CN111276704B - Preparation method of fuel cell electrode catalyst layer slurry, catalyst slurry and application thereof - Google Patents
Preparation method of fuel cell electrode catalyst layer slurry, catalyst slurry and application thereof Download PDFInfo
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Abstract
A preparation method of fuel cell electrode catalyst layer slurry comprises the steps of adding an additive in the pretreatment process of the catalyst slurry, and preparing a filter cake; in the preparation of the catalyst slurry, water, a low-boiling point solvent, a high-boiling point solvent and a high-viscosity solvent are respectively added into the obtained filter cake in sequence or simultaneously, and the catalyst slurry to be treated is prepared by ultrasonic stirring; the catalyst accounts for 0.5 to 15 percent of the mass of the catalyst slurry; fully stirring the obtained catalyst slurry to be treated in an inert atmosphere, standing, removing supernatant liquid, and repeatedly filtering until the slurry is fine and uniform; and stirring again to obtain catalyst slurry. The slurry prepared by the method has good uniformity, high stability, wide adjustable range of viscosity and viscoelasticity and strong practicability, can adjust the components according to the requirements of application targets, has wide applicable range and can be used for various electrode systems.
Description
Technical Field
The invention relates to a preparation method of catalyst slurry suitable for a membrane electrode of a fuel cell, in particular to a preparation method of slurry which can be used for preparing a gas diffusion electrode of the fuel cell or a catalyst layer electrode carried by a solid electrolyte membrane by a coating method.
The invention also relates to the application of the preparation method of the thermal catalyst slurry.
Background
In recent years, development of new clean energy, reasonable utilization of existing energy and environmental protection are coordinated with each other and developed, and the development of the world economy in this century is fundamental. Fuel Cells (Fuel Cells) are a power generation device which directly converts chemical energy into electric energy without a combustion process, have the outstanding advantages of high energy conversion efficiency, low pollution and environmental friendliness, are considered to be the first choice of clean and efficient power generation technology in the 21 st century, and become research and development focuses of governments and large companies. Fuel cells are classified into alkaline type, phosphoric acid type, solid polymer type, molten carbonate type, solid oxide type, and the like according to the type of electrolyte. Polymer Electrolyte Fuel Cells (PEFCs) are expected to be used as portable power sources, household power sources, and power sources for vehicles because they operate at low temperatures, have high output densities, and can be reduced in size and weight. After decades of development, the technology is mature and is now in the middle of commercialization. However, in order to realize large-scale use of the PEFC, breakthrough in key technology and key material must be realized to ensure stability and reliability thereof, while greatly reducing the cost thereof. A Membrane Electrode Assembly (MEA) is a core component of a PEFC, and is a key factor affecting the specific power density, energy density distribution, and operating life of the PEFC. The current MEA studies show that the problems with MEA are mainly concentrated on: the electrode catalyst layer and the gas diffusion layer are unreasonable in structure, so that the catalyst utilization rate is low, the transfer resistance of reaction gas and liquid water is high, and the concentration polarization loss of a high current density region is large; the output performance of the battery needs to be improved; the electrode preparation process is complicated, the automation degree is not high, and large-scale batch production is difficult to realize.
According to the invention, the catalyst slurry with excellent performance is prepared by catalyst pretreatment, preparation process optimization, catalyst slurry viscosity and solid content physical property optimization, and the slurry is used for preparing the catalyst layer of the fuel cell, so that the catalyst utilization rate in the prepared catalyst layer is high, and the mass transfer polarization in a high current density region in the cell reaction process is reduced.
Disclosure of Invention
The invention aims to provide a novel preparation method of catalyst slurry of a fuel cell membrane electrode, which has various slurry components and proportions and various specific preparation process flows. The preparation method of the catalyst slurry has the advantages of high preparation efficiency, high electrode performance, high electrode consistency, high operability and the like, and can be widely applied to the fields of oxyhydrogen fuel cells, direct methanol fuel cells, high-temperature polymer electrolyte membrane fuel cells, metal air cells and the like.
In order to achieve the purpose, the invention adopts the following scheme to realize the purpose:
a novel preparation method of catalyst slurry of a fuel cell membrane electrode comprises three parts of catalyst pretreatment, slurry preparation and slurry post-treatment, and a connecting step of coupling each part of processes.
A preparation method of slurry of an electrode catalyst layer of a fuel cell comprises the following steps,
a, pretreatment of a catalyst: fully mixing a catalyst with a mixed solution of water and an organic solvent to obtain a primary mixed slurry, adding an additive into the primary mixed slurry, fully mixing again, adding a high-boiling-point organic solvent, refluxing, cooling and filtering to obtain a filter cake for later use;
b, preparing a catalyst slurry: b, respectively adding water, a low-boiling point solvent, a high-boiling point solvent and a high-viscosity solvent into the filter cake obtained in the step a in sequence or simultaneously, and uniformly stirring by ultrasonic to obtain catalyst slurry to be treated; wherein the adding amount of water, the low boiling point solvent, the high boiling point solvent and the high viscosity solvent is 1 to 20 times of the mass of the catalyst respectively; the catalyst accounts for 0.5 to 15 percent of the mass of the catalyst slurry;
c, post-treatment of the catalyst slurry: b, fully stirring the catalyst slurry to be treated in the step b in an inert atmosphere, standing, removing supernatant liquid, and repeatedly filtering until the slurry is fine and uniform; and stirring again to obtain catalyst slurry.
The additive of the catalyst layer in the step a is one or more of a surfactant, a hydrophobic agent, an anticoagulant, a homogenizing agent and an ion conductor polymer, and the mass of the additive is 0.05-0.5 time of that of the catalyst. The catalyst layer additive is a key material for realizing the stability and the controllable viscosity range of the catalyst slurry;
and the high-viscosity solvent in the step b is one or more of dimethyl sulfoxide, ethylene glycol, N-methyl pyrrolidone and glycerol.
The organic solvent in the step a is one or more of ethanol, methanol, dimethylformamide, dimethylacetamide, cyclohexane, dimethyl ether, acetone and isopropanol;
the low-boiling-point solvent in the step b is one or more of ethanol, methanol, cyclohexane, dimethyl ether, acetone and isopropanol;
the high boiling point solvent in the step a or b is one or more of dimethylformamide, dimethylacetamide, ethylene glycol, dimethyl sulfoxide and formamide.
The high-boiling-point solvent in the step b is a key component for ensuring the stability of the catalyst slurry, and the catalyst slurry can keep the characteristic of difficult sedimentation for a long time in the high-speed stirring and coating processes due to the characteristic of difficult volatilization;
the high-viscosity solvent in the step b is a key component for ensuring the controllable viscosity range of the catalyst slurry, and the change of the content of the high-viscosity solvent can ensure that the viscosity of the slurry can be adjusted within a certain range so as to meet the requirement of a coating process;
and c, fully stirring under the inert atmosphere, namely sequentially adopting high-speed mechanical stirring, low-speed mechanical stirring and stirring under the ultrasonic condition.
The inert atmosphere is one or a mixture of more than two of nitrogen, helium and argon; the stirring speed of the high-speed mechanical stirring is 1000-;
the stirring speed of the low-speed mechanical stirring is 10-5000 revolutions per minute, and the duration time is 5-50 hours;
the stirring time under the ultrasonic condition is 0.5-5 hours.
C, standing for more than 0.5 hour, wherein the filtration is normal pressure or pressurization filtration, and the mesh number of a filter screen is 50-500;
the stirring is carried out for 0.5 to 4 hours under the ultrasonic condition again.
In the step a, the mass ratio of water to the organic solvent in the mixed solution of water and the organic solvent is 10:1 to 1: 10; the mass of the mixed solution of the water and the organic solvent is 5-100 times of that of the catalyst;
in the step a, the adding amount of the high-boiling-point organic solvent is 1-100 times of the mass of the primary mixed slurry; the reflux condition is reflux stirring for 1-10 hours at 80-200 ℃; the cooling is natural cooling.
The catalyst slurry prepared by the above preparation method.
The catalyst slurry is applied to preparing electrodes of direct methanol fuel cells, hydrogen-oxygen fuel cells, high-temperature polymer electrolyte membrane fuel cells or metal-air cells.
Compared with the prior art, the invention has the following advantages:
1, good slurry uniformity: the slurry prepared by the invention has good uniformity and high consistency of the particle size distribution of agglomerated particles;
2, the slurry has high stability: the prepared slurry has high stability, is not easy to settle and agglomerate after being stored for a long time, and is not easy to gather after flowing fast in a pipeline;
3, the adjustable range of viscosity and viscoelasticity is wide: the viscosity and viscoelastic property of the slurry prepared by the invention can be controlled in a larger range by adjusting the components of the slurry additive and the solvent;
4, the practicability is strong: the preparation process of the invention does not need to adopt harsh conditions, can modulate the components thereof according to the requirements of application targets, has wide applicable range and can be used for various electrode systems.
Description of the drawings:
FIG. 1, example 1 the agglomerate size distribution range of the catalyst slurry according to the invention. As shown, the agglomerate size distribution of the slurry is less than 15 microns over most of the agitation speed range. Figure 2, example 1 a catalyst slurry coating electrode loading profile prepared using the process of the present invention. As shown in the figure, the precious metal loading of the electrode catalyst layer is uniformly distributed, and the error is not more than 0.1 milligram per square centimeter.
Figure 3, example 1 a catalyst slurry coated electrode prepared using the method of the present invention, performance test results. Compared with the electrode prepared by the traditional comparative example, the electrode has better performance.
Detailed Description
The present invention will be described in detail below by way of examples, but the present invention is not limited to the following examples.
Example 1:
a, pretreatment of a catalyst:
fully wetting Pt/C (60%) catalyst powder adopted by an electrode with 2 times of deionized water, adding a mixed solution of water and ethanol with the mass ratio of 1:5, wherein the mass of the mixed solution is 5 times that of the catalyst, and ultrasonically stirring and dispersing for 1 hour until the mixed solution is uniform; adding an additive of 1:1 of polybenzimidazole and polytetrafluoroethylene, wherein the mass of the additive is 0.3 time of that of the catalyst, and fully and ultrasonically stirring for 2 hours until the mixture is uniform to obtain mixed slurry; adding a dimethylformamide solvent with the mass 50 times that of the mixed slurry, and refluxing and stirring for 5 hours at 120 ℃; naturally cooling and filtering, and keeping a filter cake for later use;
b, preparation of catalyst slurry
Adding water with 5 times of the mass of the catalyst into the filter cake obtained in the step a, and uniformly stirring by ultrasonic; adding methanol with 5 times of the mass of the catalyst, and uniformly stirring by ultrasonic; adding dimethylacetamide with the mass 2 times of that of the catalyst, and uniformly stirring by ultrasonic waves; adding dimethyl sulfoxide with the mass 3 times that of the catalyst, and ultrasonically stirring uniformly; the mass percentage of the catalyst in the total slurry is 4 percent; placing the mixed slurry in a stirring device protected by inert atmosphere, wherein the stirring speed is 50000 r/min and lasts for 2 hours, and then the stirring speed is 500 r/min and lasts for 24 hours; stirring the obtained slurry for 1 hour under the ultrasonic condition for later use;
c, post-treatment of the catalyst slurry
Standing the slurry prepared in the step for 2 hours, removing supernatant, and filtering the slurry at normal pressure by using a filter screen with the mesh number of 300; repeating the above operation for 3 times until the slurry is fine and uniform; the resulting slurry was ultrasonically stirred for 1 hour to complete the catalyst slurry preparation.
Comparative example 1:
in the traditional preparation method of the catalyst slurry, Pt/C (60%) catalyst powder adopted by an electrode is fully wetted by deionized water of 2 times, a mixed solution of water and ethanol with the mass ratio of 1:5 is added, the mass is 20 times that of the catalyst, and the mixture is ultrasonically stirred and dispersed for 1 hour until the mixture is uniform; adding a polytetrafluoroethylene additive with the mass being 0.1 time of that of the catalyst, and fully and ultrasonically stirring for 6 hours until the mixture is uniform to obtain mixed slurry.
Comparative example 2:
a, pretreatment of a catalyst:
fully wetting Pt/C (60%) catalyst powder adopted by an electrode with 2 times of deionized water, adding a mixed solution of water and ethanol with the mass ratio of 1:5, wherein the mass of the mixed solution is 5 times that of the catalyst, and ultrasonically stirring and dispersing for 1 hour until the mixed solution is uniform; adding a dimethylformamide solvent with the mass 50 times that of the mixed slurry, and refluxing and stirring for 5 hours at 120 ℃; naturally cooling and filtering, and keeping a filter cake for later use;
b, preparation of catalyst slurry
Adding water with 5 times of the mass of the catalyst into the filter cake obtained in the step a, and uniformly stirring by ultrasonic; adding methanol with 5 times of the mass of the catalyst, and uniformly stirring by ultrasonic; adding dimethylacetamide with the mass 2 times of that of the catalyst, and uniformly stirring by ultrasonic waves; adding dimethyl sulfoxide with the mass 3 times that of the catalyst, and ultrasonically stirring uniformly; the mass percentage of the catalyst in the total slurry is 4 percent; placing the mixed slurry in a stirring device protected by inert atmosphere, wherein the stirring speed is 50000 r/min and lasts for 2 hours, and then the stirring speed is 500 r/min and lasts for 24 hours; stirring the obtained slurry for 1 hour under the ultrasonic condition for later use;
c, post-treatment of the catalyst slurry
Standing the slurry prepared in the step for 2 hours, removing supernatant, and filtering the slurry at normal pressure by using a filter screen with the mesh number of 300; repeating the above operation for 3 times until the slurry is fine and uniform; the resulting slurry was ultrasonically stirred for 1 hour to complete the catalyst slurry preparation.
Slurry samples without the catalytic layer additive are easy to generate coagulation, the slurry uniformity and stability are not high, and the slurry viscosity is relatively lower than that of the additive samples, so that the coating requirement is difficult to meet.
Comparative example 3:
a, pretreatment of a catalyst:
fully wetting Pt/C (60%) catalyst powder adopted by an electrode with 2 times of deionized water, adding a mixed solution of water and ethanol with the mass ratio of 1:5, wherein the mass of the mixed solution is 5 times that of the catalyst, and ultrasonically stirring and dispersing for 1 hour until the mixed solution is uniform; adding an additive of 1:1 of polybenzimidazole and polytetrafluoroethylene, wherein the mass of the additive is 0.3 time of that of the catalyst, and fully and ultrasonically stirring for 2 hours until the mixture is uniform to obtain mixed slurry; adding a dimethylformamide solvent with the mass 50 times that of the mixed slurry, and refluxing and stirring for 5 hours at 120 ℃; naturally cooling and filtering, and keeping a filter cake for later use;
b, preparation of catalyst slurry
Adding water with 5 times of the mass of the catalyst into the filter cake obtained in the step a, and uniformly stirring by ultrasonic; adding methanol with the weight 10 times that of the catalyst, and ultrasonically stirring uniformly; the mass percentage of the catalyst in the total slurry is 6 percent; placing the mixed slurry in a stirring device protected by inert atmosphere, wherein the stirring speed is 50000 r/min and lasts for 2 hours, and then the stirring speed is 500 r/min and lasts for 24 hours; stirring the obtained slurry for 1 hour under the ultrasonic condition for later use;
c, post-treatment of the catalyst slurry
Standing the slurry prepared in the step for 2 hours, removing supernatant, and filtering the slurry at normal pressure by using a filter screen with the mesh number of 300; repeating the above operation for 3 times until the slurry is fine and uniform; the resulting slurry was ultrasonically stirred for 1 hour to complete the catalyst slurry preparation.
The slurry without the high-boiling-point solvent and the high-viscosity solvent in the step b has low stability and is easy to agglomerate, and the viscosity of the slurry is relatively lower than that of a sample with the additive, so that the coating requirement is difficult to meet.
Example 2:
a, pretreatment of a catalyst:
fully wetting PtCo/C (50%) catalyst powder adopted by an electrode with 1 time of deionized water, adding a mixed solution of water and cyclohexane in a mass ratio of 1:1, wherein the mass of the mixed solution is 10 times that of the catalyst, and ultrasonically stirring and dispersing for 4 hours until the mixed solution is uniform; adding a mixture of sodium dodecyl benzene sulfonate and perfluorosulfonic acid polymer in a molar ratio of 1:1, wherein the mass of the mixture is 0.05 times that of the catalyst, and fully and ultrasonically stirring for 2 hours until the mixture is uniform to obtain mixed slurry; adding formamide solvent with the mass 50 times of that of the mixed slurry, and refluxing and stirring for 4 hours at the temperature of 100 ℃; naturally cooling and filtering, and keeping a filter cake for later use;
b, preparation of catalyst slurry
Adding water with the mass 2 times that of the catalyst into the filter cake obtained in the step a, and uniformly stirring by ultrasonic; adding acetone with the mass 3 times that of the catalyst, and ultrasonically stirring uniformly; adding ethylene glycol with the mass 5 times of that of the catalyst, and uniformly stirring by ultrasonic; adding glycerol with the mass 3 times that of the catalyst, and uniformly stirring by ultrasonic; the mass percentage of the catalyst in the total slurry is 7 percent; placing the mixed slurry in a stirring device protected by inert atmosphere, wherein the stirring speed is 10000 revolutions per minute and lasts for 5 hours, and then the stirring speed is 200 revolutions per minute and lasts for 48 hours; stirring the obtained slurry for 1 hour under the ultrasonic condition for later use;
c, post-treatment of the catalyst slurry
Standing the slurry prepared in the step for 1 hour, removing supernatant, and performing pressure-increasing filtration by using a filter screen with 500 meshes; repeating the above operation for 5 times until the slurry is fine and uniform; the resulting slurry was ultrasonically stirred for 4 hours to complete the catalyst slurry preparation.
Claims (8)
1. A preparation method of slurry of an electrode catalyst layer of a fuel cell is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
a, pretreatment of a catalyst: fully mixing a catalyst with a mixed solution of water and an organic solvent to obtain a primary mixed slurry, adding an additive into the primary mixed slurry, fully mixing again, adding a high-boiling-point organic solvent, refluxing, cooling and filtering to obtain a filter cake for later use; the catalyst layer additive in the step a is a mixture of polybenzimidazole and polytetrafluoroethylene with a molar ratio of 1:1, and a mixture of sodium dodecyl benzene sulfonate and perfluorosulfonic acid polymer with a molar ratio of 1: 1; the mass of the additive is 0.05-0.3 time of that of the catalyst;
b, preparing a catalyst slurry: b, adding water, a low-boiling point solvent, a high-boiling point solvent and a high-viscosity solvent, or adding water, a low-boiling point solvent and a high-boiling point solvent, or adding water, a low-boiling point solvent and a high-viscosity solvent into the filter cake obtained in the step a respectively in sequence or simultaneously, and performing ultrasonic stirring uniformly to obtain catalyst slurry to be treated; wherein the adding amount of water, the low boiling point solvent, the high boiling point solvent and the high viscosity solvent is 2 to 5 times of the mass of the catalyst respectively; the catalyst accounts for 4-7% of the catalyst slurry by mass; the high-viscosity solvent in the step b is one or more of N-methyl pyrrolidone and glycerol; the low-boiling-point solvent in the step b is one or more of ethanol, methanol, cyclohexane, dimethyl ether, acetone and isopropanol;
c, post-treatment of the catalyst slurry: b, fully stirring the catalyst slurry to be treated in the step b in an inert atmosphere, standing, removing supernatant liquid, and repeatedly filtering until the slurry is fine and uniform; stirring again to obtain catalyst slurry;
the high boiling point solvent in the step a or b is one or more of dimethylformamide, dimethylacetamide, ethylene glycol, dimethyl sulfoxide and formamide.
2. The method of claim 1, wherein:
the organic solvent in the step a is one or more of ethanol, methanol, dimethylformamide, dimethylacetamide, cyclohexane, dimethyl ether, acetone and isopropanol.
3. The method of claim 1, wherein:
and c, fully stirring under the inert atmosphere, namely sequentially adopting high-speed mechanical stirring, low-speed mechanical stirring and stirring under the ultrasonic condition.
4. The method of claim 3, wherein:
the inert atmosphere is one or a mixture of more than two of nitrogen, helium and argon;
the stirring speed of the high-speed mechanical stirring is 1000-;
the stirring speed of the low-speed mechanical stirring is 10-5000 revolutions per minute, and the duration time is 5-50 hours;
the stirring time under the ultrasonic condition is 0.5-5 hours.
5. The method of claim 1, wherein:
c, standing for more than 0.5 hour, wherein the filtration is normal pressure or pressurization filtration, and the mesh number of a filter screen is 50-500;
the stirring is carried out for 0.5 to 4 hours under the ultrasonic condition again.
6. The method of claim 1, wherein:
in the step a, the mass ratio of water to the organic solvent in the mixed solution of water and the organic solvent is 10:1 to 1: 10; the mass of the mixed solution of the water and the organic solvent is 5-10 times of that of the catalyst;
in the step a, the adding amount of the high-boiling-point organic solvent is 1-100 times of the mass of the primary mixed slurry;
the reflux condition is reflux stirring for 1-10 hours at 80-200 ℃; the cooling is natural cooling.
7. A catalyst slurry prepared by the process of any one of claims 1 to 6.
8. Use of the catalyst slurry of claim 7 in the preparation of an electrode for a direct methanol fuel cell, a hydrogen-oxygen fuel cell, a high temperature polymer electrolyte membrane fuel cell or a metal air cell.
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| CN104716342A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Fuel cell catalyst slurry and application thereof |
| CN105390704A (en) * | 2014-09-02 | 2016-03-09 | 通用汽车环球科技运作有限责任公司 | electrode design with optimal ionomer content for polymer electrolyte membrane fuel cell |
| WO2018101591A1 (en) * | 2016-11-30 | 2018-06-07 | 주식회사 엘지화학 | Method for preparing membrane-electrode assembly, membrane-electrode assembly prepared therefrom, and fuel cell comprising same |
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- 2018-12-04 CN CN201811474236.3A patent/CN111276704B/en active Active
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| WO2012153915A2 (en) * | 2011-05-11 | 2012-11-15 | 한국화학연구원 | Method for manufacturing a membrane-electrode assembly for a polymer electrolyte, and membrane-electrode assembly manufactured thereby |
| CN102437343A (en) * | 2011-11-17 | 2012-05-02 | 华南理工大学 | Membrane electrode containing hydrophilic high polymer in anode catalytic layer and preparation method thereof |
| CN104716342A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Fuel cell catalyst slurry and application thereof |
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