CN115786931B - Preparation method and application of organic selenium molecule modified Co-doped transition metal sulfide - Google Patents
Preparation method and application of organic selenium molecule modified Co-doped transition metal sulfide Download PDFInfo
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to the technical field of catalytic materials, in particular to a preparation method and application of organic selenium molecule modified Co-doped transition metal sulfide, which comprises the following steps: sequentially dissolving cobalt nitrate hexahydrate and thiourea in deionized water, uniformly mixing, then transferring into a reaction kettle, placing a current collector in the reaction kettle, and growing Co-doped transition metal sulfide on the current collector by adopting a classical hydrothermal method; and then placing the current collector growing with the Co-doped transition metal sulfide into a reaction kettle dissolved with dibenzyl diselenide solution, and further carrying out hydrothermal treatment to obtain the organic selenium molecule modified Co-doped transition metal sulfide. The organic selenium molecule modified Co-doped transition metal sulfide electrocatalytic material prepared by the invention has excellent hydrophilic and hydrophobic properties, not only realizes the efficient promotion of HER and OER in the same medium, but also achieves the aim of large-current hydrogen generation under low potential, and has the properties far exceeding those of commercial noble metal-based catalysts.
Description
Technical Field
The invention relates to the technical field of catalytic materials, in particular to a preparation method and application of organic selenium molecule modified Co-doped transition metal sulfide.
Background
The hydrogen energy has the advantages of high efficiency, cleanliness, rich energy storage, high combustion heat value (142 MJ/kg), good continuity and the like, and is considered as a next generation fuel with potential for replacing fossil energy sources. The new energy automobile industry development planning (2021-2035) clearly proposes the key technology for focusing on technical innovation and accelerating the breakthrough of the hydrogen energy industry chain. Hydrogen production by using electrolyzed water is an efficient way to produce hydrogen energy, and the electrolyzed water process comprises two half reactions: oxygen Evolution Reaction (OER) and Hydrogen Evolution Reaction (HER). In theory electrochemical water dissociation requires only a potential of 1.23V, but in practice a higher voltage (typically greater than 1.8V) is required to overcome the activation potential of the reaction. The large overpotential comes from two half reactions: the slow four electron transfer kinetics of anode OER and the relatively easy two electron transfer kinetics of cathode HER. In order to reduce the overpotential of the two electrodes and to increase the energy conversion efficiency, a highly efficient electrocatalyst must be used to reduce the activation energy of the above reactions. Therefore, developing an efficient and stable electrocatalyst to reduce the potential barrier and improve the utilization efficiency of hydrogen energy is a critical problem to be solved urgently.
In general, the ideal electrocatalyst needs to have the following two requirements: (1) The electrocatalyst must be highly active for each half-reaction (HER/OER) to achieve a maximum current density at a minimum overpotential; (2) The electrocatalyst has excellent long-term stability and good tolerance in electrolytes such as acid and alkali. Current researchIt was found that superior performance HER catalysts are typically noble metal platinum (Pt) based catalysts, whereas Ru-and Ir-based compounds (RuO) 2 /IrO 2 ) The catalyst is a good OER catalyst, but the large-scale application of the catalyst is severely restricted due to the defects of short reserve, high cost, poor long-time stability and the like. Therefore, there is an urgent need to develop electrocatalysts that are efficient, inexpensive, stable, and can be prepared in large quantities to achieve a "hydrogen economy" blueprint. In addition, the high-performance dual-function electrocatalyst for simultaneously catalyzing HER and OER in the same medium can greatly simplify the manufacturing process of the electrolytic cell, is convenient for industrial application equipment and greatly reduces the production cost.
Transition metal-based materials have been attracting attention from researchers in energy storage/conversion due to the advantages of low cost, abundant reserves, ease of preparation, etc., with transition metal sulfides being the most widely used. Numerous transition metal sulfide catalysts have been developed for electrolysis of water with excellent performance to date, but most of them fail to operate at high current densities (typically less than 0.1A/cm 2 ). This is mainly due to the intense HER/OER reaction at high potential, catalyst surface products (H 2 /O 2 ) Is difficult to diffuse and separate in time, forms bubble enrichment and hinders the reactant (H) + /OH - ) The mass transfer supply of the catalyst is easy to cause the falling of active centers, seriously reduces the reaction efficiency and is not beneficial to practical application and production. Therefore, there is a need to develop a catalyst with hydrophilic and hydrophobic functions, which can accelerate the mass transfer of reactants while avoiding the enrichment of product bubbles, thereby realizing high current density (more than or equal to 1A/cm) at low potential 2 ) An industrial process for preparing hydrogen by power-assisted electrocatalytic full water decomposition. In addition, the preparation of the novel bifunctional catalytic material by modifying Co-doped transition metal sulfide with organic selenium molecules is not reported yet.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method and application of an organic selenium molecule modified Co doped transition metal sulfide, which not only realize the efficient implementation of HER and OER in the same medium, but also achieve the aim of high-current hydrogen production under low potential.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the organic selenium molecule modified Co-doped transition metal sulfide comprises the following specific steps:
step 1, preparing Co doped transition metal sulfide: weighing cobalt nitrate hexahydrate and thiourea, dispersing in deionized water, ultrasonically stirring to obtain a mixed solution, transferring the mixed solution into a reaction kettle, then placing a current collector into the reaction kettle, placing into a baking oven for hydrothermal reaction, naturally cooling after the reaction is finished, taking out a sample after the reaction, cleaning, and vacuum drying to obtain Co-doped transition metal sulfide;
step 2, preparing organic selenium molecule modified Co doped transition metal sulfide: and (3) putting the Co-doped transition metal sulfide into a reaction kettle in which dibenzyl diselenide solution is dissolved, putting into an oven for hydrothermal reaction, naturally cooling after the hydrothermal reaction, taking out a sample after the reaction, cleaning, and drying in vacuum to obtain the organic selenium molecule modified Co-doped transition metal sulfide.
Preferably, in step 1, cobalt nitrate hexahydrate (Co (NO 3 ) 2 ·6H 2 The dosage of O) is 100-mg-500 mg, thiourea (CH) 4 N 2 S) the dosage of the S) is 50 mg-200 mg; the volume of deionized water used for dispersing cobalt nitrate hexahydrate and thiourea is 40ml, the temperature is room temperature, and the ultrasonic treatment is carried out for 5-10 min until the solution is uniformly dispersed.
Preferably, in step 1, the current collector is any one of Nickel Foam (NF), iron foam, and copper foam.
Preferably, in step 1 and step 2, the temperature of the oven is selected to be 180-200 ℃ and the hydrothermal reaction time is 24 hours.
Preferably, in step 1 and step 2, the cleaning condition is that deionized water and ethanol are alternately washed, and ultrasonic treatment is carried out for 3-5s.
Preferably, in step 1 and step 2, the temperature of vacuum drying is 60 ℃ and the drying time is 12 hours.
Preferably, in step 2, dibenzyldiselenide (C 14 H 14 Se 2 ) Is used in (1)The volume of deionized water used for dispersing dibenzyl diselenide is 40 ml-50 ml, and the amount of the deionized water is 10 mg-70 mg.
The invention also provides an application of the organic selenium molecule modified Co-doped transition metal sulfide prepared by the preparation method of claim 1 in hydrogen evolution and oxygen evolution reactions.
Wherein, the organic selenium molecule modified Co-doped transition metal sulfide prepared by the invention is used as an electrocatalyst for electrocatalytically decomposing water, has excellent hydrophilic and hydrophobic properties, and can reach 1A/cm only by 0.44V in 1MKOH electrolyte 2 Is 2.17 times (0.46A/cm) 2 ) And only 1.68V is needed to reach 1A/cm 2 Is noble metal IrO under the same load 2 Is 1.58 times (0.63A/cm) 2 ) Realizes the high-current hydrogen generation performance of far-super commercialized noble metal catalysts.
The organic selenium molecule modified Co-doped transition metal sulfide prepared by the method has excellent hydrophilic and hydrophobic properties, and has obvious advantages in the aspects of improving the infiltration contact of electrolyte to the electrode catalytic surface and weakening the adhesion of generated bubbles to the electrode surface. The organic selenium molecule can be tightly combined with the transition metal-based catalyst through chelation, and the surface energy of the organic selenium molecule is regulated and controlled to realize the hydrophilic and gas-repellent aim. Therefore, the invention improves the inherent activity of the catalytic active site through simple and efficient charge transfer between the ligand and the central metal, and the electrocatalytic material has excellent electrocatalytic activity and long-term stability by utilizing the hydrophilic and hydrophobic properties.
Compared with the prior art, the invention has the following beneficial effects:
1. the Co-doped transition metal sulfide electrocatalytic material modified by the organic selenium molecules has excellent hydrophilic performance (hydrophilic contact angle is less than 5 ℃) and gas-repellent performance (gas-repellent contact angle) as an electrocatalytic agent>150 deg.), accelerating the catalyst surface product (H 2 /O 2 ) Avoiding bubble enrichment and promoting the reaction (H) in the electrolyte + /OH - ) Mass transfer feed of (a).
2、The electrochemical test shows that the catalyst has excellent catalytic activity in alkaline medium, can reach high current density under small overpotential, and has performance far exceeding that of commercial noble metal catalyst. In 1MKOH electrolyte, only 0.44V is needed to reach 1A/cm 2 Is 2.17 times (0.46A/cm) 2 ) And only 1.68V is needed to reach 1A/cm 2 Is noble metal IrO under the same load 2 Is 1.58 times (0.63A/cm) 2 )。
3. The preparation method of the invention is simple and easy (classical hydrothermal method), takes the current collector as a carrier, has low cost, is economical and environment-friendly, is integrally formed, greatly simplifies the electrode manufacturing process, and has industrial production prospect.
Drawings
FIG. 1 shows CoNi prepared in example 1 of the present invention 3 S 2 -a field emission scanning electron microscope of Se at 200nm scale;
FIG. 2 shows the CoNi prepared in example 1 of the present invention 3 S 2 -a profile of a Se sample;
FIG. 3 shows CoNi prepared in example 1 of the present invention 3 S 2 -Se、CoNi 3 S 2 With CoNi prepared in example 2 3 S 2 -XRD pattern of 3 Se;
FIG. 4 shows CoNi prepared in example 1 of the present invention 3 S 2 -Se、CoNi 3 S 2 CoNi prepared in example 2 3 S 2 -3Se, NF-lrO produced in comparative example 1 2 And an OER polarization profile of the Nickel Foam (NF) after cleaning;
FIG. 5 shows CoNi prepared in example 1 of the present invention 3 S 2 -Se、CoNi 3 S 2 CoNi prepared in example 2 3 S 2 -HER polarization profile of 3Se, NF-Pt/C prepared in comparative example 2, and Nickel Foam (NF) after cleaning;
FIG. 6 CoNi prepared in example 1 of the present invention 3 S 2 -Se、CoNi 3 S 2 As in example 2Prepared CoNi 3 S 2 -HER polarization profile of 3Se, NF-Pt/C prepared in comparative example 2, and Nickel Foam (NF) after cleaning;
FIG. 7 CoNi prepared in example 1 of the present invention 3 S 2 OER stability test pattern of Se;
FIG. 8 CoNi prepared in example 1 of the present invention 3 S 2 -HER stability test pattern of Se;
FIG. 9 CoNi prepared in example 1 of the present invention 3 S 2 Se, NF-lrO produced in comparative example 1 2 And a full water-splitting performance test chart of NF-Pt/C prepared in comparative example 2.
Detailed Description
The following technical solutions in the embodiments of the present invention will be clearly and completely described with reference to the accompanying drawings, so that those skilled in the art can better understand the advantages and features of the present invention, and thus the protection scope of the present invention is more clearly defined. The described embodiments of the present invention are intended to be only a few, but not all embodiments of the present invention, and all other embodiments that may be made by one of ordinary skill in the art without inventive faculty are intended to be within the scope of the present invention.
Example 1:
organic selenium molecule modified Co doped Ni 3 S 2 Compound (CoNi) 3 S 2 -Se) preparation:
step 1, 0.1g (0.34 mmol) Co (NO 3 ) 2 ·6H 2 O, and 0.05g (0.67 mmol) CH 4 N 2 S, adding the solution into 40mL of deionized water, uniformly dispersing by ultrasonic waves, and transferring the solution into a polytetrafluoroethylene reaction kettle;
step 2, sequentially ultrasonically cleaning foam nickel (3.0 cm multiplied by 4.0cm,0.5 mm) with ethanol (30 min), acetone (30 min multiplied by 30), 3MHCl solution (15 min) and deionized water (15 min multiplied by 3), vertically placing the foam nickel into the reaction kettle in step 1, transferring to a 180 ℃ oven for reaction for 24h, naturally cooling, taking out a sample, alternately flushing with deionized water and ethanol, ultrasonically performing vacuum drying at 60 ℃ for 12h for 3-5s, and obtaining Co doped materialImpurity Ni 3 S 2 Compound (CoNi) 3 S 2 ) A sample;
step 3, the CoNi is processed 3 S 2 The sample was placed vertically in a reaction vessel and dispersed with 0.01g (29. Mu. Mol) of C 14 H 14 Se 2 Transferring 40ml deionized water into a reaction kettle, transferring to a 180 ℃ oven for reaction for 24 hours, naturally cooling, taking out a sample, alternately flushing with deionized water and ethanol, ultrasonically treating for 3-5 seconds, and vacuum drying at 60 ℃ for 12 hours to obtain a final product (CoNi 3 S 2 -Se)。
Example 2:
co-doped Ni modified by 3-organic selenium molecule 3 S 2 Compound (CoNi) 3 S 2 -3 Se) preparation:
example 2 differs from example 1 only in the addition of C 14 H 14 Se 2 Different amounts of C added in example 2 14 H 14 Se 2 The amount was 0.03g (87. Mu. Mol).
Example 3:
7-organic selenium molecule modified Co doped Ni 3 S 2 Compound (CoNi) 3 S 2 -7 Se) preparation:
example 3 differs from example 1 only in the addition of C 14 H 14 Se 2 Different amounts of C added in example 2 14 H 14 Se 2 The amount was 0.07g (203. Mu. Mol).
Example 4:
2-Co doped Ni 3 S 2 Compound (2 CoNi) 3 S 2 ) (2 means 2 times S content) preparation:
example 4 CoNi prepared in example 1 3 S 2 Is distinguished by the addition of CH only 4 N 2 S was varied in the amount of CH added in example 4 4 N 2 The amount of S was 0.1g (1.34 mmol).
CoNi was measured at 200nm using a field emission scanning electron microscope (model ZEISSGeminiSEM300, manufactured by Karl Zeiss Co., ltd.) 3 S 2 Se is scanned, the obtained scanning electron microscope image is shown in figure 1, and the scanning electron microscope image can be used forIt can be seen that ultra-thin nanoplatelets grow closely perpendicular to the nickel foam, cross-linked nanoplatelets provide adequate channels for electron transfer, and provide more specific surface area and active sites.
CoNi was measured by a transmission electron microscope (model number FEITALOSF200X, manufactured by FEI Co., U.S.A.) 3 S 2 The Se is scanned, and the Ni, co, S, se element is uniformly distributed in the whole system structure through an energy spectrum surface distribution test chart as shown in fig. 2, and meanwhile, the successful loading of the organic selenium molecules on the surface of the sample is confirmed.
CoNi of example 1 was performed by means of an X-ray diffractometer (model Brucker D8-advance, brucker Corp., germany) 3 S 2 -Se、CoNi 3 S 2 And CoNi of example 2 3 S 2 The XRD pattern obtained by testing-3 Se is shown in figure 3, and the result shows that the organic selenium molecule is modified and treated to CoNi 3 S 2 The crystal structure of 3Se has little effect, indicating that the organic selenium molecules are only modified on the surface of the material, and do not change the bulk structure of the material.
CoNi of example 1 was measured by a contact angle measuring instrument (model SDC-100) 3 S 2 Se was tested as shown in FIG. 4, and the results showed CoNi 3 S 2 Se has excellent hydrophilic and hydrophobic properties.
Comparative example 1:
substitution of CoNi in example 1 with a commercial catalyst 3 S 2 Preparation of NF-lrO by Se catalyst 2 ：
Step 1, 4 mgrO is added 2 The catalyst was added to a mixed solution of 920. Mu.L of isopropyl alcohol and 80. Mu.L of LNafion solution, and the mixture was ultrasonically dispersed for 1 hour to obtain a uniformly dispersed slurry.
Step 2, ultrasonically cleaning foam nickel (0.5 cm multiplied by 0.5cm,0.5 mm) with ethanol (30 min), acetone (30 min multiplied by 30), 3MHCl solution (15 min) and deionized water (15 min multiplied by 3) in sequence, and then coating the solution in step 1 on the foam nickel, wherein the load is ensured to be consistent with CoNi 3 S 2 The Se system corresponds to (2 mg/cm 2 ) And drying to obtain a sample.
Comparative example 2:
substitution of CoNi in example 1 with a commercial catalyst 3 S 2 -Se catalyst, preparing NF-Pt/C:
step 1, adding 4mgPt/C catalyst into a mixed solution of 920 mu L of isopropyl alcohol and 80 mu LNafion solution, and performing ultrasonic dispersion for 1h to obtain uniformly dispersed slurry.
Step 2, ultrasonically cleaning foam nickel (0.5 cm multiplied by 0.5cm,0.5 mm) with ethanol (30 min), acetone (30 min multiplied by 30), 3MHCl solution (15 min) and deionized water (15 min multiplied by 3) in sequence, and then coating the solution in step 1 on the foam nickel, wherein the load is ensured to be consistent with CoNi 3 S 2 The Se system corresponds to (2 mg/cm 2 ) And drying to obtain a sample.
Electrochemical testing: coNi prepared in example 1 using a three electrode system with 1.0mol/LKOH solution as the electrolyte 3 S 2 -Se electrode, coNi 3 S 2 Electrode, coNi prepared in example 2 3 S 2 3Se, NF-lrO produced in comparative example 1 2 The electrode, NF-Pt/C prepared in comparative example 2 and the Nickel Foam (NF) after washing were used as working electrodes, calomel electrode as reference electrode, graphite electrode as counter electrode, respectively, and CoNi was measured 3 S 2 -Se、CoNi 3 S 2 、CoNi 3 S 2 -3Se、NF-lrO 2 Linear sweep voltammogram of NF-Pt/C and Nickel Foam (NF) after cleaning.
CoNi obtained in example 1, example 2, comparative example 1 and comparative example 2 3 S 2 -Se、CoNi 3 S 2 、 CoNi 3 S 2 -3Se、NF-lrO 2 The electrochemical performance of NF-Pt/C and cleaned foam Nickel (NF) was tested by an electrochemical workstation, which was a Cinnamomum electrochemical workstation model CHI660E.
CoNi pair by linear sweep voltammetry 3 S 2 -Se、CoNi 3 S 2 、CoNi 3 S 2 -3Se、NF-lrO 2 The OER and HER performance tests are respectively carried out on the NF-Pt/C and the cleaned foam Nickel (NF), the obtained OER and HER polarization graphs (LSV graphs) are respectively shown in figures 5 and 6, and the samples modified by the organic selenium molecules CoNi 3 S 2 -Se and CoNi 3 S 2 -3Se relatively unmodified CoNi 3 S 2 Exhibits more excellent performance while CoNi 3 S 2 Se at 1A/cm 2 With a minimum overpotential (OER: 1.68V; HER: -0.44V) and a relatively large current density at lower potentials (OER: 1.62V overpotential up to 0.5A/cm) 2 The method comprises the steps of carrying out a first treatment on the surface of the HER: an overpotential of 0.36V of 0.5A/cm 2 ) Proved by the feasibility of the scheme of the invention, the organic selenium molecules are adopted to regulate and control the electrocatalytic hydrogen evolution and oxygen evolution heavy current catalysis of Co-doped transition metal sulfides.
CoNi pair using current-time scanning 3 S 2 Se was subjected to HER and OER stability tests as shown in figures 7, 8, respectively. HER stability test current density was set at 10mA/cm 2 And 100mA/cm 2 OER stability test current density was set at 100mA/cm 2 And 500mA/cm 2 . Results show CoNi 3 S 2 Se has excellent hydrogen evolution and oxygen evolution stability under different current densities, and the current density is not obviously attenuated within 10 hours.
CoNi pair by linear sweep voltammetry 3 S 2 -Se、NF-lrO 2 And NF-Pt/C were respectively subjected to full water splitting performance test of the double-electrode system, and the obtained full water splitting polarization curve chart (LSV chart) is shown in FIG. 9. The results showed that NF-Pt/C-lrO at the same overpotential of 2.2V 2 Can only reach 435mA/cm 2 While CoNi 3 S 2 Se can reach 875mA/cm 2 Is the current density of the current commercial noble metal catalyst NF-Pt/C-lrO 2 2 times the current density, indicating CoNi 3 S 2 Se has excellent electrolyzed water catalytic activity.
In conclusion, the organic selenium molecule modified Co-doped Ni prepared by the invention 3 S 2 The compound electrocatalytic material has far better performance than noble metal catalyst (Pt/C, lrO) 2 ) The electrocatalytic full water-splitting performance is excellent in catalytic activity and cycle stability under high current density, and is beneficial to commercial application.
The description and practice of the invention disclosed herein will be readily apparent to those skilled in the art, and may be modified and adapted in several ways without departing from the principles of the invention. Accordingly, modifications or improvements may be made without departing from the spirit of the invention and are also to be considered within the scope of the invention.
Claims (4)
1. The preparation method of the organic selenium molecule modified Co-doped transition metal sulfide is characterized by comprising the following specific steps of:
step 1, preparing Co doped transition metal sulfide: weighing cobalt nitrate hexahydrate and thiourea, dispersing in deionized water, ultrasonically stirring to obtain a mixed solution, transferring the mixed solution into a reaction kettle, then placing a current collector into the reaction kettle, placing into a baking oven for hydrothermal reaction, naturally cooling after the reaction is finished, taking out a sample after the reaction, cleaning, and vacuum drying to obtain Co-doped transition metal sulfide; wherein the current collector is foam nickel;
step 2, preparing organic selenium molecule modified Co doped transition metal sulfide: putting the Co-doped transition metal sulfide into a reaction kettle in which dibenzyl diselenide solution is dissolved, putting into an oven for hydrothermal reaction, naturally cooling after the hydrothermal reaction is finished, taking out a sample after the reaction, cleaning, and vacuum drying to obtain the organic selenium molecule modified Co-doped transition metal sulfide;
in the step 1, the dosage of the cobalt nitrate hexahydrate is 100 mg-500 mg, and the dosage of the thiourea is 50 mg-200 mg; the volume of deionized water used for dispersing cobalt nitrate hexahydrate and thiourea is 40ml, the temperature is room temperature, and the ultrasonic treatment is carried out for 5-10 min until the solution is uniformly dispersed;
in the step 1 and the step 2, the temperature of the oven is selected to be 180-200 ℃ and the hydrothermal reaction time is 24 hours;
in the step 2, the dosage of the dibenzyl diselenide is 10 mg-70 mg, and the volume of deionized water used for dispersing the dibenzyl diselenide is 40 ml-50 ml.
2. The method for preparing the organic selenium molecule modified Co-doped transition metal sulfide according to claim 1, wherein in the step 1 and the step 2, the cleaning condition is that deionized water and ethanol are alternately washed, and ultrasonic treatment is carried out for 3-5s.
3. The method for preparing the organic selenium molecule modified Co-doped transition metal sulfide according to claim 1, wherein in the step 1 and the step 2, the temperature of vacuum drying is 60 ℃ and the drying time is 12 hours.
4. Use of the organic selenium molecule modified Co-doped transition metal sulfide prepared by the preparation method of claim 1 in hydrogen evolution and oxygen evolution reactions.
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| WO2021184563A1 (en) * | 2020-03-19 | 2021-09-23 | 苏州楚捷新材料科技有限公司 | Preparation method for foamed nickel-based catalyst for hydrogen production by water electrolysis |
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| WO2021184563A1 (en) * | 2020-03-19 | 2021-09-23 | 苏州楚捷新材料科技有限公司 | Preparation method for foamed nickel-based catalyst for hydrogen production by water electrolysis |
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