CN115101754A - Preparation method of graphene aerogel based gas diffusion electrode of direct methanol fuel cell and membrane electrode - Google Patents
Preparation method of graphene aerogel based gas diffusion electrode of direct methanol fuel cell and membrane electrode Download PDFInfo
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- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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Abstract
The invention discloses a preparation method of a gas diffusion electrode of a direct methanol fuel cell based on graphene aerogel and a membrane electrode, and relates to the field of fuel cells. In the fuel cell electrode prepared by the invention, the microporous layer shows a porous structure, which is beneficial to the gas-liquid two-phase transmission of substances and increases the active exposed sites of the catalyst. The microporous layer containing Nafion and graphene aerogel is added between the electrode catalyst layer and the microporous layer containing PTFE, mass transfer is optimized due to the existence of the graphene aerogel layer, transmission resistance between the microporous layer and the catalyst layer is reduced, the utilization rate of the catalyst is improved, and the performance of the battery can be effectively improved. Under the operating condition of the methanol fuel cell, the electrode has better cell performance than the traditional electrode.
Description
Technical Field
The invention relates to the field of fuel cells, in particular to a direct methanol fuel cell, and relates to a preparation method of a gas diffusion electrode of the direct methanol fuel cell based on graphene aerogel and a membrane electrode.
Background
A Direct Alcohol Fuel Cell (DAFC) is a power generation device that directly converts chemical energy stored in alcohol fuel (such as methanol, ethanol, ethylene glycol, isopropanol, etc.) and oxygen into electric energy in a highly efficient and green manner. The alcohol solution on the anode side is subjected to oxidation reaction under the catalytic action of the anode catalyst to release electrons, the oxygen on the cathode side is combined with the electrons transmitted from an external circuit under the catalytic action of the cathode catalyst to perform reduction reaction, and meanwhile, ions balance the ionic charges between the anode and the cathode through the polyelectrolyte membrane to realize an internal loop of the battery. Among various alcohol fuels, methanol is considered to be the most promising fuel, which has the simplest molecular structure, no carbon bond, is more easily oxidized than other alcohol fuels, and has an energy density of 6100Whkg -1 . Therefore, in the past decades, DMFCs have been extensively studied.
The MEA is mainly composed of a Gas Diffusion Layer (GDL), a Catalyst Layer (CL), and a Proton Exchange Membrane (PEM). In the electrochemical reaction process, all functional layers of the MEA need to participate and cooperate together, the performance of the PEMFC is restricted by the mass transfer, catalysis, conduction and other capabilities of the functional layers, and the structural optimization of all the functional layers plays a significant role in improving the performance of the PEMFC.
The gas diffusion layer plays a role in transporting reactants and products, conducting electricity, conducting heat, and supporting a catalytic layer, and is an important component of the electrode. The diffusion layer generally consists of two parts, a support layer and a Microporous layer (MPL). The diffusion layer should have high electrical conductivity, high porosity, high thermal conductivity and a suitable balance of hydrophobic and hydrophilic properties. At the present stage, the main research direction of the diffusion layer is to adjust the structure and material components of the diffusion layer, improve the utilization rate of the supported catalyst, and improve the mass transfer capacity under high current density. The traditional microporous layer is formed by single-layer carbon powder, and after a catalyst is loaded, a plurality of active sites are hidden under the surface and cannot play a catalytic role. Moreover, during the long-term operation of the battery, the catalyst may agglomerate or deposit in the microporous layer, greatly reducing the utilization rate of the catalyst and seriously affecting the performance and durability of the battery.
Disclosure of Invention
Aiming at overcoming the defects in the prior art, the invention provides a preparation method of a graphene aerogel electrode and a membrane electrode, aiming at overcoming the defects of the traditional gas diffusion electrode. According to the preparation method, the graphene aerogel electrode with the double microporous layers is prepared, the loss of the catalyst deposited in the microporous layers in the operation process of the battery is greatly reduced by using the design of the double microporous layers, the utilization rate of the catalyst is improved, and the performance of the battery is further improved compared with that of a traditional single microporous layer electrode. And through the application of the graphene aerogel, the electrochemical surface area is increased, the stability of the catalyst is improved, and the performance of the fuel cell is effectively improved.
The present invention achieves the above-described object by the following technical means.
A preparation method of a graphene aerogel based direct methanol fuel cell gas diffusion electrode comprises the following steps:
step one), firstly, preparing a hydrophobic layer on an electrode substrate layer, then spraying an outer microporous layer containing carbon powder and PTFE on the hydrophobic layer, drying and sintering, and then spraying an inner microporous layer containing graphene aerogel and Nafion on the outer microporous layer to form a gas diffusion layer with a double-microporous-layer structure;
and step two) spraying a catalyst solution on the surface of the electrode prepared in the step one), and drying to obtain the graphene aerogel gas diffusion electrode.
In the scheme, the double-micropore layer in the step one) is of a double-layer structure formed by combining a hydrophobic layer and a graphene aerogel hydrophilic layer in an array mode.
In the above scheme, the electrode substrate layer in the step one) is one of carbon fiber paper, carbon fiber woven cloth, carbon black paper and carbon felt.
In the scheme, the electrode substrate layer in the step one) needs to be boiled for 10min by acetone, and organic matters on the surface are removed.
In the scheme, the hydrophobic layer in the step one) is a mixture of carbon powder and a hydrophobic agent, and the hydrophobic agent is one of polytetrafluoroethylene and polyvinylidene fluoride.
In the scheme, the hydrophilic layer in the step one) is a mixture of graphene aerogel and a hydrophilic agent, and the hydrophilic agent is one of perfluorosulfonic acid, partially fluorinated sulfonic acid and phosphoric acid.
In the scheme, the mass ratio of the graphene aerogel to the carbon powder in the step one) is 1:3 or 1: 1.
In the scheme, the catalyst solution used in the second step) is 20g of ptru/C powder, which is diluted with 2mL of deionized water, the obtained solution contains 8g of Pt, then 5 wt.% of Nafion solution 428.5mg is added, and finally, a dispersing agent is added to obtain the catalyst solution.
In the scheme, in the step two), the dispersing agent is one of isopropanol and acetone.
A graphene aerogel gas diffusion electrode prepared by a preparation method of a direct methanol fuel cell gas diffusion electrode based on graphene aerogel is used as an anode, a Pt/C electrode is used as a cathode, the middle of the electrode is separated by a proton exchange membrane, and hot pressing is carried out, so that the membrane electrode based on the graphene aerogel double microporous layer is obtained.
Has the beneficial effects that:
by utilizing the design of the double microporous layers, the loss of the catalyst which falls off and is deposited in the microporous layers in the battery operation process is greatly reduced, the utilization rate of the catalyst is improved, and the battery performance is improved compared with the traditional single microporous layer electrode. In addition, through the application of the graphene aerogel, the electrochemical reaction active surface area is increased, the stability of the catalyst is improved, the output power of the fuel cell is effectively improved, and the service life of the fuel cell is effectively prolonged.
In the fuel cell electrode prepared by the invention, the microporous layer shows a porous structure, which is beneficial to the gas-liquid two-phase transmission of substances and increases the active exposed sites of the catalyst. The microporous layer containing perfluorosulfonic acid (Nafion) and graphene aerogel is added between the electrode catalyst layer and the microporous layer containing Polytetrafluoroethylene (PTFE), so that mass transfer is optimized due to the existence of the graphene aerogel layer, the transmission resistance between the microporous layer and the catalyst layer is reduced, the utilization rate of the catalyst is improved, and the performance of the battery can be effectively improved. Under the operating condition of the methanol fuel cell, the electrode has better cell performance than the traditional electrode.
Drawings
Fig. 1 is a flow chart of the preparation of a graphene aerogel doped double microporous layer fuel cell electrode according to the present invention;
fig. 2 is a polarization curve diagram of the novel graphene aerogel electrode according to the present invention.
Reference numerals:
1-carbon paper, 2-outer microporous layer, 3-inner microporous layer and 4-catalytic layer.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
A preparation method of a graphene aerogel based direct methanol fuel cell gas diffusion electrode comprises the following steps:
(1) treatment of the electrode base layer: cutting carbon paper or carbon cloth as electrode substrate layer into proper size, heating and washing in acetone at 30-70 deg.C for 15-30min to remove surface dirt and functional groups, ultrasonic washing in deionized water for 15-60min to remove acetone on the surface;
(2) preparing a hydrophobic electrode substrate layer: soaking the carbon paper or carbon cloth treated in the step (1) in a Polytetrafluoroethylene (PTFE) dispersion solution for hydrophobic treatment, taking out after a period of time, drying at 70 ℃ for 2h, and then placing in a 370 ℃ muffle furnace for sintering for 30min to enable the PTFE content to reach 15-20 wt%;
(3) preparing a novel gas diffusion electrode: uniformly dispersing a certain amount of carbon powder and a hydrophobic agent into isopropanol, performing ultrasonic treatment to form uniformly dispersed slurry, uniformly spraying the slurry on the surface of the hydrophobic layer prepared in the step (2), and sintering in a muffle furnace at 370 ℃ for 30min to form an outer microporous layer. Uniformly dispersing a certain amount of graphene aerogel and a hydrophilic agent in isopropanol, performing ultrasonic treatment to form uniformly dispersed slurry, and uniformly spraying the slurry on the outer microporous layer in the step one to obtain the double microporous layer. Weighing a proper amount of catalyst and hydrophilic agent, dispersing the catalyst and the hydrophilic agent in isopropanol dispersion liquid, uniformly spraying the catalyst and the hydrophilic agent on the microporous layer uniformly by ultrasonic, and drying the microporous layer at 70 ℃ for 2 hours to obtain a microporous layer Gas Diffusion Electrode (GDE);
(4) preparing a membrane electrode: and (3) taking the GDE in the step (3) as an anode, taking a conventional Pt/C electrode as a cathode, separating the GDE and the conventional Pt/C electrode by using a proton exchange membrane, and carrying out hot pressing to obtain the membrane electrode based on the graphene aerogel double microporous layer.
Example 1
And (3) doping the graphene aerogel into the methanol fuel cell electrode, and performing a discharge test. The method mainly comprises the following steps:
(1) treatment of the electrode base layer: cutting carbon paper or carbon cloth as an electrode substrate layer into proper sizes, washing in heated acetone for 15min to remove surface dirt and functional groups, and ultrasonically washing in deionized water for 15min to remove acetone on the surface;
(2) preparing a hydrophobic electrode substrate layer: soaking the carbon paper or carbon cloth treated in the step (1) in a Polytetrafluoroethylene (PTFE) dispersion solution for hydrophobic treatment, taking out after a period of time, drying at 70 ℃ for 2h, and then placing in a 370 ℃ muffle furnace for sintering for 30min to enable the PTFE content to reach 15-20 wt%;
(3) preparing a novel gas diffusion electrode: uniformly dispersing a certain amount of carbon powder and a hydrophobing agent into isopropanol, performing ultrasonic treatment to form uniformly dispersed slurry, uniformly spraying the slurry on the surface of the hydrophobic layer prepared in the step (2), and then putting the hydrophobic layer into a muffle furnace at 370 ℃ for sintering for 30min to form an outer microporous layer, wherein the loading capacity is 1.5mg cm -2 . Secondly, uniformly dispersing a certain amount of graphene aerogel and a hydrophilic agent in isopropanol, performing ultrasonic treatment to form uniformly dispersed slurry, and uniformly spraying the slurry on the outer surface of the first stepOn the microporous layer, a double microporous layer with aerogel loading of 0.5mg cm was obtained -2 . Thirdly, a certain amount of PtRu/C catalyst and hydrophilic agent are weighed and dispersed in isopropanol dispersion liquid, evenly sprayed on the double-micropore layer in the second step by ultrasonic, and the PtRu loading is 2mg cm -2 Drying at 70 ℃ for 2h to obtain a Gas Diffusion Electrode (GDE) with a double microporous layer;
(4) preparing a membrane electrode and assembling a battery: the conventional electrode prepared in step (2) of comparative example 1 (platinum loading of 2mg cm) -2 ) As a cathode, the graphene aerogel electrode prepared in the step (3) is used as an anode, the middle part of the graphene aerogel electrode is separated by a Nafion 117 membrane treated by hydrogen peroxide and sulfuric acid, and the membrane electrode is obtained by hot pressing for 5min by a hot press;
(5) and (3) testing the discharge performance: after the membrane electrode was assembled in a single cell system, a discharge test was performed. The test conditions were: the working temperature of the battery is 60 ℃, the pressure is normal, methanol is introduced into the anode, and oxygen is introduced into the cathode. Under the working voltage of 0.25V, the current density can reach 99.85mA cm -2 The maximum power density reaches 19.98mW cm -2 。
Example 2
And doping the graphene aerogel with the methanol fuel cell electrode, and performing a discharge test. The method mainly comprises the following steps:
(1) treatment of the electrode base layer: cutting carbon paper or carbon cloth as an electrode substrate layer into proper sizes, washing in heated acetone for 15min to remove surface dirt and functional groups, and ultrasonically washing in deionized water for 15min to remove acetone on the surface;
(2) preparing a hydrophobic electrode substrate layer: soaking the carbon paper or carbon cloth treated in the step (1) in a Polytetrafluoroethylene (PTFE) dispersion solution for hydrophobic treatment, taking out after a period of time, drying at 70 ℃ for 2h, and then placing in a 370 ℃ muffle furnace for sintering for 30min to enable the PTFE content to reach 15-20 wt%;
(3) preparing a novel gas diffusion electrode: uniformly dispersing a certain amount of carbon powder and a water repellent agent into isopropanol, performing ultrasonic treatment to form uniformly dispersed slurry, uniformly spraying the slurry on the surface of the hydrophobic layer prepared in the step (2), placing the hydrophobic layer in a muffle furnace at 370 ℃ for sintering for 30min to form an outer microporous layer, and loading the microporous layer with a certain amount of powderIs 1mg cm -2 . Uniformly dispersing a certain amount of graphene aerogel and a hydrophilic agent in isopropanol, performing ultrasonic treatment to form uniformly dispersed slurry, uniformly spraying the slurry on the outer microporous layer in the step I to obtain a double microporous layer, wherein the aerogel loading amount is 1mg cm -2 . Thirdly, weighing a certain amount of PtRu/C catalyst and hydrophilic agent, dispersing the PtRu/C catalyst and the hydrophilic agent in isopropanol dispersion liquid, evenly spraying the PtRu/C catalyst and the hydrophilic agent on the double-microporous layer in the second step, wherein the PtRu loading is 2mg cm -2 Drying at 70 ℃ for 2h to obtain a Gas Diffusion Electrode (GDE) with a double microporous layer;
(4) preparing a membrane electrode and assembling a battery: the conventional electrode (platinum loading of 2mg cm) prepared in step (2) of comparative example 1 was used -2 ) As a cathode, the graphene aerogel electrode prepared in the step (3) is used as an anode, the middle part of the graphene aerogel electrode is separated by a Nafion 117 membrane treated by hydrogen peroxide and sulfuric acid, and the membrane electrode is obtained by hot pressing for 5min by a hot press;
(5) and (3) testing the discharge performance: after the membrane electrode was assembled in a single cell system, a discharge test was performed. The test conditions were: the working temperature of the battery is 60 ℃, the temperature is normal pressure, methanol is introduced into the anode, and oxygen is introduced into the cathode. Under the working voltage of 0.25V, the current density can reach 99.79mA cm -2 Maximum power density of 21.42mW cm -2 。
Comparative example 1
A direct methanol fuel cell of a conventional diffusion structure was prepared and subjected to a discharge test. The anode and cathode of the fuel cell both use conventional electrodes, and the main steps are as follows:
(1) and (3) treating the carbon paper: carbon paper (Dongli-060) was used for the gas diffusion layer. Firstly, decontaminating treatment is carried out, the carbon paper is soaked in acetone, heated and boiled for 15-20min, impurities on the surface and in holes of the carbon paper are removed, and the carbon paper is dried at 70 ℃. Then soaking the PTFE powder in a dispersion liquid of Polytetrafluoroethylene (PTFE) for hydrophobic treatment, taking out after a period of time, drying for 2h at 70 ℃, and then putting the PTFE powder in a muffle furnace at 370 ℃ for sintering for 30min to enable the content of the PTFE to reach 15-20 wt%;
(2) preparation of conventional electrode: dispersing carbon powder (Vulcan XC-72R) and PTFE in isopropanol dispersion liquid, ultrasonically and uniformly spraying on carbon paper containing a hydrophobic layer, and drying at 70 deg.C2h, then placing the mixture into a muffle furnace at 370 ℃ for sintering for 30min, taking out the mixture, cooling, weighing and calculating to obtain the carbon powder loading capacity of 2mg cm -2 PTFE, C is 85% and 15% hydrophobic layer. Secondly, weighing a proper amount of 40 wt.% Pt/C (60 wt.% PtRu/C) and Nafion, dispersing the Pt/C and the Nafion into isopropanol dispersion liquid, uniformly spraying the mixture on the hydrophobic layer in the first step by ultrasonic, drying the mixture for 2 hours at 70 ℃, taking out the mixture, cooling and weighing to calculate to obtain the Pt (PtRu) catalyst with the loading capacity of 2mg cm -2 The conventional electrode of (1);
(3) preparation of conventional membrane electrode and assembly of cell: taking two conventional electrodes prepared in the step (2), wherein Pt/C is a cathode, PtRu/C is an anode, the middle of each conventional electrode is separated by a Nafion 117 membrane treated by hydrogen peroxide and sulfuric acid, and hot pressing for 5min by using a hot press to obtain a conventional membrane electrode;
(4) and (3) testing the discharge performance: after the membrane electrode was assembled in a single cell system, a discharge test was performed. The test conditions were: the working temperature of the battery is 60 ℃, the temperature is normal pressure, methanol is introduced into the anode, and oxygen is introduced into the cathode. Under the working voltage of 0.25V, the current density can reach 99.86mA cm -2 The maximum power density reaches 18.41mW cm -2 。
Compared with the comparative example 1, under the working voltage of 0.25V, the examples 1 and 2 have larger power density, which can be attributed to the design of utilizing the double microporous layer, so that the loss of the catalyst deposited in the microporous layer in the battery running process is greatly reduced, the utilization rate of the catalyst is improved, the electrochemical surface area is increased, the stability of the catalyst is improved, and the performance of the fuel cell is effectively improved through the application of the graphene aerogel. Has great significance for the development of fuel cell electrodes.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like 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. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment 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.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that those skilled in the art may make variations, modifications, substitutions and alterations within the scope of the present invention without departing from the spirit and scope of the present invention.
Claims (10)
1. A preparation method of a graphene aerogel based direct methanol fuel cell gas diffusion electrode is characterized by comprising the following steps:
step one), firstly preparing a hydrophobic layer on an electrode substrate layer, then spraying an outer microporous layer containing carbon powder and PTFE on the hydrophobic layer, drying and sintering at the temperature of 300-400 ℃ for 30-60 min, and then using a spray gun to prepare 2-4 mg ml -1 The inner microporous layer solution is sprayed on the outer microporous layer to form the gas diffusion layer with a double microporous layer structure;
step two) using a spray gun to spray 2-4 mgml on the surface of the electrode of the gas diffusion layer with the double-microporous-layer structure prepared in the step one) -1 The catalyst solution is sprayed until the catalyst loading reaches 2mgcm -2 And drying at 60-80 ℃ to obtain the graphene aerogel gas diffusion electrode.
2. The method for preparing a graphene aerogel based direct methanol fuel cell gas diffusion electrode according to claim 1, wherein the microporous layer structure in the step one) is a two-layer structure combining a hydrophobic layer and a graphene aerogel hydrophilic layer array.
3. The preparation method of the graphene aerogel based direct methanol fuel cell gas diffusion electrode according to claim 1, wherein the electrode substrate layer in the step one) is one of carbon fiber paper, carbon fiber woven cloth, carbon black paper or carbon felt.
4. The preparation method of the graphene aerogel based direct methanol fuel cell gas diffusion electrode according to claim 1, wherein in the step one), the electrode substrate layer is heated and washed by acetone for 15-30min, the heating temperature is kept at 30-70 ℃, the dirt and functional groups on the surface are removed, and then the electrode substrate layer is ultrasonically washed in deionized water for 15-60min, so that the acetone on the surface is removed.
5. The preparation method of the gas diffusion electrode of the direct methanol fuel cell based on the graphene aerogel according to claim 1, wherein in the first step, the hydrophobic layer is a mixture of carbon powder and a hydrophobic agent, and the hydrophobic agent is one of polytetrafluoroethylene and polyvinylidene fluoride; the inner microporous layer solution is a mixed dispersion of graphene aerogel and Nafion.
6. The method for preparing the gas diffusion electrode of the direct methanol fuel cell based on the graphene aerogel according to claim 1, wherein the hydrophilic layer in the step one) is a mixture of the graphene aerogel and a hydrophilic agent, and the hydrophilic agent is one of perfluorinated sulfonic acid, partially fluorinated sulfonic acid and phosphoric acid.
7. The method for preparing the gas diffusion electrode of the direct methanol fuel cell based on the graphene aerogel according to claim 1, wherein the mass ratio of the graphene aerogel to the carbon powder in the step one) is 1:3 or 1: 1.
8. The method for preparing a gas diffusion electrode for a direct methanol fuel cell based on graphene aerogel according to claim 1, wherein the catalyst solution used in step two) is 20g of ptru/C powder diluted with 2mL of deionized water, and the obtained solution contains 8g of Pt, and then 5 wt.% of Nafion solution 428.5mg is added, and finally a dispersant is added, so as to obtain the catalyst solution.
9. The method for preparing the gas diffusion electrode for the direct methanol fuel cell based on the graphene aerogel according to claim 1, wherein in the second step), the dispersant is one of isopropanol and acetone.
10. A membrane electrode based on a graphene aerogel double microporous layer, characterized in that the graphene aerogel gas diffusion electrode prepared by the method for preparing a graphene aerogel based direct methanol fuel cell gas diffusion electrode according to any one of claims 1 to 9 is used as an anode, a Pt/C electrode is used as a cathode, and the electrodes are separated by a proton exchange membrane and hot-pressed, so as to obtain the membrane electrode based on the graphene aerogel double microporous layer.
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