CN109900765B - Electrochemical testing device and method with controllable mass transfer on electrode surface - Google Patents
Electrochemical testing device and method with controllable mass transfer on electrode surface Download PDFInfo
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Abstract
The invention provides an electrochemical testing device with controllable electrode surface mass transfer and a method thereof. The multi-port electrolytic cell in the electrochemical test system comprises a liquid outlet, a liquid inlet, a nozzle hole, an air inlet, an air outlet, a working electrode fixing port, a counter electrode fixing port and a reference electrode fixing port, the flow rate control system comprises a valve, a flowmeter, an acid and alkali resistant silicone tube, a miniature circulating liquid supply pump and an air duct, and the data acquisition system comprises an electrochemical workstation, a computer, an electrode wire and a data line. The testing method by using the device realizes the accurate regulation and control of the mass transfer on the surface of the electrode and accelerates the desorption of the product on the surface of the electrode; the device has the advantages of improving the liquid phase mass transfer rate, fully exerting the catalytic capability of the catalyst, realizing the electrochemical performance research of the catalyst in common electrolyte and obtaining a performance curve with good regularity and reproducibility, along with low cost and easy construction compared with the traditional device.
Description
Technical Field
The present invention relates to an electrochemical test device; in particular to an electrochemical testing device and method with controllable mass transfer on the surface of an electrode.
Background
Since the forty years of the last century, with the continuous and deep research in the field of electrochemical science, people have recognized that the field of electrode reactions is mainly concentrated on the surface area of electrodes, and that such reactions mainly include two processes, namely, the mass transfer process of reactants from a liquid phase to the surface of electrodes and the substance conversion process of the surfaces of electrodes.
The method for effectively improving the surface mass transfer rate of the electrode adopts a rotating disc electrode as a working electrode, combines a counter electrode and a reference electrode, and forms an electrochemical testing device together with an electrochemical workstation and a computer. When the electrode works, a catalyst is dripped on the surface of the disc electrode, the centrifugal force generated by the rotation of the disc electrode is utilized to improve the diffusion speed of a reactant in the electrolyte to a catalyst layer on the surface of the electrode, so that the electrolyte containing the reactant is fully contacted with the catalyst on the surface of the disc electrode, and the liquid-phase mass transfer rate of the reactant in the electrolyte to the catalyst layer on the surface of the electrode is improved (Zhong et al, Journal of environmental Sciences,2008, 20, 927-. However, the above-mentioned test device has high requirements on the design and processing of the rotating disk electrode, particularly on the electrode geometry, the sealing and electrode lead-out system, which inevitably increases the cost of the whole electrochemical test device. Meanwhile, in order to objectively evaluate the activity of the catalyst, a sufficient mass transfer rate on the surface of the electrode needs to be provided, so that the rotating disk electrode needs to keep a high rotating speed (usually more than or equal to 1000 rpm) when in work, and serious damage to a reference electrode or a counter electrode is likely to be caused if the rotating disk electrode is not operated properly. Therefore, the problem to be solved at present is to find an electrochemical testing device with controllable electrode surface mass transfer, which has low testing cost, high safety, good stability and is easy to build.
Disclosure of Invention
The invention provides an electrochemical testing device and method with controllable electrode surface mass transfer, which are used for controlling the mass transfer rate of the electrode surface and solving the problems of complexity, high cost, poor safety and stability, easiness in repairing and the like of the conventional device.
The invention provides an electrochemical testing device with controllable electrode surface mass transfer, which comprises an electrochemical testing system 5, a flow velocity control system and a data acquisition system,
the electrochemical test system 5 comprises a multi-port electrolytic cell, and the multi-port electrolytic cell is provided with a liquid outlet 5-1, a liquid inlet 5-2, a nozzle hole 5-3, a gas inlet 5-4, a gas outlet 5-5, a working electrode fixing port 5-6, a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
the flow rate control system comprises a valve 1, a flowmeter 2, an air duct 3, a micro circulating liquid supply pump 4 and an acid and alkali resistant silicone tube 6;
the data acquisition system comprises an electrochemical workstation 7, a computer 8, an electrode lead 9 and a data line 10;
wherein, the valve 1 and the flowmeter 2 are connected with the air inlet 5-4 of the multi-port electrolytic cell through the air duct 3; the liquid inlet end of the micro circulating liquid supply pump 4 is connected with the liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, and the liquid outlet end is connected with the liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6; the working electrode 5-9, the counter electrode 5-10 and the reference electrode 5-11 are fixed in the multi-port electrolytic cell through the working electrode fixing port 5-6, the counter electrode fixing port 5-7 and the reference electrode fixing port 5-8 and are connected with the electrochemical workstation 7 through an electrode lead 9, and the electrochemical workstation 7 is connected with the computer 8 through a data line 10.
The valve 1 is used for controlling the closing or opening of the gas circuit, and the flow meter 2 is used for controlling the flow rate of the gas; the gas is oxygen, nitrogen or argon.
The miniature circulating liquid supply pump 4 is a constant-flow peristaltic pump, a miniature diaphragm pump or a miniature self-priming pump.
The invention relates to a measuring method realized by an electrochemical testing device with controllable electrode surface mass transfer, which comprises the following steps:
electrolyte is filled in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow rate of gas introduced into the electrolyte is controlled by the flowmeter 2, meanwhile, a liquid inlet end of a miniature circulating liquid supply pump 4 is connected with a liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, a liquid outlet end of the miniature circulating liquid supply pump is connected with a liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, a power supply of the miniature circulating liquid supply pump is opened, the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and the flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting the working electrode 5-9 coated with the catalyst on the surface of the electrode core into the working electrode fixing port 5-6 to ensure that the working electrode faces the nozzle hole 5-3 and the distance between the working electrode and the nozzle hole is adjusted, controlling the mass transfer flow rate of the electrolyte on the surface of the electrode core through the micro circulating liquid supply pump 4, and fixing the counter electrode 5-10 and the reference electrode 5-11 in the counter electrode fixing port 5-7 and the reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with the electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with the computer 8 through a data line 10, a starting program is used for collecting data, and after the electrochemical test is finished, a catalyst performance curve can be obtained.
The electrolyte is 0.1mol/L KOH and 0.1mol/L HCIO4、1 mol/L H2SO4Or 1mol/L KOH.
The distance between the surface of the electrode core of the working electrode 5-9 and the nozzle hole 5-3 is 0.2-2 mm, and the diameter of the electrode core of the working electrode 5-9 is 3-5 mm.
The diameter of the nozzle hole 5-3 is 0.5-1 mm.
The controllable electrode surface mass transfer flow rate range of the micro circulating liquid supply pump 4 in the flow rate control system is 0-120 mL/min.
The invention has the following beneficial effects:
the electrochemical testing device and the method have good applicability, and can finish the electrochemical testing of the catalyst in common electrolyte (such as 0.1mol/L KOH and 0.1mol/L HCIO)4Etc.) in the electrochemical cell. The micro circulating liquid supply pump 4 is used for controlling the mass transfer flow rate of the electrolyte on the surface of the working electrode in the electrochemical test system 5, so that the desorption of a product on the surface of the electrode can be accelerated, the liquid phase mass transfer rate is improved, and the catalytic capability of the catalyst on the surface of the electrode is fully exerted. Compared with a traditional test system with a rotary disk electrode as a working electrode, the electrochemical test device is low in cost and easy to build, evaluation and research on the performance of the catalyst can be completed only by using various common electrodes (such as glassy carbon electrodes) with the thickness of 3-5 mm as the working electrode, and the obtained performance curve has good regularity and reproducibility.
Drawings
FIG. 1 shows that when the mass transfer flow rate of oxygen-containing electrolyte on the surface of an electrode is controlled by using a constant-current peristaltic pump, commercial platinum-carbon catalysts are used in (a) 0.1mol/L KOH and (b) 0.1mol/L HCIO4Oxygen reduction (ORR) performance polarization curve in electrolyte.
FIG. 2 shows the mass transfer flow rate of oxygen-containing electrolyte on the electrode surface controlled by a micro-diaphragm pump under conditions of (a) 0.1mol/L KOH and (b) 0.1mol/L HCIO4ElectrolysisOxygen reduction in liquid (ORR) performance polarization curve.
FIG. 3 shows the mass transfer flow rate of oxygen-containing electrolyte on the electrode surface controlled by miniature self-priming pump using commercial platinum-carbon catalyst at (a) 0.1mol/L KOH and (b) 0.1mol/L HCIO4Oxygen reduction (ORR) performance polarization curve in electrolyte.
Curves A, B, C, D, E and F in FIGS. 1, 2, and 3 represent polarization curves for oxygen reduction (ORR) performance at electrode surface mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min, respectively.
FIG. 4 is a polarization curve of electrochemical Oxygen Evolution (OER) performance of a commercial ruthenium oxide catalyst in a 1mol/L KOH electrolyte using different micro-circulating liquid supply pumps to control the mass transfer flow rate of the electrolyte. Wherein (a), (b) and (c) represent polarization curves of Oxygen Evolution (OER) performance measured using a constant-flow peristaltic pump, a micro diaphragm pump and a micro self-priming pump, respectively.
FIG. 5 is a schematic composition diagram of an electrochemical testing device with controllable electrode surface mass transfer according to the present invention
In fig. 5, 1 is a valve, 2 is a flowmeter, 3 is an air guide tube, 4 is a micro circulating liquid supply pump, 5 is an electrochemical testing system, 6 is an acid and alkali resistant silicone tube, 7 is an electrochemical workstation, 8 is a computer, 9 is an electrode lead, and 10 is a data line.
FIG. 6 is a front view of a multi-port electrolytic cell.
Figure 7 is a top view of a multi-port electrolytic cell.
The same reference numerals in fig. 6 and 7 are used to denote the same structures and elements, namely a liquid outlet 5-1, a liquid inlet 5-2, a nozzle hole 5-3, a gas inlet 5-4, a gas outlet 5-5, a working electrode fixing port 5-6, a counter electrode fixing port 5-7, a reference electrode fixing port 5-8, a working electrode 5-9, a counter electrode 5-10 and a reference electrode 5-11.
Detailed Description
The first embodiment is as follows: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
0.1mol/L KOH is filled in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct, the valve 1 is opened, the flow rate of oxygen introduced into electrolyte is controlled to be 20mL/min by utilizing the flowmeter 2, meanwhile, a liquid inlet end of a constant-current peristaltic pump is connected with a liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, a liquid outlet end of the constant-current peristaltic pump is connected with a liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, and a power supply of the constant-current peristaltic pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and a flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 4 mm) coated with a commercial platinum carbon catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 0.5 mm, adjusting the distance between the working electrode and the nozzle hole to be 1mm, controlling the mass transfer flow rate of the electrolyte on the surface of the electrode core by a constant-current peristaltic pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a starting program collects data, and after the electrochemical test is finished, an oxygen reduction (ORR) performance polarization curve of the commercial platinum-carbon catalyst can be obtained.
As shown in FIG. 1 (a), by applying the device of the present invention, oxygen reduction (ORR) performance polarization curves of commercial platinum-carbon catalysts at mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min can be obtained, and good regularity is provided, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate of the electrode surface, and complete the oxygen reduction (ORR) performance test of the catalyst in 0.1mol/L KOH.
The second embodiment is as follows: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
multiple electrolytic cells in the electrochemical test system 5 contain 0.1mol/L HCIO4The valve 1 and the flow meter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow meter 2 is utilized to control the flow rate of oxygen introduced into the electrolyte to be 20mL/min, meanwhile, the liquid inlet end of the constant-current peristaltic pump is connected with the liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, the liquid outlet end of the constant-current peristaltic pump is connected with the liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, and the power supply of the constant-current peristaltic pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical test system 5 and the flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 4 mm) coated with a commercial platinum carbon catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 0.5 mm, adjusting the distance between the working electrode and the nozzle hole to be 2mm, controlling the mass transfer flow rate of the electrolyte on the surface of the electrode core by a constant-current peristaltic pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a starting program collects data, and after the electrochemical test is finished, an oxygen reduction (ORR) performance polarization curve of the commercial platinum-carbon catalyst can be obtained.
As shown in FIG. 1 (b), by applying the device of the present invention, oxygen reduction (ORR) performance polarization curves of commercial platinum-carbon catalysts at mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min can be obtained with good regularity, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate on the surface of the electrode, and complete the catalyst at HCIO of 0.1mol/L4Oxygen reduction (ORR) performance test in (1).
The third concrete implementation mode: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
0.1mol/L KOH is contained in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow rate of oxygen introduced into electrolyte is controlled to be 20mL/min by utilizing the flowmeter 2, meanwhile, a liquid inlet end of a miniature diaphragm pump is connected with a liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, a liquid outlet end of the miniature diaphragm pump is connected with a liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, a power supply of the miniature diaphragm pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and a flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 5 mm) coated with a commercial platinum carbon catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 0.5 mm, adjusting the distance between the working electrode and the nozzle hole to be 1mm, controlling the mass transfer flow rate of electrolyte on the surface of the electrode core through a miniature diaphragm pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a starting program collects data, and after the electrochemical test is finished, an oxygen reduction (ORR) performance polarization curve of the commercial platinum-carbon catalyst can be obtained.
As shown in FIG. 2 (a), by applying the device of the present invention, oxygen reduction (ORR) performance polarization curves of commercial platinum-carbon catalysts at mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min can be obtained, and good regularity is provided, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate of the electrode surface, and complete the oxygen reduction (ORR) performance test of the catalyst in 0.1mol/L KOH.
The fourth concrete implementation mode: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
multiple ports in the electrochemical test system 50.1mol/L HCIO is contained in the electrolytic cell4The valve 1 and the flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow rate of oxygen introduced into electrolyte is controlled to be 20mL/min by using the flowmeter 2, meanwhile, the liquid inlet end of the miniature diaphragm pump is connected with the liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, the liquid outlet end of the miniature diaphragm pump is connected with the liquid inlet 5-2 through the acid and alkali resistant silicone tube 6, and the power supply of the miniature diaphragm pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical test system 5 and the flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 5 mm) coated with a commercial platinum carbon catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 0.5 mm, adjusting the distance between the working electrode and the nozzle hole to be 2mm, controlling the mass transfer flow rate of electrolyte on the surface of the electrode core through a miniature diaphragm pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a starting program collects data, and after the electrochemical test is finished, an oxygen reduction (ORR) performance polarization curve of the commercial platinum-carbon catalyst can be obtained.
As shown in FIG. 2 (b), by applying the device of the present invention, oxygen reduction (ORR) performance polarization curves of commercial platinum-carbon catalysts at mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min can be obtained with good regularity, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate on the surface of the electrode, and complete the catalyst at HCIO of 0.1mol/L4Oxygen reduction (ORR) performance test in (1).
The fifth concrete implementation mode: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
0.1mol/L KOH is filled in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow velocity of oxygen introduced into electrolyte is controlled to be 20mL/min by utilizing the flowmeter 2, meanwhile, a liquid inlet end of a micro self-priming pump is connected with a liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, a liquid outlet end of the micro self-priming pump is connected with the liquid inlet 5-2 through the acid and alkali resistant silicone tube 6, and a power supply of the micro self-priming pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and a flow velocity control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 4 mm) coated with a commercial platinum-carbon catalyst on the surface of the electrode core into a working electrode fixing port 5-6, enabling the working electrode to be opposite to a nozzle hole 5-3 with the diameter of 1mm, adjusting the distance between the working electrode and the nozzle hole to be 0.2 mm, controlling the mass transfer flow rate of electrolyte on the surface of the electrode core through a micro self-priming pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a starting program collects data, and after the electrochemical test is finished, an oxygen reduction (ORR) performance polarization curve of the commercial platinum-carbon catalyst can be obtained.
As shown in FIG. 3 (a), by applying the device of the present invention, an oxygen reduction (ORR) performance polarization curve of a commercial platinum-carbon catalyst under mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min can be obtained, and the device has good regularity, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate of the electrode surface, and complete the oxygen reduction (ORR) performance test of the catalyst in 0.1mol/L KOH.
The sixth specific implementation mode: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
multiple electrolytic cells in the electrochemical test system 5 contain 0.1mol/L HCIO4The valve 1 and the flowmeter 2 are connected with the air inlet 5-4 of the multi-port electrolytic cell through the air duct 3, the valve 1 is opened, and the flowmeter 2 is utilized to control the oxygen to be introduced into the electrolysisThe flow rate of the liquid is 20mL/min, meanwhile, the liquid inlet end of the miniature self-priming pump is connected with the liquid outlet 5-1 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, the liquid outlet end of the miniature self-priming pump is connected with the liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, and the power supply of the miniature self-priming pump is turned on, so that the electrolyte circularly flows in the device formed by the electrochemical test system 5 and the flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 4 mm) coated with a commercial platinum-carbon catalyst on the surface of the electrode core into a working electrode fixing port 5-6, enabling the working electrode to be opposite to a nozzle hole 5-3 with the diameter of 1mm, adjusting the distance between the working electrode and the nozzle hole to be 2mm, controlling the mass transfer flow rate of electrolyte on the surface of the electrode core through a micro self-priming pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a starting program collects data, and after the electrochemical test is finished, an oxygen reduction (ORR) performance polarization curve of the commercial platinum-carbon catalyst can be obtained.
As shown in FIG. 3 (b), by applying the device of the present invention, oxygen reduction (ORR) performance polarization curves of commercial platinum-carbon catalysts at mass transfer flow rates of 15 mL/min, 30 mL/min, 45 mL/min, 60 mL/min, 75 mL/min, and 90 mL/min can be obtained with good regularity, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate on the surface of the electrode, and complete the catalyst at HCIO of 0.1mol/L4Oxygen reduction (ORR) performance test in (1).
The seventh embodiment: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
1mol/L KOH is filled in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flowmeter 2 is used for controlling the flow rate of nitrogen introduced into electrolyte to be 10 mL/min, meanwhile, a liquid inlet end of a constant-current peristaltic pump is connected with a liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, a liquid outlet end of the constant-current peristaltic pump is connected with a liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, and a power supply of the constant-current peristaltic pump is turned on, so that the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and a flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 4 mm) coated with a commercial ruthenium oxide catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 0.5 mm, adjusting the distance between the working electrode and the nozzle hole to be 1mm, controlling the mass transfer flow rate of the electrolyte on the surface of the electrode core by a constant-current peristaltic pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a start-up program collects data, and after the electrochemical test is finished, the Oxygen Evolution (OER) performance polarization curve of the commercial ruthenium oxide catalyst can be obtained.
As shown in FIG. 4 (a), by applying the device of the present invention, Oxygen Evolution (OER) performance polarization curves of commercial ruthenium oxide catalysts at mass transfer flow rates of 0mL/min, 20mL/min, 40 mL/min, 60 mL/min, 80 mL/min, 100 mL/min and 120mL/min can be obtained, and good regularity is provided, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate of the electrode surface, and complete the performance test of the catalyst on Oxygen Evolution (OER) in 1mol/L KOH.
The specific implementation mode is eight: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
1mol/L KOH is filled in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow rate of introducing electrolyte into nitrogen is controlled to be 10 mL/min by utilizing the flowmeter 2, meanwhile, the liquid inlet end of a miniature diaphragm pump is connected with the liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, the liquid outlet end of the miniature diaphragm pump is connected with the liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, and the power supply of the miniature diaphragm pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and the flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 4 mm) coated with a commercial ruthenium oxide catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 1mm, adjusting the distance between the working electrode and the nozzle hole to be 1mm, controlling the mass transfer flow rate of electrolyte on the surface of the electrode core through a miniature diaphragm pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a start-up program collects data, and after the electrochemical test is finished, the Oxygen Evolution (OER) performance polarization curve of the commercial ruthenium oxide catalyst can be obtained.
As shown in FIG. 4 (b), by applying the device of the present invention, the polarization curve of Oxygen Evolution (OER) performance of the commercial ruthenium oxide catalyst under the mass transfer flow rates of 0mL/min, 20mL/min, 40 mL/min, 60 mL/min, 80 mL/min, 100 mL/min and 120mL/min can be obtained, and the device has good regularity, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate of the electrode surface, and complete the performance test of the catalyst on Oxygen Evolution (OER) in 1mol/L KOH.
The specific implementation method nine: the measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer in the embodiment comprises the following steps:
1mol/L KOH is filled in a multi-port electrolytic cell in an electrochemical testing system 5, a valve 1 and a flowmeter 2 are connected with an air inlet 5-4 of the multi-port electrolytic cell through an air duct 3, the valve 1 is opened, the flow rate of introducing electrolyte into nitrogen is controlled to be 10 mL/min by utilizing the flowmeter 2, meanwhile, the liquid inlet end of a miniature self-priming pump is connected with a liquid outlet 5-1 of the multi-port electrolytic cell through an acid and alkali resistant silicone tube 6, the liquid outlet end of the miniature self-priming pump is connected with a liquid inlet 5-2 of the multi-port electrolytic cell through the acid and alkali resistant silicone tube 6, and a power supply of the miniature self-priming pump is opened, so that the electrolyte circularly flows in a device formed by the electrochemical testing system 5 and a flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode 5-9 (the diameter of the electrode core is 3 mm) coated with a commercial ruthenium oxide catalyst on the surface of the electrode core into a working electrode fixing port 5-6 to ensure that the working electrode is opposite to a nozzle hole 5-3 with the diameter of 1mm, adjusting the distance between the working electrode and the nozzle hole to be 2mm, controlling the mass transfer flow rate of electrolyte on the surface of the electrode core by a micro self-priming pump, and simultaneously inserting a counter electrode 5-10 and a reference electrode 5-11 into a counter electrode fixing port 5-7 and a reference electrode fixing port 5-8;
(iii) the working electrodes 5-9, the counter electrodes 5-10 and the reference electrodes 5-11 are connected with an electrochemical workstation 7 through electrode leads 9, the electrochemical workstation 7 is connected with a computer 8 through a data line 10, a start-up program collects data, and after the electrochemical test is finished, the Oxygen Evolution (OER) performance polarization curve of the commercial ruthenium oxide catalyst can be obtained.
As shown in FIG. 4 (c), by applying the device of the present invention, the polarization curve of Oxygen Evolution (OER) performance of the commercial ruthenium oxide catalyst under the mass transfer flow rates of 0mL/min, 20mL/min, 40 mL/min, 60 mL/min, 80 mL/min, 100 mL/min and 120mL/min can be obtained, and the device has good regularity, which indicates that the device of the present invention can realize accurate regulation of the mass transfer flow rate of the electrode surface, and complete the performance test of the catalyst on Oxygen Evolution (OER) in 1mol/L KOH.
Claims (9)
1. An electrochemical testing device with controllable electrode surface mass transfer is characterized in that: the electrochemical testing device comprises an electrochemical testing system (5), a flow rate control system and a data acquisition system,
the electrochemical test system (5) comprises a multi-port electrolytic cell, wherein the multi-port electrolytic cell is provided with a liquid outlet (5-1), a liquid inlet (5-2), a nozzle hole (5-3), a gas inlet (5-4), a gas outlet (5-5), a working electrode fixing port (5-6), a counter electrode fixing port (5-7) and a reference electrode fixing port (5-8);
the flow rate control system comprises a valve (1), a flowmeter (2), an air duct (3), a micro circulating liquid supply pump (4) and an acid and alkali resistant silicone tube (6);
the data acquisition system comprises an electrochemical workstation (7), a computer (8), an electrode lead (9) and a data line (10); wherein, the valve (1) and the flowmeter (2) are connected with a multi-port electrolytic cell air inlet (5-4) through an air duct (3); the liquid inlet end of the micro circulating liquid supply pump (4) is connected with the liquid outlet (5-1) of the multi-port electrolytic cell through an acid and alkali resistant silicone tube (6), and the liquid outlet end is connected with the liquid inlet (5-2) of the multi-port electrolytic cell through the acid and alkali resistant silicone tube (6); the working electrode (5-9), the counter electrode (5-10) and the reference electrode (5-11) are fixed in the multi-port electrolytic cell through the working electrode fixing port (5-6), the counter electrode fixing port (5-7) and the reference electrode fixing port (5-8) and are connected with the electrochemical workstation (7) through an electrode lead (9); the working electrode (5-9) is opposite to the nozzle hole (5-3); the electrochemical workstation (7) is connected with the computer (8) through a data line (10).
2. The electrochemical testing device with controllable mass transfer on the surface of the electrode as claimed in claim 1, wherein: the valve (1) is used for controlling the closing or opening of the gas circuit, and the flow meter (2) is used for controlling the gas flow rate; the gas is oxygen, nitrogen or argon.
3. The electrochemical testing device with controllable mass transfer on the surface of the electrode as claimed in claim 1, wherein: the miniature circulating liquid supply pump (4) is of a constant-flow peristaltic pump, a miniature diaphragm pump or a miniature self-priming pump.
4. The measurement method implemented by the electrochemical testing device with the controllable electrode surface mass transfer according to any one of claims 1-3, is characterized by comprising the following steps:
electrolyte is filled in a multi-port electrolytic cell in an electrochemical testing system (5), a valve (1) and a flowmeter (2) are connected with an air inlet (5-4) of the multi-port electrolytic cell through an air duct (3), the valve (1) is opened, the flow rate of the gas introduced into the electrolyte is controlled by the flowmeter (2), meanwhile, the liquid inlet end of a miniature circulating liquid supply pump (4) is connected with the liquid outlet (5-1) of the multi-port electrolytic cell through an acid and alkali resistant silicone tube (6), the liquid outlet end of the miniature circulating liquid supply pump is connected with the liquid inlet (5-2) of the multi-port electrolytic cell through the acid and alkali resistant silicone tube (6), the power supply of the miniature circulating liquid supply pump is opened, the electrolyte is enabled to circularly flow in a device formed by the electrochemical testing system (5) and the flow rate control system, and the whole device is ensured to be in a working state;
(ii) inserting a working electrode (5-9) coated with a catalyst on the surface of the electrode core into the working electrode fixing port (5-6) to face the nozzle hole (5-3) and adjusting the distance between the nozzle hole and the nozzle hole, controlling the mass transfer flow rate of the electrolyte on the surface of the electrode core by a micro circulating liquid supply pump (4), and fixing the counter electrode (5-10) and the reference electrode (5-11) in the counter electrode fixing port (5-7) and the reference electrode fixing port (5-8);
(iii) the working electrode (5-9), the counter electrode (5-10) and the reference electrode (5-11) are connected with an electrochemical workstation (7) through an electrode lead (9), the electrochemical workstation (7) is connected with a computer (8) through a data line (10), a program is started to collect data, and after the electrochemical test is finished, a catalyst performance curve can be obtained.
5. The measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer according to claim 4, is characterized in that: the electrolyte is 0.1mol/L KOH and 0.1mol/L HCIO4、1mol/L H2SO4Or 1mol/L KOH.
6. The measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer according to claim 4, is characterized in that: the distance between the electrode core surface of the working electrode (5-9) and the nozzle hole (5-3) is 0.2-2 mm.
7. The measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer according to claim 4, is characterized in that: the diameter of an electrode core of the working electrode (5-9) is 3-5 mm.
8. The measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer according to claim 4, is characterized in that: the diameter of the nozzle hole (5-3) is 0.5-1 mm.
9. The measurement method implemented by the electrochemical testing device with controllable electrode surface mass transfer according to claim 4, is characterized in that: the controllable electrode surface mass transfer flow rate range of the micro circulating liquid supply pump (4) in the flow rate control system is 0-120 mL/min.
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| CN205665129U (en) * | 2016-04-12 | 2016-10-26 | 中国石油大学(华东) | High temperature high pressure contains erosion -corrosion simulation of solid particle fluid and electrochemistry testing experiment device |
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| CN205665129U (en) * | 2016-04-12 | 2016-10-26 | 中国石油大学(华东) | High temperature high pressure contains erosion -corrosion simulation of solid particle fluid and electrochemistry testing experiment device |
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