CN115839991B - In-situ monitoring method for stability of iridium-based oxygen evolution electrocatalyst - Google Patents
In-situ monitoring method for stability of iridium-based oxygen evolution electrocatalyst Download PDFInfo
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Abstract
The invention belongs to the technical field of electrochemistry, and discloses an in-situ monitoring method for stability of an iridium-based oxygen evolution electrocatalyst. The in-situ monitoring method comprises the following steps: preparing slurry of an iridium-based oxygen evolution electrocatalyst, coating the slurry on the surface of a disk electrode of a rotary disk ring disk electrode, and drying to obtain an oxygen evolution electrocatalyst layer; immersing a rotating disc ring electrode into electrolyte solution, introducing inert gas into the electrolyte solution, testing an alternating current impedance spectrum or a high-frequency internal resistance value of open-circuit potential in a static state of the rotating disc ring electrode, and realizing the stabilization and activation of the surface of an oxygen evolution electrocatalytic layer by a cyclic voltammetry; rotating the ring electrode of the rotary circular disk, applying a potential of 0.7-1.25V vs. RHE to the ring electrode, performing linear volt-ampere scanning, potentiostatic method or chronoamperometry to the disk electrode to test oxygen evolution activity of the oxygen evolution electrocatalytic layer, and monitoring ring current data. The method has reliable test results and can realize repeatability measurement and visual experimental results.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to an in-situ monitoring method for stability of an iridium-based oxygen evolution electrocatalyst.
Background
In the electrochemical field, the anodic Oxygen Evolution Reaction (OER) is one of key reactions of technologies such as water electrolysis hydrogen production, carbon dioxide electrochemical reduction, solar water decomposition, renewable fuel cells and the like, however, the slow dynamic process restricts the improvement of the reaction efficiency of the system. The development of anode oxygen evolution reaction catalysts with low cost, high efficiency, long term stability is still challenging. In particular, the iridium-based oxygen evolution electrocatalyst represented by iridium black, iridium oxide and iridium-M composite metal oxide under acidic conditions is the only catalyst capable of meeting the requirements of activity and stability. However, iridium is one of the rarest and most expensive elements in the crust, as a noble metal of the platinum group, with global yields of less than 9 tons/year. Most of the research on iridium-based oxygen evolution electrocatalysts is mainly focused on improving the activity and reducing the material cost, and only a few people focus on evaluation and improvement strategies of the stability of the iridium-based oxygen evolution electrocatalysts.
To evaluate the electrocatalyst anode oxygen evolution reactivity and stability, the prior art generally uses Rotating Disk Electrodes (RDEs) or Membrane Electrodes (MEA). The rotary disk electrode is convenient and simple to test, has low cost of raw materials, cannot explain the performance attenuation mechanism of the electrocatalyst, has large difference from practical application, and can lead to erroneous conclusion due to small changes of experimental results when different electrolytes, electrode materials or different batteries are adopted. Membrane electrode evaluation, while approaching practical application, is more complex and takes longer. And the stability of the rotating disc electrode and the membrane electrode to the anode oxygen evolution reaction of the electrocatalyst can be evaluated only after the accelerated decay test or the long-time life test, and the electrolyte solution or the electrode catalytic layer can not be sampled and analyzed, so that the stability of the electrocatalyst can not be accurately evaluated in situ.
Accordingly, there is a need to provide a new method for evaluating or monitoring the stability of iridium-based oxygen evolution electrocatalyst.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides an in-situ monitoring method for the stability of an iridium-based oxygen evolution electrocatalyst. The in-situ monitoring method is suitable for the real-time evaluation of the stability (or stability and activity) of the iridium-based oxygen evolution electrocatalyst in an electrolyte solution system. In a four-electrode solution system of a rotating disk ring electrode (RRDE), the oxygen evolution stability of an iridium-based oxygen evolution electrocatalyst is monitored and evaluated in situ by the current response of a given potential across the ring electrode. The method aims to solve the problems that the operation process is complicated, the time consumption is long, and the stability and the activity of the catalyst cannot be rapidly and accurately represented in the stability evaluation of the electrocatalyst.
The in-situ monitoring method for the stability of the iridium-based oxygen evolution electrocatalyst combines the advantages of the traditional three-electrode rotating disk electrode RDE system for quickly and simply detecting the oxygen evolution activity of the catalyst, effectively avoids the bottleneck caused by mass transmission limitation or conductivity under a double-electrode Membrane Electrode Assembly (MEA) system, and provides a relatively reasonable testing method, experimental parameters and testing system based on a four-electrode rotating disk electrode RRDE framework for the oxygen evolution catalyst activity and stability, and the benchmark test of the oxygen evolution catalyst activity and stability is realized under the condition of simulating an electrolytic cell, so that the guarantee is provided for designing a better catalyst.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
specifically, the in-situ monitoring method for the stability of the iridium-based oxygen evolution electrocatalyst comprises the following steps:
(1) Preparing slurry of an iridium-based oxygen evolution electrocatalyst, coating the slurry on the surface of a disk electrode of a rotary disk ring disk electrode, and drying to obtain an oxygen evolution electrocatalyst layer;
(2) Immersing a rotating disc ring electrode into electrolyte solution, introducing inert gas into the electrolyte solution, testing an alternating current impedance spectrum or a high-frequency internal resistance value of open-circuit potential in a static state of the rotating disc ring electrode, and realizing the stabilization and activation of the surface of an oxygen evolution electrocatalytic layer by a cyclic voltammetry;
(3) Rotating a rotary circular disc electrode, applying potential to the circular electrode, performing linear volt-ampere scanning, potentiostatic method or chronoamperometry on the circular electrode to test oxygen evolution activity of an oxygen evolution electrocatalytic layer and monitoring circular current data;
in the step (3), the potential applied to the ring electrode is in the range of 0.7 to 1.25V vs. RHE.
Preferably, an in-situ monitoring method for stability of iridium-based oxygen evolution electrocatalyst comprises the following steps:
(1) Mixing an iridium-based oxygen evolution electrocatalyst, a binder and a solvent to obtain slurry, coating the slurry on the surface of a disk electrode of a rotary disk ring disk electrode, and drying to obtain the surface of the disk electrode of the rotary disk ring disk electrode to form an oxygen evolution electrocatalyst layer;
(2) Immersing the rotating disc ring electrode obtained in the step (1) into electrolyte solution, continuously introducing inert gas into the electrolyte solution, testing the alternating current impedance spectrum or the high-frequency internal resistance value of open-circuit potential in a static state of the rotating disc ring electrode, and then realizing the stabilization and activation of the surface of the oxygen evolution electro-catalytic layer by Cyclic Voltammetry (CV);
(3) Rotating the ring plate electrode of the rotating circular plate, applying potential to the ring electrode in the ring plate electrode of the rotating circular plate, performing linear volt-ampere scanning, potentiostatic method or chronoamperometry on the plate electrode of the ring plate electrode of the rotating circular plate to test the oxygen evolution activity of the oxygen evolution electro-catalytic layer and monitoring ring current data, and synchronously monitoring and evaluating the activity and stability of the iridium-based oxygen evolution electro-catalyst according to the current response characteristics of the plate electrode and the ring electrode.
Preferably, in the step (1), the iridium-based oxygen evolution electrocatalyst is an iridium-based catalyst of metallic iridium, iridium oxide and Ir-M composite metal oxide, wherein M is at least one of Ru, pt, mn, fe, co, ni, se, mo, W.
Preferably, in the step (1), the binder is a perfluorosulfonic acid polymer, for example, perfluorosulfonic acid ionomer represented by Nafion (r) manufactured by Dupont company.
Preferably, in the step (1), the solvent is a mixed solvent of ethanol or isopropanol and water (or deionized water).
Preferably, in the step (1), the rotary circular disc ring electrode includes a disc electrode and a ring electrode, the center is the disc electrode and the outer ring is the ring electrode, and an electrical isolation insulating ring is arranged between the disc electrode and the ring electrode.
Preferably, in the step (1), the load of the iridium-based oxygen evolution electrocatalyst in the oxygen evolution electrocatalyst layer on the surface of the disk electrode is 0.03-2mg/cm 2 Preferably 0.05-1mg/cm 2 。
Preferably, in the step (2), the electrolyte solution is an acid solution or an alkali solution of 0.1 to 1 mol/L.
Preferably, the acid solution comprises a sulfuric acid solution or a perchloric acid solution.
Preferably, the alkali solution comprises a potassium hydroxide solution or a sodium hydroxide solution.
Preferably, in the step (2), the potential of the Cyclic Voltammetry (CV) is set in a range of 0-1.4V (vs. RHE reversible hydrogen electrode), the potential sweeping speed is 50-500mV/s, and the number of sweeping turns is not less than 10.
Preferably, in the step (2), the rotating disk ring electrode is immersed in the electrolyte solution together with the counter electrode and the reference electrode.
Preferably, the counter electrode is a graphite, platinum or gold electrode having a larger surface area than the rotating disk ring electrode.
Preferably, the reference electrode is selected from any one of a saturated calomel electrode, an Ag/AgCl electrode, an Hg/HgO electrode, an Hg/Hg2SO4 electrode or a standard hydrogen electrode.
Preferably, the counter electrode, the reference electrode, the disk electrode in the rotary disk ring disk electrode and the ring electrode form a four-electrode system, and are immersed into electrolyte solution together, and are connected and controlled through a double-constant potential rectifier or a multi-channel electrochemical workstation.
Preferably, in step (2), the inert gas is selected from nitrogen or a rare gas.
In step (2), the ac impedance spectrum or high frequency internal resistance value of the open circuit potential is tested to ensure that the additional resistance caused by the electrode lines or connections is within a reasonable range.
Preferably, in step (3), the rotational speed of the rotating disc ring electrode is 400 to 4000 rpm, preferably 500 to 3000 rpm.
Preferably, in the step (3), the rotating disc ring electrode is rotated, and the potential is applied to the ring electrode in the rotating disc ring electrode, wherein the potential applied to the ring electrode is in the range of 0.8-1.2v vs. rhe.
The principle of testing the change of the ring current given the ring electrode potential in the above step (3): when the iridium-based oxygen evolution electrocatalyst participates in the oxygen evolution reaction, the valence change of Ir ions is an important reason for the stability attenuation of the iridium-based oxygen evolution electrocatalyst. At a certain rotating disk electrode rotating speed, a part of high-valence Ir ions generated by the attenuation of the iridium-based oxygen evolution electrocatalyst can diffuse from the disk electrode to the ring electrode position along with the convection of the electrolyte solution. Therefore, when a proper potential is applied to the ring electrode, the Ir ions in high valence state can be reduced and a reduction current can be generated. The reduction current of the ring electrodes of different iridium-based oxygen evolution electrocatalysts is compared under the condition of given ring electrode potential, and the on-line monitoring and evaluation of the electrocatalytic stability of each iridium-based oxygen evolution electrocatalyst to be tested can be completed while the catalytic activity of the iridium-based oxygen evolution electrocatalyst is evaluated. The larger the ring current of the iridium-based oxygen evolution electrocatalyst to be detected is, the larger the stability attenuation is, and the poorer the stability is when oxygen evolution reaction occurs.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention expands the application range of the rotary circular disk ring electrode, fully utilizes the special structure that the disk electrode and the ring electrode are mutually independent in the rotary circular disk ring electrode, and monitors and evaluates the stability of the oxygen evolution electrocatalytic layer at the disk electrode on line through the high valence ion reduction current response generated by applying specific potential on the ring electrode and due to the stability attenuation of the iridium-based oxygen evolution electrocatalytic agent. The invention provides a complete electrocatalytic performance evaluation method, wherein a pretreatment program comprises an impedance spectrum test or a high-frequency internal resistance test under an open circuit potential, so that additional resistance caused by a circuit or connection is ensured to be in a reasonable range, and meanwhile, the surface activation of an electrode is realized through repeated CV scanning, so that the problem of unstable surface of the electrode is effectively avoided, the experimental result is more reliable and repeatable, and the repeatable measurement of different oxygen evolution catalysts can be realized.
(2) The in-situ monitoring method provided by the invention has the advantages that the cost of experimental materials is low, the operation process is simple, the experimental result is visual, and the problems that the stability evaluation time is long, the operation process is complicated, and the stability data of the iridium-based oxygen evolution electrocatalyst cannot be quantitatively obtained in-situ on line in the prior general technology are solved. Meanwhile, the invention can also be suitable for evaluating the activity and stability of other metal and metal oxide electrocatalysts under a liquid electrolyte system, and expands the application range of the electrocatalyst.
(3) In the in-situ monitoring method, raw materials such as the binder, the solvent, the reference electrode, the counter electrode and the like used in the experiment can be obtained commercially, and the acquisition channels are various. Commercial RRDE (such as PINE company) adopts high-quality materials, has uniform density and stable chemical performance, and can ensure that each electrode has the same characteristic by assisting with a precise mature processing technology.
Drawings
FIG. 1 is a graph showing the stability test of iridium-based oxygen evolution electrocatalysts according to example 1, example 8, comparative example 1, and comparative example 2 of the present invention;
FIG. 2 is a graph showing the stability test of iridium-based oxygen evolution electrocatalysts according to example 1, example 2 and example 3 in an acidic medium;
FIG. 3 is a graph showing the stability test of iridium-based oxygen evolution electrocatalysts according to example 4, example 5, and example 6 of the present invention in alkaline medium.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
The binder used in the following is Nafion ionomer which is produced by Dupont and is represented by Nafion.
The rotating disk ring electrode (RRDE) is supplied by PINE Inc. USA and is model E6R2.
Example 1
An in-situ monitoring method for the stability of an iridium-based oxygen evolution electrocatalyst, comprising the following steps:
(1) IrMnO is added to x Catalyst (i.e. Ir-Mn composite metal oxide iridium-based catalyst, wherein the subscript x of O in the catalyst has the function of balancing valence, the specific value of x is not required to be given in the field, the catalyst is similarly expressed), powder, nafion ionomer, isopropanol and water are sequentially placed in a 20mL sample bottle and are subjected to ultrasonic treatment for 30min, so as to obtain uniformly mixed slurry, wherein IrMnO is prepared by x The mass ratio of the catalyst to the Nafion ionomer is 2:1, the mass ratio of isopropanol to water is 9:1. then the slurry is coated on the surface of a disk electrode of a rotary disk ring disk electrode (RRDE), and is sufficiently dried, and the surface of the disk electrode of the obtained rotary disk ring disk electrode forms an oxygen evolution electro-catalytic layer, and IrMnO on the surface of the disk electrode x The loading of the catalyst was 0.08mg/cm 2 ；
(2) Immersing the rotating disk ring electrode obtained in the step (1) into a sulfuric acid electrolyte solution of 0.5mol/L, and immersing N 2 Continuously introducing sulfuric acid electrolyte solution (the obtained electrolyte solution is called inert gas saturated electrolyte solution), testing alternating current impedance spectrum of open-circuit potential under the static state of a rotating disc ring electrode, and then realizing the stabilization and activation of the surface of an oxygen evolution electro-catalytic layer through Cyclic Voltammetry (CV), wherein the potential of the Cyclic Voltammetry (CV) is set in a range of 0.4-1.4V (vs. RHE reversible hydrogen electrode), the potential sweeping speed range is 300mV/s, and the number of scanning turns is not lower than 10 turns;
(3) Immersing a counter electrode (the counter electrode is a graphite electrode) and a reference electrode (the reference electrode is a saturated calomel electrode) into electrolyte solution, connecting and controlling a multi-channel electrochemical workstation, rotating a rotary disc ring electrode (the rotating speed of the rotary disc ring electrode is 1500 revolutions per minute), applying a potential to the ring electrode in the rotary disc ring electrode, applying a potential of 0.9V (vs. RHE) to the ring electrode, performing linear voltammetric scanning (LSV) of 1.35-1.6V to the disc electrode of the rotary disc ring electrode, testing oxygen evolution activity of an oxygen evolution electrocatalytic layer, monitoring ring current data, and synchronously monitoring and evaluating the activity and stability of the iridium-based oxygen evolution electrocatalytic according to current response characteristics of the disc electrode and the ring electrode.
Example 2
Example 2 differs from example 1 only in that IrFeO is used in example 2 x Catalyst replaces IrMnO in example 1 x A catalyst.
Example 3
Example 3 differs from example 1 only in that IrCoO is used in example 3 x Catalyst replaces IrMnO in example 1 x A catalyst.
Example 4
Example 4 differs from example 1 only in that Ir is used in example 4 0.8 Co 0.2 O x Catalyst replaces IrMnO in example 1 x Catalyst, and in example 4, 0.5mol/L sulfuric acid electrolyte solution in example 1 was replaced with 1mol/L KOH electrolyte solution.
Example 5
Example 5 differs from example 4 only in that Ir is used in example 5 0.4 Co 0.6 O x Catalyst replaces Ir in example 4 0.8 Co 0.2 O x A catalyst.
Example 6
Example 6 differs from example 1 only in that Ir is used in example 6 0.2 Co 0.8 O x Catalyst replaces IrMnO in example 4 x A catalyst.
Example 7
Example 7 differs from example 1 only in that commercial IrO is used in example 7 x The IrMnOx catalyst in example 1 was replaced by a catalyst (model 043396, supplied by Alfa Aesar Alfa inc.).
Example 8
Example 8 differs from example 1 only in that in step (3) of example 8, the potential applied to the ring electrode is 1.1V (vs. rhe).
Comparative example 1
In comparison with example 7, comparative example 1 differs only in that O is used in step (2) of comparative example 1 2 Instead of N in example 1 2 。
Comparative example 2
The difference of comparative example 2 compared with comparative example 1 is only that in step (3) of comparative example 2, the potential applied to the ring electrode is 1.1V (vs. rhe).
Effect testing
FIG. 1 is a graph showing the stability test of iridium-based oxygen evolution electrocatalysts according to example 1, example 8, comparative example 1, and comparative example 2 of the present invention; as can be seen from fig. 1, in the oxygen-saturated electrolyte solution systems (comparative examples 1 and 2), the ring current remains zero after the potential is applied to the ring electrode, indicating that the current generated by the oxygen reduction (ORR) reaction is not represented in the form of the ring current, and the interference of the ORR current on the reduction current generated by the reduction of high valence ions is eliminated. After eliminating ORR current interference, in the nitrogen saturated electrolyte solution system (example 1, example 8), different ring electrode potentials were applied at the same disk electrode potential, with a reduction current at 0.9V potential greater than that at 1.1V potential. The method directly reflects that different potentials on the ring electrode can influence the observation of the reduction current, and is more suitable for the observation of the reduction current under the potential of the ring electrode of 0.9V, so as to monitor and evaluate the on-line stability of the catalyst to be tested.
FIG. 2 is a graph showing the stability test of iridium-based oxygen evolution electrocatalysts according to example 1, example 2 and example 3 in an acidic medium.
FIG. 2 shows that the Ir-M complex metal oxide is at N at a ring electrode potential of 0.9V 2 The stability test curve of the iridium-based oxygen evolution electrocatalyst in saturated sulfuric acid electrolyte solution of 0.5mol/L shows that the in-situ evaluation method of the stability is feasible in an acidic environment.
Meanwhile, after different transition metal elements are added, the oxygen evolution activity sequence of each iridium-based oxygen evolution electrocatalyst can be found by a linear scanning curve on a disk electrode: example 1≡example 3> example 2.
FIG. 3 is a graph showing the stability test of iridium-based oxygen evolution electrocatalysts according to example 4, example 5, and example 6 of the present invention in alkaline medium.
As can be seen from FIG. 3, ir-Co composite metal oxide iridium-based oxygen evolution electrocatalyst (example 4, example 5, example 6) at 0.9V ring electrode voltage was shown in N 2 The electrocatalytic stability test curves in saturated 1mol/L KOH electrolyte solution show that the stability evaluation method disclosed by the invention is still feasible in alkaline environment.
Claims (5)
1. An in-situ monitoring method for the stability of an iridium-based oxygen evolution electrocatalyst is characterized by comprising the following steps:
(1) Mixing an iridium-based oxygen evolution electrocatalyst, a binder and a solvent to obtain slurry, coating the slurry on the surface of a disk electrode of a rotary disk ring disk electrode, and drying to obtain the surface of the disk electrode of the rotary disk ring disk electrode to form an oxygen evolution electrocatalyst layer;
(2) Immersing the rotating disc ring electrode obtained in the step (1) into electrolyte solution, continuously introducing inert gas into the electrolyte solution, and testing the alternating current impedance spectrum or the high-frequency internal resistance value of open-circuit potential in a static state of the rotating disc ring electrode, so as to realize the stabilization and activation of the surface of the oxygen evolution electrocatalytic layer through cyclic voltammetry;
(3) Rotating a rotating disc ring electrode, applying potential to a ring electrode in the rotating disc ring electrode, performing linear volt-ampere scanning, potentiostatic method or chronoamperometry on the disc electrode of the rotating disc ring electrode to test oxygen evolution activity of an oxygen evolution electro-catalytic layer and monitor ring current data, and synchronously monitoring and evaluating activity and stability of the iridium-based oxygen evolution electro-catalyst according to current response characteristics of the disc electrode and the ring electrode;
in the step (3), the potential applied to the ring electrode is 0.9V vs. RHE;
the iridium-based oxygen evolution electrocatalyst is an iridium-based catalyst of an Ir-M composite metal oxide, wherein M is at least one of Ru, pt, mn, fe, co, ni, se, mo, W;
in the step (2), the electrolyte solution is an acid solution or an alkali solution with the concentration of 0.1-1 mol/L; the acid solution is sulfuric acid solution;
in the step (2), the rotary circular disc electrode is matched with a counter electrode and a reference electrode and is immersed in electrolyte solution;
the counter electrode is a graphite, platinum or gold electrode with larger surface area than the rotating circular disk ring electrode; the reference electrode is selected from saturated calomel electrode, ag/AgCl electrode, hg/HgO electrode, hg/Hg 2 SO 4 Either an electrode or a standard hydrogen electrode.
2. The in-situ monitoring method according to claim 1, wherein in the step (1), the load of iridium-based oxygen evolution electrocatalyst in the oxygen evolution electrocatalyst layer on the surface of the disk electrode is 0.03-2mg/cm 2 。
3. The in-situ monitoring method according to claim 1, wherein in the step (2), the potential of the cyclic voltammetry is set in a range of 0-1.4v vs. rhe, the potential sweep speed is 50-500mV/s, and the number of sweep cycles is not less than 10.
4. The in-situ monitoring method of claim 1, wherein the counter electrode, the reference electrode, and the disk electrode and the ring electrode in the rotating disk ring disk electrode form a four-electrode system, are immersed in an electrolyte solution together, and are connected and controlled by a double potentiostat or a multi-channel electrochemical workstation.
5. The in-situ monitoring method of claim 1, wherein in step (3), the rotational speed of the rotating disk ring electrode is 400-4000 rpm.
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