To remove dissolved oxygen. And a testing loop is formed by taking mercury oxide as a reference electrode, a Pt sheet as a counter electrode and a glassy carbon electrode dripped with a sample. The CV (rotation speed: 400 r) is swept for 15 circles until coincidence, and then the LSV (rotation speed: 1600 r) is tested until coincidence, the corresponding electrochemical sweep rate is 10 mV/s, and the sweep 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 solution 2 When is Co 3 S 4 /SnS x The overpotential of the heterogeneous nano-sheet is 321.67mV, which is lower than that of commercial IrO 2 380.29mV, slightly higher than commercial RuO, of the catalyst at the same current density 2 297.06mV of the catalyst. From FIG. 5b, co can be seen 3 S 4 /SnS x The Tafel slope of the heterogeneous nanosheets is 77mV/dec, which is lower than that of commercial IrO 2 90 mV/dec of catalyst, slightly higher than commercial RuO 2 68mV/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 IrO 2 Catalyst, slightly lower than commercial RuO 2 CatalysisAgents indicating their substituted commercial IrO 2 Potential 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 modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. 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 (5)
1. Co 3 S 4 Doping SnS x The preparation method of the heterogeneous nanosheet is characterized by comprising the following steps: mixing the Co, sn-thiourea complex with the dodecylamine solution, heating to 245-250 ℃, and reacting for 50-60min under the condition of heat preservation to obtain Co 3 S 4 Doping SnS x A heterogeneous nanosheet electrocatalyst; the mass volume ratio of the Co, sn-thiourea complex to the dodecylamine solution is 25mg:1ml; the preparation method of the Co, sn-thiourea complex comprises the following steps: heating a mixed solution of stannous chloride dihydrate, cobalt chloride hexahydrate, thiourea and deionized water to 110 ℃, and drying after heat preservation reaction to obtain a Co, sn-thiourea complex; the molar ratio of the stannous chloride dihydrate to the cobalt chloride hexahydrate is 1:1.
2. the method of claim 1, wherein the temperature is raised to 245-250 ℃ at a rate of 4 ℃/min.
3. The preparation method of claim 1, wherein the product obtained after the heat preservation reaction is performed for 50-60min is subjected to dispersion and sedimentation by using n-heptane and ethanol solution.
4. The method according to claim 3, wherein the volume ratio of n-heptane to ethanol solution is 3.5:1.
5. co prepared by the preparation method according to any one of claims 1 to 4 3 S 4 Doping SnS x Application of the heterogeneous nanosheet as an OER catalyst in a 0.1M KOH alkaline medium.
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| CN104821240B (en) * | 2015-04-29 | 2017-05-10 | 岭南师范学院 | SnS2/MoS2 composite material one-step hydrothermal synthesizing method and application thereof |
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| CN109289874B (en) * | 2018-11-16 | 2021-03-16 | 安徽师范大学 | Cobalt-doped tin disulfide nanosheet array material and preparation method and application thereof |
| CN109647536B (en) * | 2019-01-14 | 2020-06-26 | 中国科学技术大学 | Cobalt-nickel double-doped tin sulfide nanosheet as well as preparation method and application thereof |
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