CN110165228B - Self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure and preparation method thereof - Google Patents
Self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure and preparation method thereof Download PDFInfo
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- CN110165228B CN110165228B CN201910435294.3A CN201910435294A CN110165228B CN 110165228 B CN110165228 B CN 110165228B CN 201910435294 A CN201910435294 A CN 201910435294A CN 110165228 B CN110165228 B CN 110165228B
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Abstract
The invention relates to the technical field of fuel cells, and provides a self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure and a preparation method thereof, wherein an array structure is grown on the surface of carbon fiber by a hydrothermal method; then carrying out carbon coating by a hydrothermal method to obtain a carbon-coated array structure; the catalyst loading was carried out on a carbon-coated array support at room temperature. Compared with the traditional proton exchange membrane fuel cell cathode, the surface of the integrated electrode prepared by the method has good hydrophobicity, the ordered carrier is more beneficial to the transmission of reactants and products, the hydrophobicity effectively avoids the flooding phenomenon, and the operation efficiency and stability of the cell are improved.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a preparation method of a self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure.
Background
The non-renewable fossil energy and the enhancement of people's awareness of environmental protection, clean energy naturally becomes the mainstream of world attention. The fuel cell, whether reactant or product, is fully compliant with clean energy standards. Proton exchange membrane fuel cells are attracting attention as the most ideal vehicle energy supply device. However, platinum, which is the most catalytic catalyst and is difficult to replace, is a high cost fuel cell, and in addition, the cathode has a higher overpotential compared to the anodic oxidation process, which reduces the actual output voltage of the fuel cell. Therefore, many researches are established on the basis of modification of the platinum-based catalyst, and the catalytic performance is improved by constructing Pt with different morphologies and introducing non-noble metals. In the preparation process of the fuel cell cathode, the diffusion layer is usually composed of carbon paper and a carbon powder layer on the carbon paper, and the carbon powder layer is mainly used as a carrier of the catalyst, but in the actual operation of the fuel cell, the degradation of the cell performance is actually caused by corrosion of the carbon powder layer in the diffusion layer under long-time high-potential operation, so that the catalyst on the surface is aggregated and dropped off, and most of the catalytic activity is finally lost. The stable catalyst support may be a key factor in achieving stable operation of the fuel cell for a long time.
The commonly used stable carrier materials mainly include metal oxides, carbides, high molecular polymers and the like. Meanwhile, in consideration of proton, electron and material transmission in the fuel cell, the combination of a simple carrier and a catalyst cannot provide a smooth transmission channel. Therefore, the construction of ordered material conveying channels can realize the rapid conveying of each material and provide more three-phase reaction areas. At present, the most representative is an organic whisker array structure prepared by American 3M, which replaces the traditional carbon powder layer carrier, and a Pt film is prepared on the organic whisker array structure, so that the movement of Pt on the surface of the Pt film is effectively prevented, and a cathode with higher stability is obtained.
In the fuel cell, because the product of the cathode reaction is water, the water cannot be removed in time, which causes a flooding phenomenon, and seriously affects the performance of the fuel cell. Hydrophobicity is another indicator of the cathode. The most common hydrophobic treatment is the addition of a dispersion of PTFE, but the loss of catalyst is due to the PTFE being non-conductive and covering the surface of the catalyst.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a preparation method of a self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure, solves the problems of unstable long-time operation and water flooding of a proton exchange membrane fuel cell, and simultaneously realizes hydrophobicity, order and construction of a high-stability fuel cell cathode.
The invention adopts the following technical scheme:
a preparation method of a self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure comprises the following steps:
s1, dissolving the target array precursor and the coordination agent in an organic solution, and fully stirring to prepare a solution A;
s2, placing the two diffusion layers in the inner liner of the reaction kettle, transferring the solution A into the inner liner, and reacting at a certain temperature to enable the array structure to grow on the surface of the diffusion layers;
s3, after the reaction in the step S2 is finished, cooling the diffusion layer to room temperature, washing and drying; sintering at a certain temperature to obtain an array structure B;
s4, placing the array structure B in a reaction kettle lining, adding a carbon source with a certain concentration, and carrying out carbon coating at a certain temperature;
s5, after the reaction in the step S4 is finished, cooling the array structure B to room temperature, washing and drying, and sintering at a certain temperature atmosphere to obtain a carbon-coated array structure C;
s6, placing the carbon-coated array structure C in a reaction container, and loading platinum on the carbon-coated array structure C by reducing a Pt-based precursor to obtain the self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure D with a certain loading capacity, wherein the surface of the platinum catalyst layer presents hydrophobic characteristics.
Further, in step S1, the target array precursor includes chloride and nitrate; the complexing agent comprises glucose and thioacetamide.
Further, in step S2, the carbon paper serves as a diffusion layer.
Further, in step S2, the array structure is a metal oxide, a nitride, or a polymer organic.
Further, in step S2, the reaction temperature is 160-200 ℃, and the reaction time is 12-36 hours.
Further, in step S3, the sintering temperature is 350-; the sintering time is 1-3 hours.
Further, in step S4, the carbon source includes sucrose, glucose, and vitamin C; the concentration of the carbon source solution is 0.02-0.1mol/L, and 20-40ml of the carbon source solution is taken; when the carbon is coated, the hydrothermal reaction temperature is 160-190 ℃, and the reaction time is 3-24 hours.
Further, in step S5, the sintering conditions are: sintering for 1-5 hours at 500-900 ℃ under the atmosphere of argon, and the heating rate is 1-5 ℃/min.
Further, in step S6, the reducing agent includes ethylene glycol, formic acid, and sodium borohydride; the Pt-based precursor is chloroplatinic acid or acetylacetone platinum; the reaction time is 1 minute to 72 hours, and the platinum loading capacity is 0.05 mg/cm to 0.25mg/cm2。
A self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure is prepared by the preparation method.
The self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure is applied to proton exchange membrane fuel cells.
The invention has the beneficial effects that:
1. the catalyst carrier prepared by the invention is of an ordered array structure, and provides a good material transmission channel;
2. compared with the traditional carbon carrier, the carrier structure has better stability, and is beneficial to the long-time stable operation of the battery;
3. the surface of the platinum catalyst prepared by the method has a hydrophobic characteristic, so that the method is beneficial to water removal, effectively reduces the possibility of flooding and improves the utilization rate of the catalyst.
Drawings
Fig. 1 shows comparative test patterns of contact angles of the self-hydrophobic integrated ordered catalytic layer-diffusion layer electrode structure prepared in example 1 and a commercial catalyst layer, wherein (a) is the commercial catalyst layer, and (b) is the self-hydrophobic integrated ordered catalytic layer-diffusion layer electrode structure prepared in example 1.
FIG. 2 is an electron microscope image of the self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure prepared by the embodiment of the invention; (b) an enlarged view of (a).
Fig. 3 shows a cyclic voltammetry test chart and an active area decay curve (c) for a commercial catalyst (a) and a self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure (b) prepared by the embodiment of the invention.
Fig. 4 shows electron micrographs of commercial catalysts (a) - (c) and self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structures (d) - (f) prepared by the embodiment of the invention after 3000 cycles of accelerated cycle testing. Wherein (a) and (d) are electron micrographs before and after the cycle.
FIG. 5 is a contact angle test chart of electrode structures of the integrated ordered catalytic layer-diffusion layer with different platinum loading amounts, prepared in the embodiment of the invention; wherein (a) is a commercial catalyst and the platinum loadings of (b) - (f) are 0.05, 0.1, 0.15, 0.20, 0.25mg.cm, respectively2。
Fig. 6 is a cyclic voltammetry test chart (a) and an electrochemical active area (b) of the integrated ordered catalytic layer-diffusion layer electrode structures with different platinum loadings prepared in the examples of the present invention.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered as being isolated, and they may be combined with each other to achieve better technical effects.
Example 1
Dissolving a certain amount of stannic chloride and thioacetamide in isopropanol solution, immersing the diffusion layer in a reaction kettle containing the solution, and reacting at 180 ℃ for 24 hours. Cooling to room temperature, drying, calcining at 500 deg.C in air for 2 hr to form SnO2the/CP structure. Preparing glucose solution, and adding prepared SnO2Placing the/CP at the bottom of the reaction kettle, injecting glucose solution, placing the reaction kettle in an oven for 24 hours at 180 ℃, cooling to room temperature, drying, calcining for 2 hours at 500 ℃ under the atmosphere of argon to obtain SnO2@ C/CP. Prepared SnO2The @ C/CP is placed in a self-made container, and deionized water, formic acid and chloroplatinic acid are added. Standing at room temperature for 72 hours, repeatedly washing with deionized water, and drying for later use. Is marked as Pt-SnO2@ C/CP. The contact angle test result is shown in fig. 1, the contact angle can reach 134 degrees after the Pt is loaded, the contact angle of the commercial Pt/C catalytic layer is 127.3 degrees, and the integrated electrode structure has more excellent hydrophobic capability. By passingThe cyclic voltammetry tests characterize the electrochemically active area of the sample and evaluate the stability of the sample through 3000 cycles of accelerated cycling tests. From the electrochemically active area, Pt-SnO2The active area of @ C/CP is essentially the same as that of 40% commercial Pt/C, due to Pt-SnO2The special morphology of Pt in @ C/CP makes the active area of Pt slightly high, and under the condition of the same platinum loading capacity, the Pt-SnO is explained2The @ C/CP Pt has more active sites, and the utilization rate of Pt is improved. And the active area is attenuated to different degrees through a cyclic voltammetry test of 3000 circles. The commercial Pt/C active area is only the initial 17%, while Pt-SnO2The active area of @ C/CP may be maintained at 60% of the initial area. This indicates that the latter has less loss of active area, the cause of which can be analyzed from the electron micrographs after cycling. As shown in fig. 4, after the Pt/C is operated for a long time, Pt is obviously aggregated, part of carbon powder has no Pt load, and the loss of the active area is because a large amount of Pt is aggregated due to the instability of the carbon powder layer, so that the active surface area is reduced. And for Pt-SnO2The structure of @ C/CP can be seen from the figure, the morphology does not obviously change before and after long-time test, and SnO2The @ C array support has better stability, and the fluffy Pt catalyst is uniformly covered on the surface of the support without further aggregation. The reduction in active area may be due to the partial carrier becoming sparse. Analysis by the above experiment, Pt-SnO2@ C/CP has superior catalytic activity and stability to commercial Pt/C.
Example 2
Dissolving a certain amount of stannic chloride and thioacetamide in isopropanol solution, immersing the diffusion layer in a reaction kettle containing the solution, and reacting at 180 ℃ for 24 hours. Cooling to room temperature, drying, calcining at 500 deg.C in air for 2 hr to form SnO2the/CP structure. Preparing glucose solution, and adding prepared SnO2Placing the/CP at the bottom of the reaction kettle, injecting glucose solution, placing the reaction kettle in an oven for 24 hours at 180 ℃, cooling to room temperature, drying, calcining for 2 hours at 500 ℃ under the atmosphere of argon to obtain SnO2@ C/CP. Placing the prepared SnO2@ C/CP into a self-made container, and changing the amount of Pt load0.05, 0.10, 0.15, 0.20, 0.25mg cm respectively-2. Standing at room temperature for 72 hours, repeatedly washing with deionized water, and drying for later use. The contact angle test was performed, and as shown in fig. 5, the contact angle and the electrochemically active area showed a tendency of increasing and then decreasing with increasing Pt content, wherein the Pt loading was 0.15 mg-cm-2The contact angle is the largest. Meanwhile, the electrochemical active area has the same change trend with the contact angle, and the contact angle and the active area are less than 0.15mg cm-2The improvement is mainly due to the gradual increase of platinum on the surface of the carrier, and the high-density villous platinum enables the surface to show better hydrophobicity. When the platinum loading capacity is further increased, platinum loading is carried out on the surface of the carrier at positions where no empty space exists, excessive platinum can only grow on the surface of the platinum, the catalyst on the bottom layer is covered, the utilization rate of the platinum is reduced, and therefore the active area is reduced. The villous voids are covered with excess platinum to render the catalyst surface hydrophilic. In conclusion, an appropriate platinum loading may achieve an increase in hydrophobicity and an increase in electrochemical active area.
In the embodiment of the invention, the ordered stannic oxide and the carbon-coated stannic oxide carrier array are prepared by a hydrothermal method, and hydrophobic villous platinum is loaded on the carrier by a chemical reduction method. The invention provides a preparation method of a self-hydrophobic ordered array cathode structure by utilizing the advantages of simplicity and high efficiency of hydrothermal and room temperature reduction and combining the hydrophobic characteristic of villous platinum, the ordered carrier is more favorable for material transmission, the hydrophobic catalyst surface effectively avoids the flooding phenomenon, and the operation efficiency and stability of the battery are improved.
While several embodiments of the present invention have been presented herein, it will be appreciated by those skilled in the art that changes may be made to the embodiments herein without departing from the spirit of the invention. The above examples are merely illustrative and should not be taken as limiting the scope of the invention.
Claims (6)
1. A preparation method of a self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure is characterized by comprising the following steps:
s1, dissolving tin tetrachloride and thioacetamide in an organic solution, and fully stirring to prepare a solution A;
s2, placing the two diffusion layers in the inner liner of a reaction kettle, transferring the solution A into the reaction kettle, and reacting at a certain temperature to enable SnS2Growing on the surface of the diffusion layer; the reaction temperature is 160-200 ℃, and the reaction time is 12-36 hours;
s3, after the reaction in the step S2 is finished, the diffusion layer is cooled to room temperature, washed, dried and sintered at a certain temperature to obtain SnO2a/CP structure, wherein CP is a diffusion layer;
s4, mixing SnO2the/CP structure is placed in the inner liner of the reaction kettle, and a carbon source with a certain concentration is added for carbon coating at a certain temperature; the carbon source is sucrose, glucose or vitamin C; the concentration of the carbon source solution is 0.02-0.1mol/L, and 20-40ml of the carbon source solution is taken; when carbon coating is carried out, the hydrothermal reaction temperature is 160-190 ℃, and the reaction time is 3-24 hours;
s5, after the reaction in the step S4 is finished, cooling to room temperature, washing, drying, and sintering at a certain temperature to obtain SnO with a carbon-coated structure2@C/CP；
S6, coating carbon with SnO2@ C/CP is placed in a reaction container, and SnO is coated on a carbon coating structure by reducing Pt-based precursor2The @ C/CP is loaded with platinum to obtain a certain load amount of self-hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure Pt-SnO2@ C/CP, when the catalytic layer surface exhibits hydrophobic properties.
2. The method according to claim 1, wherein in step S3, the sintering temperature is 350-550 ℃, and the temperature rise rate is 1-5 ℃/min; the sintering time is 1-3 hours.
3. The method for preparing a self-hydrophobic integrated ordered catalytic layer-diffusion layer electrode structure according to claim 1, wherein in step S5, the sintering conditions are as follows: sintering for 1-5 hours at 500-900 ℃ under the atmosphere of argon, and the heating rate is 1-5 ℃/min.
4. The method according to claim 1, wherein in step S6, the reducing agent comprises ethylene glycol, formic acid, or sodium borohydride; the Pt-based precursor is chloroplatinic acid or acetylacetone platinum; the reaction time is 1 minute to 72 hours, and the platinum loading capacity is 0.05 mg/cm to 0.25mg/cm2。
5. A self-hydrophobic integrated ordered catalytic layer-diffusion layer electrode structure prepared by the preparation method of any one of claims 1 to 4.
6. The self-hydrophobic integrated ordered catalytic layer-diffusion layer electrode structure of claim 5, applied to a proton exchange membrane fuel cell.
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