CN114525525B - Carbon-supported Co-based monatomic catalyst for ORR 2 electron path, active site structure regulation method and application - Google Patents
Carbon-supported Co-based monatomic catalyst for ORR 2 electron path, active site structure regulation method and application Download PDFInfo
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Abstract
The invention belongs to the field of new material preparation and application, and provides a carbon-supported Co-based monatomic catalyst for an ORR 2 electron path, an active site structure regulation method and application. The invention provides a regulating and controlling means of active sites of a monatomic catalyst, which introduces abundant oxygen-containing functional groups around the active sites in an ozone post-treatment mode to ensure that the monatomic active sites generate structural reconstruction, and further regulates the ORR process from a 4 electron path to a 2 electron path.
Description
Technical Field
The invention belongs to the field of new material preparation and application, and relates to a carbon-supported Co-based monatomic catalyst for an ORR 2 electron path, an active site structure regulation method and application.
Background
The monatomic catalyst is the leading edge and the hot spot of research in the field of catalysis at present, and attracts the wide attention of researchers, the utilization rate of active metal atoms of the monatomic catalyst reaches the maximum, the definite active site structure is favorable for the researchers to understand the reaction mechanism from the molecular atom scale, the monatomic catalyst is considered to be a bridge for communicating homogeneous catalysis and heterogeneous catalysis, and the monatomic catalyst shows excellent catalytic performance in the aspects of electrocatalysis, photocatalysis, thermocatalysis and the like.
Y Chen et al [ adv.mater.,2019,31,1806312 ] in SiO 2 Is a hard template, histidine is a carbon source and a nitrogen source, and Fe-N is prepared 4 A monatomic catalyst of structure; a Han et al [ adv. Mater.,2018,30, 1706508 ] prepared with a polymer encapsulation strategy with Co-N 4 A monatomic catalyst of structure; y Qu et al [ Nat. Catal.,2018,1,781-786 ] by direct emission of atoms from bulk metals followed by NH 3 Assisted capture on porous carbon to prepare the catalyst with Cu-N 4 A monatomic catalyst of structure. Although such catalysts exhibit some 4-electron pathway catalytic activity for ORR, the reported synthesis methods lack some site-regulating means.
Y Wang et al [ Angew. Chem. Int. Ed.,2020,59,13057-13062 ] constructed on carbon support with Ni-N 2 O 2 A single atom catalyst of a site can catalyze the ORR process 2 electron pathway. B Li et al [ adv.mater.,2019,31,1808173 ] and C Tang et al [ j.am.chem.soc.,2021,143,7819-7827 ] also found the presence of oxygen-containing functional groups near the metal active center to facilitate the progression of the ORR process 2 electron path.
In conclusion, although monatomic catalysts are widely studied in the ORR field, the preparation strategies reported so far generally lack active site regulation means, i.e. the active site structure is uncontrollable. Meanwhile, the oxygen-containing functional group is used for modifying the metal monoatomic active center, so that the 2 electron path generation of the ORR process can be promoted. Therefore, the Co-based carbon-supported monatomic catalyst is taken as a research object, the structure of the metal active site is regulated and controlled in a mode of combining molten salt assisted pyrolysis and ozone post-treatment, and the ORR reaction path is regulated from a 4-electron process to a 2-electron process.
Disclosure of Invention
The invention aims to develop a simple regulating and controlling means of the active site of the monatomic catalyst, so as to lead the active center to carry out structural reconstruction and lead the Co monatomic active site to be separated from Co-N 4 Cl and Co-N 2 Co-N for adjusting Cl structure coexistence 2 (OH), two C atoms around the pyridine N to which the Co atom is bonded, are bonded to OH groups, respectively (the schematic structure is shown below), and the ORR reaction pathway is adjusted from a 4-electron process to a 2-electron process.
Schematic structure of Co single-atom site before and after structure reconstruction (a is before reconstruction, b is after reconstruction)
The technical scheme of the invention is as follows:
a carbon supported Co-based monatomic catalyst for ORR 2 electron pathway, the carbon supported Co-based monatomic catalyst having the structural formula:
a method for regulating and controlling an active site of a carbon-supported Co-based monatomic catalyst takes the Co-based monatomic catalyst as an object to regulate and control an active center deliberately, and comprises the following steps:
step (1): preparation of carbon-supported Co-based monatomic catalyst CoN/C
1)NaCl、ZnCl 2 Carbon precursor and Co precursorMixing uniformly; mixing in a ball milling mode, wherein the ball milling time is 5-120min and 200-1000 rpm, and a ball milling tank is sealed and kept dry;
NaCl and ZnCl 2 Is not more than 1,NaCl and ZnCl 2 The mass ratio of the sum of the two to the carbon precursor is 50-1, the mass ratio of the Co precursor to the carbon precursor is 0.005-0.05;
2) Heating the uniformly mixed materials for 0.5 to 5 hours in an inert atmosphere at the temperature of 700 to 1100 ℃, and then cooling;
3) Taking out the heated material, heating and stirring the heated material in dilute hydrochloric acid with the temperature of 50-150 ℃ and the concentration of 0.1-3M for 3-24 h, and washing off reaction residues;
4) Filtering and drying the solution to obtain a carbon-supported Co-based monatomic catalyst CoN/C;
step (2): performing structure regulation on the carbon-supported Co-based monatomic catalyst CoN/C active site obtained in the step (1) to obtain CoNO/C;
1) Dissolving the carbon-supported Co-based monatomic catalyst prepared in the step (1) in deionized water, wherein the concentration of the carbon-supported Co-based monatomic catalyst is 0.1-5 mg ml -1 Uniformly mixing the components in a mode of ultrasonic and stirring;
2) Introducing ozone for 10-240 min while stirring in a bubbling mode until the color of the solution changes;
3) Centrifuging at high speed to remove most of the supernatant, and collecting the lower layer precipitate;
4) Heating and washing in dilute hydrochloric acid with the temperature of 50-150 ℃ and the concentration of 0.1-3M for 3-24 h, obtaining a precipitate, filtering, and drying to obtain the catalyst CoNO/C with the active site adjusted inside.
In the step (1), the carbon precursor is adenine or hypoxanthine; the Co precursor is Co powder, co metal oxide or Co salt.
In the step (1), the inert atmosphere is Ar gas or N 2 And (4) air atmosphere.
In the step (2), the ultrasonic power is 500W, the frequency is 35-40 kHz, and the ultrasonic time is 5-60 min; the stirring speed is 200-1000 rpm, and the time is 5-60 min.
In the step (2), the centrifugal speed is 8000 rpm-50000 rpm.
The application of a catalyst CoNO/C in ORR comprises the following steps:
1) Adding a catalyst CoNO/C into a mixed solution of ethanol and Nafion, performing ball milling and then ultrasonic treatment, and uniformly mixing in a ball milling and ultrasonic treatment combined mode to obtain catalyst ink;
the ball milling time is 0.5 to 3 hours, and the rotating speed is 200 to 1000rpm;
the ultrasonic power is 500W, the frequency is 35-40 kHz, and the time is 0.5-5 h;
the concentration of the catalyst CoNO/C is 0.5-10 mg ml -1 The volume ratio of Nafion to ethanol is 0.01-0.06;
2) The catalyst ink is dripped on the electrode of the rotating ring disk, and the loading capacity of the catalyst is 0.01-10 mgcm -2 Spontaneous combustion drying to obtain a catalyst film;
3) Introducing O into electrolyte solution 2 To O in the electrolyte solution 2 Saturation; the electrolyte solution is 0.1MHClO 4 Solution, 0.5M H 2 SO 4 Solution or 0.1M KOH solution;
4) Applying the electrode coated with the catalyst film at O 2 Testing LSV curve in saturated solution, and continuously introducing O in the testing process 2 And calculating H from the LSV curve 2 O 2 Selectivity, and thus define the ORR reaction pathway;
the rotating speed is set to be 400-2500 rpm, and the ring disk electrode H 2 O 2 The collection coefficient is 0.37, the applied potential of the ring electrode is 1.0-1.5V vs.RHE, the test range is 0-1.2V vs.RHE, and the scanning speed is 0.001-1V s -1 。
The invention has the beneficial effects that: the invention provides a regulating and controlling means of active sites of a monatomic catalyst, which introduces abundant oxygen-containing functional groups around the active sites in an ozone post-treatment mode to ensure that the monatomic active sites generate structural reconstruction, and further regulates the ORR process from a 4 electron path to a 2 electron path.
Drawings
FIG. 1 is TEM images of a Co-based monatomic catalyst before and after active site structure reconstruction; wherein (a) is before the structure reconstruction and (b) is after the structure reconstruction.
FIG. 2 is an SEM image of a Co-based monatomic catalyst before and after active site structure reconstruction; wherein, the method (a) is before the reconstruction of the CoN/C structure, and the method (b) is after the reconstruction of the CoNO/C structure.
FIG. 3 is an XRD pattern of a Co-based monatomic catalyst before and after active site structure reconstruction; wherein CoN/C is before structure reconstruction, and CoNO/C is after structure reconstruction.
FIG. 4 is a HAADF-STEM diagram of a Co-based monatomic catalyst before and after active site structure reconstruction; wherein, the method (a) is before the reconstruction of the CoN/C structure, and the method (b) is after the reconstruction of the CoNO/C structure.
FIG. 5 is a diagram of a Co-based monatomic catalyst XAS before and after active site structure reconfiguration; wherein, the method (a) is before the reconstruction of the CoN/C structure, and the method (b) is after the reconstruction of the CoNO/C structure.
FIG. 6 is a diagram of ORR performance of a Co-based monatomic catalyst before and after active site structure reconstruction; wherein (a) is 0.1M HClO 4 LSV curve measured at 1600rpm in solution, (b) calculated H 2 O 2 And (4) a selectivity graph.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1
1g of adenine, 5g of NaCl and 5g of ZnCl are weighed respectively 2 And ball milling 50mg of Co powder for 30min to mix evenly, and adopting a ball milling 5min interval 5min mode to prevent a large amount of heat from being released in the ball milling process. Then heating for 1h at 900 ℃ in Ar atmosphere, and slowly cooling to room temperature. Taking out the material, stirring the material in 2M HCl solution at 80 ℃ for 12h, filtering and washing the material by using enough water until the solution is neutral, and drying the material in vacuum at 60 ℃ to obtain the Co-based carbon-supported monatomic catalyst (CoN/C).
Example 2
200mg of the catalyst CoN/C prepared in example 1 was weighed, 200ml of deionized water was added, the mixture was subjected to ultrasonic treatment for 30min, stirred for 15min, and then ozone was bubbled through the mixture for 120min while stirring. Then, the mixture was centrifuged at 18000rpm, the supernatant was decanted, the precipitate was taken out, 250ml of 0.5M HCl solution was added, the mixture was stirred at 80 ℃ for 12 hours, filtered and washed with sufficient water until the solution became neutral, and dried under vacuum at 60 ℃ to obtain a Co-based catalyst (CoNO/C) having a reconstituted structure.
The active site structure of the catalyst prepared in example 1 is Co-N 4 Cl and Co-N 2 Cl structure coexists, active site structural reconstruction occurs after ozone post-treatment in example 2, and Co-N is adjusted 2 (OH), the C atom around the pyridine N to which the Co atom is attached, is attached to an OH group as shown by the aforementioned restructured structure. The coordination environment of the active center before and after the structure reconstruction can be verified by XAS and XPS fitting results, for example, as shown in FIG. 5 (a), the fitting result of CoN/C catalyst at Co k edge, the coordination number of N is 3.2 by three-path fitting of Co-N, co-Cl and Co-C, which indicates that Co-N 4 And Co-N 2 Coexistence of a step of,
the position has an obvious coordination peak which shows that the catalyst is axially connected with Cl, and finally the catalyst active site structure is Co-N 4 Cl and Co-N 2 The Cl structure coexists. FIG. 5 (b) shows the fitting result of CoNO/C catalyst at Co k edge, by Co-N, co-C dual-path fitting, the coordination number of N is 2, i.e., co is Co-N 2 The active structure of the compound is Co-N, and the C and OH around pyridine N are connected after ozone treatment according to the XPS analysis result 2 (OH)。
Example 3
Weighing 1g of hypoxanthine, 5g of NaCl and 5g of ZnCl respectively 2 50mg of Co powder is ball-milled for 30min and uniformly mixed, and in order to prevent a large amount of heat from being released in the ball-milling process, a ball-milling mode is adopted for 5min at intervals of 5min. Then heating for 1h at 900 ℃ in Ar atmosphere, and slowly cooling to room temperature. Taking out the material, stirring the material in 2M HCl solution at 80 ℃ overnight, filtering and cleaning the material by using enough water until the solution is neutral, and drying the solution in vacuum at 60 ℃ to obtain the Co-based carbon-supported monatomic catalyst.
Example 4
1g of adenine, 5g of NaCl and 5g of ZnCl are weighed respectively 2 ,50mg Co 2 O 3 Ball milling is carried out for 30min, mixing is carried out uniformly, and in order to prevent a large amount of heat from being released in the ball milling process, a ball milling mode of 5min is adopted at intervals of 5min. Then heating for 1h at 900 ℃ in Ar atmosphere, and slowly cooling to room temperature. Taking out the material at 2MStirring the solution in HCl solution at 80 ℃ overnight, filtering and washing the solution by using enough water until the solution is neutral, and drying the solution in vacuum at 60 ℃ to obtain the Co-based carbon-supported monatomic catalyst.
Example 5
4mg of the catalyst prepared in example 1 (CoN/C) were weighed out, 960. Mu.L of ethanol were added and ball milled at 500rpm for 150min in such a way that the ball milling was carried out for 5min at 5-min intervals. Then 40. Mu.L of Nafion solution is added, and the mixture is subjected to ultrasonic treatment for 2 hours to obtain uniform catalyst ink. 5 mul of catalyst ink is drawn and is dripped on the surface of the glassy carbon of the ring disk electrode, and the area of the glassy carbon disk is 0.2475cm 2 . Then 1600rpm at O 2 Saturated 0.1M HClO 4 Testing LSV curve in solution, potential range is 0-1.0V (vs. RHE), sweep speed is 0.01V s -1 . Continuously introducing O in the test process 2 . Obtaining LSV curve and calculating H according to the LSV curve 2 O 2 And (4) selectivity.
Example 6
4mg of the catalyst prepared in example 2 (CoNO/C) were weighed out, 960. Mu.L of ethanol was added and ball milled at 500rpm for 150min in such a way that the ball milling was carried out 5min apart. Then 40. Mu.L of Nafion solution is added, and the mixture is subjected to ultrasonic treatment for 2 hours to obtain uniform catalyst ink. 5 mul of catalyst ink is drawn and is dripped on the surface of the glassy carbon of the ring disk electrode, and the area of the glassy carbon disk is 0.2475cm 2 . Then 1600rpm at O 2 Saturated 0.1M HClO 4 Testing LSV curve in solution, potential range is 0-1.0V (vs. RHE), sweep speed is 0.01V s -1 . Continuously introducing O in the test process 2 . Obtaining LSV curve and calculating H according to the LSV curve 2 O 2 And (4) selectivity.
Results of performance testing of examples 5 and 6 as shown in FIG. 6 in comparison, it can be seen from FIG. 6 (a) that the disk current of the catalyst obtained in example 5 (CoN/C) catalyzed the ORR process is significantly greater than the catalyst obtained in example 6 (CoNO/C) and the ring current is much less than the catalyst obtained in example 6. H is calculated by the LSV test result of (a) diagram 2 O 2 Selectivity As shown in FIG. (b), coN/C catalyzes the ORR Process H 2 O 2 Selectivity is less than 30%, indicating that the ORR experiences 4 electron paths. Example 6 CoNO/C catalyzed ORR Process H by ozone post-treatment due to structural remodeling of the active sites 2 O 2 Is selectively achievedAbove 90%, it indicates that 2 electron paths are experienced by the ORR.
Claims (8)
1. A carbon supported Co-based monatomic catalyst for ORR 2 electron pathway, wherein the carbon supported Co-based monatomic catalyst has the structural formula:
2. a method for regulating and controlling an active site of a carbon-supported Co-based monatomic catalyst takes the Co-based monatomic catalyst as an object to regulate and control an active center deliberately, and is characterized by comprising the following steps:
step (1): preparation of carbon-supported Co-based monatomic catalyst CoN/C
1)NaCl、ZnCl 2 Uniformly mixing the carbon precursor and the Co precursor; mixing in a ball milling mode, wherein the ball milling time is 5-120min and 200-1000 rpm, and a ball milling tank is sealed and kept dry;
NaCl and ZnCl 2 Is not more than 1,NaCl to ZnCl 2 The mass ratio of the sum of the two to the carbon precursor is 50-1, and the mass ratio of the Co precursor to the carbon precursor is 0.005-0.05;
the carbon precursor is adenine or hypoxanthine;
2) Heating the uniformly mixed materials for 0.5 to 5 hours in an inert atmosphere at the temperature of between 700 and 1100 ℃, and then cooling;
3) Taking out the heated material, heating and stirring the heated material in dilute hydrochloric acid with the temperature of 50-150 ℃ and the concentration of 0.1-3M for 3-24 h, and washing off reaction residues;
4) Filtering and drying the solution to obtain a carbon-supported Co-based monatomic catalyst CoN/C;
step (2): performing structure regulation on the carbon-supported Co-based monatomic catalyst CoN/C active site obtained in the step (1) to obtain CoNO/C;
1) Dissolving the carbon-supported Co-based monatomic catalyst prepared in the step (1) in deionized water, wherein the carbon-supported Co-based Shan YuanThe concentration of the sub-catalyst is 0.1-5 mg/ml -1 Uniformly mixing in an ultrasonic and stirring combined mode;
2) Introducing ozone for 10-240 min while stirring in a bubbling mode until the color of the solution changes;
3) Centrifuging at high speed to remove most of the supernatant, and collecting the lower layer precipitate;
4) Heating and washing in dilute hydrochloric acid with the temperature of 50-150 ℃ and the concentration of 0.1-3M for 3-24 h, obtaining a precipitate, filtering, and drying to obtain the catalyst CoNO/C with the adjusted active site.
3. A control method according to claim 2, wherein in step (1), the Co precursor is Co powder, a metal oxide of Co, or a Co salt.
4. The control method according to claim 2 or 3, wherein in the step (1), the inert atmosphere is Ar gas or N 2 And (4) air atmosphere.
5. A regulating and controlling method according to claim 2 or 3, characterized in that in the step (2), the ultrasonic power is 500W, the frequency is 35-40 kHz, and the ultrasonic time is 5-60 min; the stirring speed is 200-1000 rpm, and the time is 5-60 min.
6. The method according to claim 5, wherein in the step (2), the centrifugal rotation speed is 8000rpm to 50000rpm.
7. The use of a Co-based monatomic catalyst on carbon in ORR 2 for the electronic pathway of ORR, according to claim 1, wherein the steps are as follows:
1) Adding a catalyst CoNO/C into a mixed solution of ethanol and Nafion, performing ball milling and then ultrasonic treatment, and uniformly mixing in a ball milling and ultrasonic treatment combined mode to obtain catalyst ink;
the ball milling time is 0.5 to 3 hours, and the rotating speed is 200 to 1000rpm;
the ultrasonic power is 500W, the frequency is 35-40 kHz, and the time is 0.5-5 h;
the concentration of catalyst CoNO/C is 0.5-10 mg/ml -1 The volume ratio of Nafion to ethanol is 0.01-0.06;
2) The catalyst ink is dripped on the electrode of the rotating ring disk, and the loading capacity of the catalyst is 0.01-10 mg cm -2 Naturally drying to obtain a catalyst film;
3) Introducing O into electrolyte solution 2 To O in the electrolyte solution 2 Saturation;
4) Applying the electrode coated with the catalyst film to O 2 Testing LSV curve in saturated solution, and continuously introducing O in the testing process 2 And calculating H from the LSV curve 2 O 2 Selectivity, and thus define the ORR reaction pathway;
the rotating speed is set to be 400-2500 rpm, and the ring disk electrode H 2 O 2 The collection coefficient is 0.37, the applied potential of the ring electrode is 1.0-1.5V vs.RHE, the test range is 0-1.2V vs.RHE, and the scanning speed is 0.001-1 V.s -1 。
8. Use according to claim 7, wherein the electrolyte solution is 0.1M HClO 4 Solution, 0.5M H 2 SO 4 Solution or 0.1M KOH solution.
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