CN114388820A - Catalyst slurry for fuel cell and preparation method thereof - Google Patents
Catalyst slurry for fuel cell and preparation method thereof Download PDFInfo
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- CN114388820A CN114388820A CN202111500342.6A CN202111500342A CN114388820A CN 114388820 A CN114388820 A CN 114388820A CN 202111500342 A CN202111500342 A CN 202111500342A CN 114388820 A CN114388820 A CN 114388820A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
Abstract
The invention relates to the technical field of catalyst slurry, in particular to catalyst slurry for a fuel cell and a preparation method thereof. Firstly, uniformly mixing functional additives in ultrapure water to obtain a first dispersion liquid; adding the catalyst powder into the first dispersion liquid, and uniformly mixing to obtain a second dispersion liquid; then adding alcohol and ionomer into the second dispersion liquid, and uniformly mixing to obtain a third dispersion liquid; finally, performing reinforced dispersion on the third dispersion liquid to obtain catalyst slurry for the fuel cell; the method optimizes the rheological property and the dispersity of the catalyst slurry. In the preparation process of the catalyst slurry, the functional auxiliary agent is added to assist the dispersion of the catalyst powder, the viscosity of the catalyst slurry is increased, the improvement of the dispersion uniformity of catalyst slurry particles, the reduction of the particle size in the slurry and the improvement of the utilization rate of Pt are facilitated, and the power generation performance of a fuel cell can be further improved when the catalyst slurry is applied to a membrane electrode.
Description
Technical Field
The invention relates to the technical field of catalyst slurry, in particular to catalyst slurry for a fuel cell and a preparation method thereof.
Background
The catalyst slurry is the starting point of the preparation of the membrane electrode which is the core component of the proton exchange membrane fuel cell, and the property of the catalyst slurry and the drying process thereof determine the structure and the performance of the catalytic layer of the power generation part in the membrane electrode. The catalyst slurry is a multi-component, multi-phase system comprising catalyst powder, dispersing solvent, ionomer, the internal structure of which is maintained in relative equilibrium by the interaction of the components and under the action of external forces. The conventional membrane electrode preparation method at present is slit extrusion coating, slurry is dried after being coated on a base material to form a catalyst layer, catalyst distribution, ionomer distribution and pore structure distribution in the catalyst layer jointly form a structure of the catalyst layer, and an ideal catalyst layer structure requires that catalyst powder in the slurry is dispersed as much as possible to achieve the maximum utilization of Pt. This limits the performance of the catalyst ink. For enterprise production, dispersion control of the slurry is necessary. In addition, the state of the particles and binder within the slurry can affect its processability, mainly in terms of its rheological properties, which are suitable for facilitating slurry coating, resulting in a regular, defect-free wet film coating.
Through literature search and market research in the prior art, the regulation and control of the internal structure of the catalyst slurry in the preparation process are generally optimized based on a formula or a process, so that the aims of improving the particle dispersion uniformity and regulating and controlling the rheological property of the catalyst slurry are fulfilled. In the chinese patent "method for preparing high-stability fuel cell catalyst coating slurry" (publication No. CN112563518A), zhao ming quan et al proposed a method of dispersing twice and adding ionomer solution and solvent in several times to improve slurry dispersion stability, and reduce particle size to improve power generation performance of fuel cells. In the chinese patent "application of sulfonated polyaryletherketone as a binder in a membrane electrode of a proton exchange membrane fuel cell, a membrane electrode and a preparation method" (publication No. CN113161557A), zhao cheng ji proposes to use sulfonated polyaryletherketone as a binder to improve the interface compatibility of the binder and the proton exchange membrane, and optimize the three-phase interface in the catalyst layer, thereby improving the power generation performance of the fuel cell. In the chinese patent "a proton exchange membrane fuel cell catalyst layer and a method for preparing the same" (publication No. CN112786904A), it is proposed by luggin et al that cetyl trimethyl ammonium bromide and a sulfonate group with negative charges in perfluorosulfonic acid resin are added to a slurry to reduce the compactness of the perfluorosulfonic acid resin film in the catalyst layer by the action of electrostatic force, thereby improving the oxygen transport capability of the catalyst layer. The Chinese patent 'platinum monatomic dispersed catalyst and the preparation method thereof' (application number: 201511017815.1) designs and prepares a platinum monatomic catalyst by taking a carbon carrier, a non-metallic impurity atom reagent and a platinum compound as raw materials, and improves the utilization rate of platinum. However, the conventional dispersing process and formula addition auxiliary agent are not considered to be matched to increase the dispersibility of the slurry and regulate and control the rheological property of the slurry in the existing related researches, and a synergistic optimization method for the rheological property and the dispersion uniformity of the slurry is lacked.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a catalyst slurry for a fuel cell and a method for preparing the same. Firstly, uniformly mixing functional additives in ultrapure water to obtain a first dispersion liquid; adding the catalyst powder into the first dispersion liquid, and uniformly mixing to obtain a second dispersion liquid; then adding alcohol and ionomer into the second dispersion liquid, and uniformly mixing to obtain a third dispersion liquid; finally, performing reinforced dispersion on the third dispersion liquid to obtain catalyst slurry for the fuel cell; the method optimizes the rheological property and the dispersity of the catalyst slurry. In the preparation process of the catalyst slurry, the functional auxiliary agent is added to assist the dispersion of the catalyst powder, the viscosity of the catalyst slurry is increased, the improvement of the dispersion uniformity of catalyst slurry particles, the reduction of the particle size in the slurry and the improvement of the utilization rate of Pt are facilitated, and the power generation performance of a fuel cell can be further improved when the catalyst slurry is applied to a membrane electrode.
The purpose of the invention can be realized by the following technical scheme:
the invention aims to provide a preparation method of catalyst slurry for a fuel cell, which comprises the following steps:
(1) uniformly mixing the functional additive in ultrapure water to obtain a first dispersion liquid;
(2) adding catalyst powder into the first dispersion liquid obtained in the step (1), and uniformly mixing to obtain a second dispersion liquid;
(3) adding alcohol and ionomer into the second dispersion liquid obtained in the step (2), and uniformly mixing to obtain a third dispersion liquid;
(4) and (4) performing enhanced dispersion on the third dispersion liquid obtained in the step (3) to obtain the catalyst slurry for the fuel cell.
In one embodiment of the present invention, in step (1), the functional auxiliary is selected from one or more of polyurethane, acrylic acid, sodium hydroxypropyl methylcellulose or sodium carboxymethyl cellulose.
In one embodiment of the invention, in the step (1), the mass ratio of the functional assistant to the ultrapure water is 1-100: 1000.
in one embodiment of the invention, in the step (1), the blending is ultrasonic blending, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes.
In one embodiment of the present invention, in the step (2), the catalyst powder is selected from one or more of a Pt/C catalyst, a PtCo/C catalyst or a PtNi/C catalyst.
In one embodiment of the present invention, in the step (2), the mass ratio of the catalyst powder to the ultrapure water in the first dispersion is 1 to 8: 20.
in one embodiment of the invention, in the step (2), the blending is ultrasonic blending, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes.
In one embodiment of the present invention, in the step (3), the alcohol is selected from one or more of n-propanol, isopropanol, ethanol or methanol.
In one embodiment of the present invention, in step (3), the mass ratio of alcohol to ionomer is 7: 8; the mass ratio of the alcohol to the ultrapure water in the second dispersion liquid is 7-15: 10.
in one embodiment of the invention, in the step (3), the blending is ultrasonic blending, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes.
In one embodiment of the present invention, in the step (4), the intensive dispersion is one or more selected from homogeneous dispersion, ultrasonic dispersion, high-speed shearing or hydrodynamic cavitation.
In one embodiment of the present invention, in the step (4), the intensive dispersion time is 10min to 120 min.
A second object of the present invention is to provide a catalyst slurry for a fuel cell prepared by the above method.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the catalyst slurry for the fuel cell, disclosed by the invention, is also a preparation method of the catalyst slurry with optimized rheological property and dispersibility.
Drawings
FIG. 1 is a flow chart of a method for preparing a catalyst slurry for a fuel cell according to the present invention;
FIG. 2 is a graph comparing shear stress of example 1 and comparative example 1 in accordance with the present invention;
FIG. 3 is a graph comparing viscosity curves of example 1 and comparative example 1 in accordance with the present invention;
FIG. 4 is a graph comparing particle size curves for example 1 and comparative example 1 in accordance with the present invention;
FIG. 5 is a graph comparing shear stress of example 2 and comparative example 2 according to the present invention;
FIG. 6 is a graph comparing viscosity curves of example 2 and comparative example 2 in accordance with the present invention;
FIG. 7 is a graph comparing particle size curves for example 2 and comparative example 2 in accordance with the present invention;
FIG. 8 is a graph comparing shear stress of example 3 and comparative example 1 in accordance with the present invention;
FIG. 9 is a graph comparing viscosity curves of example 3 and comparative example 1 in accordance with the present invention;
FIG. 10 is a graph comparing particle size curves of example 3 and comparative example 1 in accordance with the present invention.
Detailed Description
The invention provides a preparation method of catalyst slurry for a fuel cell, which comprises the following steps:
(1) uniformly mixing the functional additive in ultrapure water to obtain a first dispersion liquid;
(2) adding catalyst powder into the first dispersion liquid obtained in the step (1), and uniformly mixing to obtain a second dispersion liquid;
(3) adding alcohol and ionomer into the second dispersion liquid obtained in the step (2), and uniformly mixing to obtain a third dispersion liquid;
(4) and (4) performing reinforced dispersion on the third dispersion liquid obtained in the step (3) to obtain catalyst slurry.
In one embodiment of the present invention, in step (1), the functional auxiliary is selected from one or more of polyurethane, acrylic acid, sodium hydroxypropyl methylcellulose or sodium carboxymethyl cellulose.
In one embodiment of the invention, in the step (1), the mass ratio of the functional assistant to the ultrapure water is 1-100: 1000.
in one embodiment of the invention, in the step (1), the blending is ultrasonic blending, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes.
In one embodiment of the present invention, in the step (2), the catalyst powder is selected from one or more of a Pt/C catalyst, a PtCo/C catalyst or a PtNi/C catalyst.
In one embodiment of the present invention, in the step (2), the mass ratio of the catalyst powder to the ultrapure water in the first dispersion is 5 to 40: 100.
in one embodiment of the invention, in the step (2), the blending is ultrasonic blending, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes.
In one embodiment of the present invention, in the step (3), the alcohol is selected from one or more of n-propanol, isopropanol, ethanol or methanol.
In one embodiment of the present invention, in step (3), the mass ratio of alcohol to ionomer is 17.5: 1; the mass ratio of the alcohol to the ultrapure water in the second dispersion liquid is 7-15: 10.
in one embodiment of the invention, in the step (3), the blending is ultrasonic blending, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes.
In one embodiment of the present invention, in the step (4), the intensive dispersion is one or more selected from homogeneous dispersion, ultrasonic dispersion, high-speed shearing or hydrodynamic cavitation.
In one embodiment of the present invention, in the step (4), the intensive dispersion time is 10min to 120 min.
The invention provides a catalyst slurry for a fuel cell prepared by the method.
The invention is described in detail below with reference to the figures and specific embodiments.
The ionomer in the examples is komer D520; the others are commercially available unless otherwise specified.
Example 1
The embodiment provides a catalyst slurry for a fuel cell and a preparation method thereof.
(1) Adding 0.014g of sodium carboxymethylcellulose into 14g of ultrapure water for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a first dispersion liquid;
(2) adding 4g of 60 wt% Pt/C catalyst into the first dispersion liquid for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes to obtain a second dispersion liquid;
(3) adding 14g of n-propanol and 16g of Komer D520 (the mass percentage concentration is 5%) into the second dispersion liquid for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a third dispersion liquid;
(4) and (4) performing reinforced dispersion on the third dispersion liquid in an ultrasonic dispersion mode for 10min, wherein the pressure of a homogenizer is 500Bar, and thus obtaining the catalyst slurry for the fuel cell.
Example 2
The embodiment provides a catalyst slurry for a fuel cell and a preparation method thereof.
(1) Adding 1.4g of acrylic acid into 14g of ultrapure water for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a first dispersion liquid;
(2) adding 5.6g of 60 wt% PtCo/C catalyst into the first dispersion liquid for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a second dispersion liquid;
(3) adding 9.8g of isopropanol and 11.2g of Komer D520 (the mass percentage concentration is 5%) into the second dispersion liquid for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a third dispersion liquid;
(4) and (4) intensively dispersing the third dispersion liquid in a high-speed shearing mode for 120min at the rotating speed of 4000rpm to obtain the catalyst slurry for the fuel cell.
Example 3
The embodiment provides a catalyst slurry for a fuel cell and a preparation method thereof.
(1) Adding 0.4g of polyurethane into 14g of ultrapure water for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a first dispersion liquid;
(2) adding 0.7g of 60 wt% PtNi/C catalyst into the first dispersion liquid for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes to obtain a second dispersion liquid;
(3) adding 21g of ethanol and 24g of Kemei D520 (the mass percentage concentration is 5%) into the second dispersion liquid for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a third dispersion liquid;
(4) and (3) performing reinforced dispersion on the third dispersion liquid in an ultrasonic dispersion mode for 60min, wherein the ultrasonic power is 100W, and the ultrasonic temperature is 15 ℃, so as to obtain the catalyst slurry for the fuel cell.
Comparative example 1
The present example provides a catalyst paste and a method for preparing the same.
(1) Adding 4g of 60 wt% Pt/C catalyst into 14g of ultrapure water for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes to obtain a first dispersion liquid;
(2) adding 14g of n-propanol and 16g of Komer D520 (the mass percentage concentration is 5%) into the first dispersion liquid, and carrying out ultrasonic treatment, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a second dispersion liquid;
(3) performing intensified dispersion on the second dispersion liquid in a homogeneous dispersion mode for 30min to obtain catalyst slurry; wherein the homogenizer pressure is 500 Bar.
Comparative example 2
The present example provides a catalyst paste and a method for preparing the same.
(1) Adding 4g of 60 wt% Pt/C catalyst into 14g of ultrapure water for ultrasonic dispersion, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes to obtain a first dispersion liquid;
(2) adding 14g of n-propanol and 16g of Komer D520 (the mass percentage concentration is 5%) into the first dispersion liquid, and carrying out ultrasonic treatment, wherein the ultrasonic power is 80W, the ultrasonic temperature is 15 ℃, and the ultrasonic time is 5 minutes, so as to obtain a second dispersion liquid;
(3) and (4) intensively dispersing the second dispersion liquid in a high-speed shearing mode for 120min at the rotating speed of 4000rpm to obtain catalyst slurry.
And (4) experimental conclusion:
FIG. 1 is a block diagram of a method for preparing a catalyst slurry for a fuel cell according to examples 1, 2 and 3;
as shown in FIG. 2, the shear stress at the same shear rate due to the addition of the functional assistant in example 1 is higher than that in comparative example 1, and particularly the yield stress is 2.50 higher than that in comparative example 1, which is 1.56. This indicates that the addition of the functional assistant can enhance the structural strength of the catalyst slurry particles;
as shown in fig. 3, the viscosities of comparative example 1 and example 1 are substantially the same in the high shear region and the low shear region, respectively, a shear viscosity plateau occurs in the medium shear region, and the increase in viscosity of example 1 is higher than that of comparative example 1, which contributes to the improvement in the stability of the catalyst slurry.
As shown in fig. 4, the particle size of example 1 is smaller than that of comparative example 1, and the distribution of large particles is also lower than that of comparative example 1, indicating that the addition of the functional assistant can reduce the particle size of the catalyst slurry particles and improve the particle dispersion uniformity.
As shown in fig. 5 and 8, examples 2 and 3 can increase the yield stress of the catalyst slurry due to the addition of the functional assistant, fig. 6 and 9 show that examples 2 and 3 can increase the viscosity of the catalyst slurry due to the addition of the functional assistant, and fig. 7 and 10 show that examples 2 and 3 can reduce the particle size of particles in the catalyst slurry due to the addition of the functional assistant.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of catalyst slurry for a fuel cell is characterized by comprising the following steps:
(1) uniformly mixing the functional additive in ultrapure water to obtain a first dispersion liquid;
(2) adding catalyst powder into the first dispersion liquid obtained in the step (1), and uniformly mixing to obtain a second dispersion liquid;
(3) adding alcohol and ionomer into the second dispersion liquid obtained in the step (2), and uniformly mixing to obtain a third dispersion liquid;
(4) and (4) performing enhanced dispersion on the third dispersion liquid obtained in the step (3) to obtain the catalyst slurry for the fuel cell.
2. The method for preparing a catalyst slurry for a fuel cell according to claim 1, wherein in the step (1), the functional auxiliary is one or more selected from polyurethane, acrylic acid, sodium hydroxypropyl methylcellulose and sodium carboxymethyl cellulose.
3. The method for preparing a catalyst slurry for a fuel cell according to claim 1, wherein in the step (1), the mass ratio of the functional assistant to the ultrapure water is 1 to 100: 1000.
4. the method of claim 1, wherein in the step (2), the catalyst powder is selected from one or more of a Pt/C catalyst, a PtCo/C catalyst and a PtNi/C catalyst.
5. The method of producing a catalyst paste for a fuel cell according to claim 1, wherein in the step (2), the mass ratio of the catalyst powder to the ultrapure water in the first dispersion liquid is from 1 to 8: 20.
6. the method for preparing a catalyst slurry for a fuel cell according to claim 1, wherein in the step (3), the alcohol is one or more selected from n-propanol, isopropanol, ethanol, and methanol.
7. The method of preparing a catalyst slurry for a fuel cell according to claim 1, wherein in the step (3), the mass ratio of the alcohol to the ionomer is 17.5: 1; the mass ratio of the alcohol to the ultrapure water in the second dispersion liquid is 7-15: 10.
8. the method for preparing a catalyst slurry for a fuel cell according to claim 1, wherein in the step (4), the intensive dispersion is one or more selected from the group consisting of homogeneous dispersion, ultrasonic dispersion, high-speed shear and hydrodynamic cavitation.
9. The method for preparing a catalyst slurry for a fuel cell according to claim 1, wherein the intensive dispersion time in the step (4) is 10min to 120 min.
10. A fuel cell catalyst slurry prepared by the method of any one of claims 1 to 9.
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| JP2016170949A (en) * | 2015-03-12 | 2016-09-23 | 凸版印刷株式会社 | Catalyst ink for formation of electrode catalyst layer of solid polymer fuel cell, and method for manufacturing the same |
| CN108461786A (en) * | 2016-12-10 | 2018-08-28 | 中国科学院大连化学物理研究所 | A kind of preparation method and fuel cell of fuel cell membrane electrode |
| CN111261878A (en) * | 2020-01-23 | 2020-06-09 | 同济大学 | Catalyst slurry containing aqueous gel, catalyst layer and fuel cell electrode produced therefrom |
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2021
- 2021-12-09 CN CN202111500342.6A patent/CN114388820A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH08236123A (en) * | 1994-12-28 | 1996-09-13 | Tokyo Gas Co Ltd | Fuel cell electrode and manufacture thereof |
| JP2005302473A (en) * | 2004-04-09 | 2005-10-27 | Toyota Motor Corp | Powdery catalyst material, its manufacturing method, electrode for solid polymer fuel cell using powdery catalyst material |
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