CN114280135A - Fuel cell metal catalyst atomic scale durability on-line detection system and method - Google Patents
Fuel cell metal catalyst atomic scale durability on-line detection system and method Download PDFInfo
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Abstract
The invention provides a fuel cell metal catalyst atomic scale durability on-line detection system and a method thereof, relating to the technical field of fuel cells, the on-line detection system comprises an electrochemical detection device and an inductively coupled plasma mass spectrometry detection device which are connected with each other, the electrochemical detection device comprises a solid-state rotating disk electrode and electrochemical detection equipment, wherein the solid-state rotating disk electrode comprises a fixed probe, a probe seat and a rotating disk electrode, one end of the fixed probe is arranged at the bottom of the rotating disc electrode, the other end of the fixed probe penetrates through the probe seat and then is connected with the inductively coupled plasma mass spectrometry detection device, one end of the rotating disc electrode is suitable for being in contact with a metal catalyst to be detected, and the other end of the rotating disc electrode penetrates through the probe seat and then is connected with the electrochemical detection equipment. The method has short detection period and can provide theoretical guidance for the use working condition of the catalyst and the design and selection of the catalyst.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a fuel cell metal catalyst atomic scale durability online detection system and method.
Background
The fuel cell is a power generation device which directly converts chemical energy of fuel into electric energy in an electrochemical reaction mode without combustion, is considered to be one of the power generation technologies with the greatest development prospects in the 21 st century, mainly comprises a proton exchange membrane fuel cell, a direct alcohol fuel cell and the like, and has the advantages of high energy density, quick start, high energy conversion efficiency and the like.
The proton exchange membrane fuel cell technology is an efficient and clean energy conversion device, is expected to solve the problems of world energy crisis and environmental pollution, and has wide application prospects in the fields of electric automobiles, portable power supplies, fixed power stations and the like. Noble metals Pt and its alloys are currently the most effective catalysts for proton exchange membrane fuel cells. However, Pt is a scarce resource and expensive, which leads to high cost of fuel cells and severely restricts the commercialization process of proton exchange membrane fuel.
The performance of the catalyst is gradually reduced in the application process of the fuel cell, and the durability detection of the fuel cell catalyst in the prior art needs to consume a long detection period which is about several weeks to several months, and sometimes even one year.
Disclosure of Invention
The invention solves the problem that the durability detection period of the fuel cell catalyst in the prior art is long.
In order to solve the above problems, the present invention provides an online detection system for atomic scale durability of a fuel cell metal catalyst, comprising an electrochemical detection device and an inductively coupled plasma mass spectrometry detection device, which are connected to each other, wherein the electrochemical detection device comprises a solid rotating disk electrode and an electrochemical detection device, the solid rotating disk electrode comprises a fixed probe, a probe seat and a rotating disk electrode, one end of the fixed probe is disposed at the bottom of the rotating disk electrode, the other end of the fixed probe penetrates through the probe seat and then is connected to the inductively coupled plasma mass spectrometry detection device, one end of the rotating disk electrode is suitable for contacting with a metal catalyst to be detected, and the other end of the rotating disk electrode penetrates through the probe seat and then is connected to the electrochemical detection device.
Preferably, the fixed probe comprises a probe head and an element collecting device which are connected with each other, the element collecting device is used for being connected with the inductively coupled plasma mass spectrometry detection apparatus, the probe head is provided with an opening for absorbing metal elements, and a gap is arranged between the probe head and the rotating disk electrode.
Preferably, the electrochemical detection device further comprises an auxiliary electrode and a reference electrode connected with the electrochemical detection equipment, wherein the auxiliary electrode is made of silver, platinum, graphite rod or nickel, and the reference electrode comprises a standard hydrogen electrode, a calomel electrode or a silver/silver chloride electrode.
Preferably, the rotating disc electrode is a glassy carbon electrode, and the diameter of the glassy carbon electrode ranges from 5 mm to 6 mm.
Preferably, the electrochemical detection device further comprises an electrolytic cell, and the rotating disk electrode, the auxiliary electrode and the reference electrode are adapted to be immersed in an electrolyte in the electrolytic cell.
Preferably, the electrolyte is selected from one of perchloric acid, dilute sulfuric acid and potassium hydroxide, and the concentration of the electrolyte is 0.1-0.5 mol/L.
Compared with the prior art, the fuel cell metal catalyst atomic scale durability on-line detection system has the advantages that:
according to the invention, the electrochemical detection device and the inductively coupled plasma mass spectrometry detection device are linked, so that the dissolution rate of the nano metal particles of the metal catalyst of the fuel cell can be rapidly detected, the performance attenuation principle of the metal catalyst can be assisted to be analyzed, and the development of the fuel cell catalyst with high durability is facilitated, therefore, theoretical guidance can be provided for the use working condition of the catalyst and the design and selection of the catalyst.
In order to solve the above problems, the present invention further provides an online detection method for durability of a fuel cell metal catalyst at atomic scale, and the online detection system for durability of a fuel cell metal catalyst at atomic scale is based on the method, and is characterized by comprising the following steps:
step S1, dissolving the nano-catalyst in a solvent to obtain catalyst slurry;
step S2, coating 5-20ul of the catalyst slurry on the surface of a rotating disc electrode, and drying at 60-90 ℃;
step S3, placing the dried rotating disc electrode, the auxiliary electrode and the reference electrode in an electrolytic cell, connecting with electrochemical detection equipment, and connecting the fixed probe with an inductively coupled plasma mass spectrometry detection device;
and step S4, starting the electrochemical detection equipment and the inductively coupled plasma mass spectrometry detection device, and measuring the dissolution rate of the nano catalyst in the atomic scale.
Preferably, in step S1, the solvent includes at least one of deionized water, isopropyl alcohol, ethanol, and perfluorosulfonic acid resin.
Preferably, the electrochemical analysis test method adopted by the electrochemical detection device comprises a cyclic voltammetry test method, a polarization curve test method, an accelerated test method, a constant voltage test method or a constant current test method.
Preferably, the rotating speed of the rotating disk electrode is 100-.
Compared with the prior art, the fuel cell metal catalyst atomic scale durability online detection method and the fuel cell metal catalyst atomic scale durability online detection system have the same advantages, and are not repeated herein.
Drawings
FIG. 1 is a schematic structural diagram of an on-line fuel cell metal catalyst durability detection system according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a solid state rotating disk electrode in an embodiment of the present invention;
FIG. 3 is a flow chart of a method for detecting durability of a fuel cell metal catalyst on an atomic scale in an embodiment of the invention;
FIG. 4 is a graph showing the dissolution rate of Pt measured by the cyclic voltammetry in an acid electrolyte according to an example of the present invention;
FIG. 5 is a graph showing the dissolution rate test of Pt in different nanosizes and atomic layers under acidic conditions in the examples of the present invention;
FIG. 6 is a graph showing the dissolution rate of Fe measured by a cyclic voltammetry method under an argon atmosphere for an Fe catalyst in an example of the present invention;
FIG. 7 is a graph showing the dissolution rate of Fe measured by a polarization curve test method under an oxygen atmosphere for an Fe catalyst in an embodiment of the present invention;
FIG. 8 is a graph showing the dissolution rate of Fe measured under high potential conditions for an Fe catalyst in an example of the present invention.
Description of reference numerals:
the method comprises the following steps of 1-rotating disc electrode, 2-fixed probe, 21-probe head, 22-element collecting equipment, 3-electrochemical detection equipment, 4-inductively coupled plasma mass spectrometry detection device, 5-probe seat, 6-metal catalyst, 7-auxiliary electrode and 8-reference electrode.
Detailed Description
The technical solutions in the embodiments of the present application will be described in detail and clearly with reference to the accompanying drawings.
In the description of the embodiments herein, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
As shown in fig. 1-2, an embodiment of the present invention provides an online detection system for atomic scale durability of a fuel cell metal catalyst, including an electrochemical detection device and an inductively coupled plasma mass spectrometry detection device 4 that are connected to each other, where the electrochemical detection device includes a solid-state rotating disk electrode and an electrochemical detection device 3, the solid-state rotating disk electrode includes a fixed probe 2, a probe holder 5, and a rotating disk electrode 1, one end of the fixed probe 2 is disposed at the bottom of the rotating disk electrode 1, the other end of the fixed probe 2 passes through the probe holder 5 and then is connected to the inductively coupled plasma mass spectrometry detection device 4, one end of the rotating disk electrode 1 is adapted to contact with a metal catalyst 6 to be detected, and the other end of the rotating disk electrode 1 passes through the probe holder 5 and then is connected to the electrochemical detection device 3.
Therefore, the electrochemical detection device and the inductively coupled plasma mass spectrometry detection device 4 are linked, so that the dissolution rate of the metal catalyst 6 nano metal particles of the fuel cell can be rapidly detected, the detection period is shortened, the performance attenuation principle of the metal catalyst 6 can be assisted to be analyzed, and the development of the fuel cell catalyst with high durability is facilitated, so that theoretical guidance can be provided for the use condition of the catalyst and the design and selection of the catalyst.
It should be noted that, in this embodiment, the shape of the probe seat 5 is not limited, and may be any geometric shape, and in some preferred embodiments, the shape of the probe seat 5 is cylindrical, so that the structure is simple, and the appearance is beautiful.
As shown in fig. 2, in some embodiments, the fixed probe 2 includes a probe head 21 and an element collecting device 22, which are connected to each other, the element collecting device 22 is used to connect with the inductively coupled plasma mass spectrometry apparatus 4, the probe head 21 is provided with an opening for absorbing metal elements, and a gap is provided between the probe head 21 and the rotating disk electrode 1, so as to avoid the influence on the electric field distribution during the electrochemical testing process due to the movement of the liquid level when the probe absorbs the metal elements.
In some preferred embodiments, the probe head 21 is vertically connected with the element collecting device 22, the structure is simple, and the element collecting device 22 passes through the probe base 5 to be connected with the inductively coupled plasma mass spectrometry apparatus 4, so that the connection between the probe head 21 and the element collecting device 22 and the inductively coupled plasma mass spectrometry apparatus 4 is convenient.
In this embodiment, the element collecting device 22 penetrates through the probe base 5 and is connected with the inductively coupled plasma mass spectrometry device 4 through a transmission pipeline, so that the connection is convenient, and the analysis of the dissolved nano metal particles by the inductively coupled plasma mass spectrometry device 4 is facilitated.
In some embodiments, the electrochemical detection apparatus further comprises an auxiliary electrode 7 and a reference electrode 8 connected to the electrochemical detection device 3, and the rotating disk electrode 1 in this embodiment is a working electrode, so that a three-electrode electrochemical test system is used in this embodiment, and two loops are formed, namely: a measurement loop: the electrochemical reaction tester consists of a rotating disc electrode 1 (working electrode) and a reference electrode 8, and is used for testing the electrochemical reaction process generated on the working electrode, and electrodeless current flows in the circuit and only extremely small measuring current flows; a polarization loop: the device consists of a rotating disc electrode 1 (working electrode) and a counter electrode, wherein polarization current exists in a polarization loop, can be measured and controlled, and plays a role in transmitting electrons to form a loop. Therefore, in the present embodiment, a three-electrode system is used, which not only allows polarized current to pass through the interface of the rotating disk electrode 1 (working electrode), but also does not interfere with the control and measurement of the potential of the rotating disk electrode 1 (working electrode), so that the control and measurement of current and potential can be simultaneously realized, and the measurement accuracy is high.
In some preferred embodiments, the material of the auxiliary electrode 7 is selected from silver, platinum, graphite rod or nickel, the reference electrode 8 comprises a standard hydrogen electrode, a calomel electrode or a silver/silver chloride electrode, and the suitable electrode material can be selected according to actual application to meet different test requirements.
In some embodiments, the rotating disk electrode 1 is a glassy carbon electrode, and the glassy carbon electrode has a diameter in the range of 5-6 mm. Good conductivity, high chemical stability, small coefficient of thermal expansion, hard texture and good air tightness.
In some embodiments, the electrochemical detection device further comprises an electrolytic cell, and the rotating disk electrode 1, the auxiliary electrode 7 and the reference electrode 8 are adapted to be immersed in an electrolyte in the electrolytic cell. Thereby facilitating electrochemical testing.
In some embodiments, the electrolyte is selected from one of perchloric acid, dilute sulfuric acid and potassium hydroxide, and the concentration of the electrolyte is 0.1 to 0.5 mol/L.
Therefore, the fuel cell metal catalyst atomic scale durability online detection system of the embodiment of the invention has the advantages over the prior art that: in the embodiment, the electrochemical detection device and the inductively coupled plasma mass spectrometry detection device 4 are linked, so that the dissolution rate of the metal catalyst 6 nano metal particles of the fuel cell can be rapidly detected, the performance attenuation principle of the metal catalyst 6 can be assisted to be analyzed, the development of the fuel cell catalyst with high durability is facilitated, and theoretical guidance can be provided for the use working condition of the catalyst and the design and selection of the catalyst.
As shown in fig. 3, another embodiment of the present invention further provides an online detection method for durability of a fuel cell metal catalyst at atomic scale, based on an online detection system for durability of a fuel cell metal catalyst at atomic scale, including the following steps:
step S1, dissolving the nano-catalyst in a solvent to obtain catalyst slurry;
step S2, coating 5-20ul of catalyst slurry on the surface of the rotating disc electrode 1, and drying at 60-90 ℃;
step S3, placing the dried rotating disc electrode 1, the auxiliary electrode 7 and the reference electrode 8 in an electrolytic cell, connecting with the electrochemical detection equipment 3, and connecting the fixed probe 2 with the inductively coupled plasma mass spectrometry detection device 4;
and step S4, starting the electrochemical detection device 3 and the inductively coupled plasma mass spectrometry detection device 4, and measuring the dissolution rate of the nano catalyst in the atomic scale.
It should be noted that, in this embodiment, the inductively coupled plasma mass spectrometry apparatus 4 has high detection accuracy, which can reach 1ppt level, that is, 1X10-6A molecular layer.
In some embodiments, in step S1, the solvent includes at least one of deionized water, isopropyl alcohol, ethanol, and perfluorosulfonic acid resin. Thereby, the nano catalyst can be dissolved better.
In some specific embodiments, when the perfluorosulfonic acid resin is mixed with other solvents, the mass ratio range is less than 10%, and the cost is saved.
In some preferred embodiments, in step S1, the nanocatalyst is dissolved in a solvent to obtain a catalyst slurry, which specifically includes: the nanocatalyst is ultrasonically dissolved in the solvent until a uniform ink-like slurry is formed. Under the ultrasonic condition, the nano catalyst can be better dissolved.
In some embodiments, the electrochemical detection apparatus 3 employs an electrochemical analytical test method including a cyclic voltammetry test method, a polarization curve test method, an accelerated test method, a constant voltage test method, or a constant current test method.
In some preferred embodiments, the rotating speed of the rotating disk electrode 1 is 100-. Thus, the measured data is more accurate.
In the cyclic voltammetry test method and the polarization curve test method, the scanning speed is 5-50mV/s, and the scanning voltage range is-2-2V; in the constant voltage test method, the constant voltage range is-2-2V, and the set time is 0-100 h; in the constant current test method, the setting range of the constant current is 0.1-10mA/cm2(ii) a The temperature range is 4-80 ℃, and can be regulated and controlled according to requirements.
It should be further noted that, in this embodiment, the accelerated test method is adopted to perform repeated tests under the same working condition, so that the dissolution condition of the metal nanoparticles in the catalyst under the same working condition can be detected in a short period, and the test period is shortened.
Compared with the prior art, the fuel cell metal catalyst 6 atomic scale durability online detection method and the fuel cell metal catalyst atomic scale durability online detection system have the same advantages, and are not repeated herein.
Example 1
The Pt-based nanomaterial used in fuel cells is a highly active electrocatalyst with catalytic oxygen reduction (ORR) capability. The higher cathode potential can cause the Pt-based catalyst to dissolve in the ORR process, and the durability of the Pt-based catalyst is reduced, so that the research on the dissolving process of the Pt-based catalyst has very important significance for improving the stability of the catalyst, further reducing the cost and prolonging the service life of equipment.
Therefore, the present embodiment provides an online detection method for the durability of the Pt catalyst in the atomic scale of the fuel cell, which is based on an online detection system for the durability of the Pt catalyst in the metal catalyst in the fuel cell, and includes the following steps:
step S1, dissolving the Pt-based nano-catalyst in a solvent to obtain Pt-based catalyst slurry;
step S2, coating 15ul Pt-based catalyst slurry on the surface of the rotating disc electrode 1, and drying at 80 ℃;
step S3, placing the dried rotating disc electrode 1, the auxiliary electrode 7 and the reference electrode 8 in an electrolytic cell, connecting with the electrochemical detection equipment 3, and connecting the fixed probe 2 with the inductively coupled plasma mass spectrometry detection device 4;
and step S4, starting the electrochemical detection device 3 and the inductively coupled plasma mass spectrometry detection device 4, and measuring the dissolution rate of the Pt-based nano catalyst in the atomic scale.
The dissolution rates of the Pt-based nanocatalysts measured in this example at the atomic scale are shown in fig. 4-5.
FIG. 4 is a graph showing the dissolution rate of Pt measured by the cyclic voltammetry method in the acid electrolyte in this example. Wherein, the upper curve is a cyclic voltammetry curve of the Pt catalyst, and the lower curve is the solubility of Pt in the reaction solution under different potentials corresponding to the cyclic voltammetry curve, so that it can be seen that, under the same potential, the higher the concentration is, the faster the Pt dissolution rate is, and vice versa.
Fig. 5 is a graph showing the dissolution rate test of Pt at different nano-sizes and atomic layers measured under acidic conditions in this example. Wherein NF represents nano particles, TF represents a film, and ML represents a molecular layer, so that it can be seen that the nano size and atomic layer thickness can significantly affect the dissolution rate of Pt, and the larger the nano size, the lower the dissolution rate; the greater the thickness of the film, the lower the dissolution rate.
Example 2
The embodiment provides an online detection method for durability of an Fe catalyst in atomic scale of a fuel cell, and an online detection system for durability of a metal catalyst in atomic scale of a fuel cell comprises the following steps:
step S1, dissolving the Fe-based nano catalyst in a solvent to obtain Fe-based catalyst slurry;
step S2, coating 20ul Fe-based catalyst slurry on the surface of the rotating disc electrode 1, and drying at 70 ℃;
step S3, placing the dried rotating disc electrode 1, the auxiliary electrode 7 and the reference electrode 8 in an electrolytic cell, connecting with the electrochemical detection equipment 3, and connecting the fixed probe 2 with the inductively coupled plasma mass spectrometry detection device 4;
and step S4, starting the electrochemical detection device 3 and the inductively coupled plasma mass spectrometry detection device 4, and measuring the dissolution rate of the Fe-based nano catalyst in the atomic scale.
The dissolution rates of the Fe-based nanocatalysts measured in this example at the atomic scale are shown in fig. 6-8.
Fig. 6 is a graph showing the dissolution rate of Fe measured by the cyclic voltammetry method under an argon atmosphere for the Fe catalyst in the example of the present invention. Wherein, the lower graph is a cyclic voltammetry curve, the upper graph corresponds to the concentration of the Fe catalyst in the solution under different potentials, and the dissolution rate of Fe is judged according to the concentration.
Fig. 7 is a graph showing the dissolution rate of Fe measured by a polarization curve test method under an oxygen atmosphere for the Fe catalyst in the example of the present invention. The lower graph is a polarization curve performance graph, the upper graph is corresponding to the concentration of the Fe catalyst in the solution under different potentials, and the dissolution rate of Fe is judged according to the concentration.
FIG. 8 is a graph showing the dissolution rate of Fe measured under high potential conditions for an Fe catalyst in an example of the present invention. In the present example, the highest potential of the test is 1.7V, and the dissolution rate of the Fe catalyst under the high potential condition can be monitored through the test.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. An on-line detection system for the durability of a fuel cell metal catalyst in atomic scale is characterized by comprising an electrochemical detection device and an inductively coupled plasma mass spectrometry detection device (4) which are connected with each other, the electrochemical detection device comprises a solid-state rotating disk electrode and an electrochemical detection device (3), the solid-state rotating disk electrode comprises a fixed probe (2), a probe seat (5) and a rotating disk electrode (1), one end of the fixed probe (2) is arranged at the bottom of the rotating disc electrode (1), the other end of the fixed probe (2) penetrates through the probe seat (5) and then is connected with the inductively coupled plasma mass spectrometry detection device (4), one end of the rotating disk electrode (1) is suitable for contacting with a metal catalyst (6) to be measured, the other end of the rotating disk electrode (1) penetrates through the probe seat (5) and then is connected with the electrochemical detection equipment (3).
2. The fuel cell metal catalyst atomic scale durability on-line detection system of claim 1, characterized in that the fixed probe (2) comprises a probe head (21) and an element collecting device (22) which are connected with each other, the element collecting device (22) is used for being connected with the inductively coupled plasma mass spectrometry detection apparatus (4), the probe head (21) is provided with an opening for absorbing metal elements, and a gap is arranged between the probe head (21) and the rotating disk electrode (1).
3. The fuel cell metal catalyst atomic scale durability on-line detection system of claim 1, characterized in that the electrochemical detection device further comprises an auxiliary electrode (7) and a reference electrode (8) connected with the electrochemical detection device (3), wherein the material of the auxiliary electrode (7) is selected from silver, platinum, graphite rod or nickel, and the reference electrode (8) comprises a standard hydrogen electrode, a calomel electrode or a silver/silver chloride electrode.
4. The fuel cell metal catalyst atomic scale durability on-line detection system of claim 1, characterized in that the rotating disk electrode (1) is a glassy carbon electrode and the glassy carbon electrode has a diameter in the range of 5-6 mm.
5. The fuel cell metal catalyst atomic scale durability on-line detection system of claim 3, characterized in that the electrochemical detection device further comprises an electrolytic cell, the rotating disk electrode (1), the auxiliary electrode (7) and the reference electrode (8) being adapted to be submerged in an electrolyte within the electrolytic cell.
6. The fuel cell metal catalyst atomic scale durability on-line detection system of claim 5, wherein the electrolyte is selected from one of perchloric acid, dilute sulfuric acid and potassium hydroxide, and the concentration of the electrolyte is 0.1-0.5 mol/L.
7. An on-line detection method for durability of a fuel cell metal catalyst on an atomic scale is based on the on-line detection system for durability of the fuel cell metal catalyst on an atomic scale as claimed in any one of claims 1 to 6, and is characterized by comprising the following steps:
step S1, dissolving the nano-catalyst in a solvent to obtain catalyst slurry;
step S2, coating 5-20ul of the catalyst slurry on the surface of the rotating disc electrode (1), and drying at 60-90 ℃;
step S3, placing the dried rotating disc electrode (1), the auxiliary electrode (7) and the reference electrode (8) in an electrolytic cell, connecting with electrochemical detection equipment (3), and connecting the fixed probe (2) with an inductively coupled plasma mass spectrometry detection device (4);
and step S4, starting the electrochemical detection device (3) and the inductively coupled plasma mass spectrometry detection device (4), and measuring the dissolution rate of the nano catalyst in the atomic scale.
8. The on-line detection method for atomic scale durability of a fuel cell metal catalyst according to claim 7, wherein in step S1, the solvent comprises at least one of deionized water, isopropanol, ethanol, and perfluorosulfonic acid resin.
9. The fuel cell metal catalyst atomic scale durability online detection method of claim 8, wherein the electrochemical detection device employs an electrochemical analysis test method comprising a cyclic voltammetry test method, a polarization curve test method, an accelerated test method, a constant voltage test method, or a constant current test method.
10. The method as claimed in claim 7, wherein the rotation speed of the rotating disk electrode is 100-1600 r/min.
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