CN114941153A - Water electrolysis membrane electrode based on proton exchange membrane, preparation method, assembly and application - Google Patents
Water electrolysis membrane electrode based on proton exchange membrane, preparation method, assembly and application Download PDFInfo
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- 238000011068 loading method Methods 0.000 claims abstract description 24
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- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 5
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- 239000000463 material Substances 0.000 claims description 4
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- 239000002184 metal Substances 0.000 claims description 4
- 229910000566 Platinum-iridium alloy Inorganic materials 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- CRBDXVOOZKQRFW-UHFFFAOYSA-N [Ru].[Ir]=O Chemical compound [Ru].[Ir]=O CRBDXVOOZKQRFW-UHFFFAOYSA-N 0.000 claims description 2
- HWLDNSXPUQTBOD-UHFFFAOYSA-N platinum-iridium alloy Chemical class [Ir].[Pt] HWLDNSXPUQTBOD-UHFFFAOYSA-N 0.000 claims description 2
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- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
- C25B11/053—Electrodes comprising one or more electrocatalytic coatings on a substrate characterised by multilayer electrocatalytic coatings
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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Abstract
The invention belongs to the technical field of water electrolysis membrane electrodes, and particularly relates to a water electrolysis membrane electrode based on a proton exchange membrane, a preparation method, an assembly and application. The structure of the water electrolysis membrane electrode is specifically as follows: a first anode catalyst layer and a second anode catalyst layer are sequentially arranged on one side of the proton exchange membrane, and a cathode catalyst layer is arranged on the other side of the proton exchange membrane; the first anode catalyst layer comprises a platinum-based catalyst and first ion exchange resin, and the content of the first ion exchange resin is 50-95 wt%; the thickness of the first anode catalytic layer is not more than 20 mum; the second anode catalytic layer comprises an oxygen evolution catalyst and a second ion exchange resin, and the content of the second ion exchange resin is not more than 30 wt%. The membrane electrode structure not only effectively reduces the hydrogen concentration in the anode product, but also can improve the utilization rate of the oxygen evolution catalyst, and reduce the noble metal loading capacity of the oxygen evolution catalyst to 0.2-0.6 mg/cm 2 。
Description
Technical Field
The invention belongs to the technical field of water electrolysis membrane electrodes, and particularly relates to a water electrolysis membrane electrode based on a proton exchange membrane, a preparation method, an assembly and application.
Background
The water electrolyzer has the advantages of compact system, high current density, direct production of high-pressure hydrogen and the like, can be used with fluctuating renewable energy sources (wind power, photoelectricity, hydropower and the like), and has wide application prospect.
The membrane electrode is a key core component of a PEM water electrolyzer, and generally comprises a proton exchange membrane, an anode catalyst layer, a cathode catalyst layer and the like. The anode side and the cathode side of the water electrolysis membrane electrode respectively generate oxygen and hydrogen, and the proton exchange membrane plays a role in transferring protons and separating a cathode chamber from an anode chamber. The high-performance water electrolysis membrane electrode should have reasonable pore structure and pore distribution so as to facilitate the transmission of reactants and products, and the catalytic layer and the proton exchange membrane should be well combined so as to reduce the contact resistance.
At present, the methodThe commercial water electrolysis membrane electrode still adopts anode catalyst with higher loading (1.5-2.5 mg) IrO2 /cm 2 ) The performance and stability of the electrolytic cell are ensured, and the Ir resource has limited reserves and high price, and must become one of the bottlenecks in large-scale development of hydrogen production by water electrolysis. The invention patent with publication number CN102260877B discloses a preparation method of a pure water electrolytic ion membrane electrode, which mainly adopts a transfer printing method to replace a hot pressing method to prepare the membrane electrode, solves the problems of wrinkling of the membrane electrode, uneven coating of a catalyst layer and the like in the preparation process, but the loading amount of the used anode catalyst is up to 4.2mg/cm 2 The cost is high.
In addition, thicker proton exchange membranes (e.g., Nafion) are still used as commercial water electrolysis membrane electrodes TM 115 and Nafion TM 117 films with thicknesses of 127 μm and 183 μm, respectively) to prevent hydrogen diffusion to the anode. Thicker proton exchange membranes, while effective in reducing hydrogen permeation, tend to reduce cell voltage. The adoption of thinner proton exchange membranes is the development direction of water electrolysis membrane electrodes, but the problem of how to solve the high-pressure hydrogen permeation is a difficult problem. The permeation of hydrogen to the anode causes the following problems: 1) potential safety hazards are caused by mixing hydrogen and oxygen; 2) reducing the purity of the oxygen product; 3) reducing the durability of the anode catalyst; 4) the hydrogen permeating to the anode directly reacts with the anode to generate water, and the electrolysis efficiency is reduced.
The patent publication CN113235120B discloses a water electrolysis CCM (catalyst-coated membrane) with a sandwich-type PEM as the substrate material, wherein the sandwich is a platinum or iridium-based catalyst, and is located between two proton exchange membranes for oxidizing permeated hydrogen (cathode high pressure), suppressing the amount of hydrogen permeation, and reducing the risk. The method has complex process, and the proton exchange membranes positioned at the two sides of the interlayer need to be contacted with the interlayer (catalyst layer), so that the contact resistance between layers is obviously increased, and the performance of the membrane electrode is reduced.
Disclosure of Invention
The invention aims to: aiming at the technical problems of low utilization rate and high-pressure hydrogen permeation of anode catalysts of water electrolysis membrane electrodes in the prior art, a water electrolysis membrane electrode based on a proton exchange membrane and a preparation method thereof are provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a water electrolysis membrane electrode is characterized in that a first anode catalyst layer and a second anode catalyst layer are sequentially arranged on one side of a proton exchange membrane, and a cathode catalyst layer is arranged on the other side of the proton exchange membrane;
the first anode catalytic layer comprises a platinum-based catalyst and a first ion exchange resin; the content of the first ion exchange resin is 50-95 wt%;
the second anode catalyst layer comprises an oxygen evolution catalyst and second ion exchange resin, and the content of the second ion exchange resin is not more than 30 wt%.
The invention provides a water electrolysis membrane electrode structure, wherein a first anode catalyst layer is added between a second anode catalyst layer and a proton exchange membrane. The second anode catalytic layer mainly functions to catalyze the decomposition of water into oxygen and to transport reactants (water) and products (O) 2 ) The main purpose of controlling the ion exchange resin content in this layer to a low level (not more than 30 wt%) includes two: on one hand, the method is favorable for exposing more catalyst active sites and improving the utilization rate of the oxygen evolution catalyst, and on the other hand, the ion exchange resin with lower content is favorable for keeping higher porosity of the second anode catalyst layer, thereby improving the transmission efficiency of reactants and products in the second anode catalyst layer. The first anode catalyst layer is added between the second anode catalyst layer and the proton exchange membrane, so that the contact resistance of an interface is reduced, the performance of the membrane electrode is improved, the platinum-containing catalyst in the first anode catalyst layer can catalyze hydrogen to be oxidized, hydrogen permeated from a cathode is not collected or discharged, and the safety risk is reduced.
As a preferable aspect of the present invention, the thickness of the first anode catalytic layer is not more than 15 μm. Preferably, the thickness of the first anode catalyst layer is 2-15 μm.
In a preferred embodiment of the present invention, the roughness of the first anode catalyst layer ranges from Ra 0.1 μm to Ra12.5 μm. The first anode catalyst layer with the main content of ion exchange resin is added between the second anode catalyst layer and the proton exchange membrane, and the surface roughness of the first anode catalyst layer is adjusted, so that an interface layer with an irregular surface is formed on the surface of the transition layer, the contact area between the first anode catalyst layer and the second anode catalyst layer can be increased, and the utilization rate of the catalyst in the second anode catalyst layer is further improved. More preferably, the roughness of the first anode catalytic layer ranges from Ra 0.8 μm to Ra6.3 μm.
As a preferable scheme of the invention, the first anode catalytic layer is composed of a platinum-based catalyst and a first ion exchange resin, wherein the content of the first ion exchange resin is 60 wt% to 90 wt%; the first ion exchange resin is a perfluorosulfonic acid resin.
Further preferably, the platinum-based catalyst in the first anode catalyst layer includes platinum black, a carbon-supported platinum catalyst, a platinum-based binary metal catalyst, a platinum-based multi-element metal catalyst, a platinum-based core-shell binary catalyst, or a platinum-based core-shell multi-element catalyst.
As a preferable scheme of the invention, the platinum loading capacity in the first anode catalyst layer is 0.01-0.05 mg/cm 2 。
In a preferred embodiment of the present invention, the second anode catalyst layer contains 2 to 20 wt% of the second ion exchange resin.
In a preferred embodiment of the present invention, the oxygen evolution catalyst of the second anode catalyst layer comprises one or more of iridium black, ruthenium black, iridium oxide, ruthenium oxide, platinum-iridium alloy, iridium-ruthenium oxide, and a supported catalyst containing the above materials, and the noble metal loading is 0.2 to 0.6mg/cm 2 。
In a preferred embodiment of the present invention, the proton exchange membrane is any one of a perfluorosulfonic acid resin membrane, a modified perfluorosulfonic acid resin membrane, and a reinforced perfluorosulfonic acid resin membrane; the modified perfluorinated sulfonic acid resin film comprises an inorganic substance doped modified perfluorinated sulfonic acid resin film, an inorganic acid-perfluorinated sulfonic acid resin composite film and an organic acid-perfluorinated sulfonic acid resin composite film, and the enhanced perfluorinated sulfonic acid film comprises a polytetrafluoroethylene enhanced perfluorinated sulfonic acid film, a polyimide enhanced perfluorinated sulfonic acid film and a polyether-ether-ketone enhanced perfluorinated sulfonic acid film.
Further preferably, the thickness of the proton exchange membrane is preferably not more than 100 μm. The inventor adds the first anode catalyst layer between the proton exchange membrane and the second anode catalyst layer, reduces the thickness of the proton exchange membrane by 50-100 μm compared with the thickness of the traditional proton exchange membrane, and not only can save materials, but also can reduce the cost of the membrane electrode, and can improve the proton conduction efficiency, thereby obviously improving the performance of the membrane electrode.
As a preferable scheme of the invention, the cathode catalyst layer consists of a third ion exchange resin and a platinum-based catalyst, wherein the resin content is 5-30 wt%.
A preparation method of a water electrolysis membrane electrode comprises the following steps:
s1: respectively preparing first anode catalyst slurry, second anode catalyst slurry and cathode catalyst slurry for later use;
s2: preparing a cathode catalyst layer on one side of a proton exchange membrane, and then sequentially preparing a first anode catalyst layer and a second anode catalyst layer on the other side of the proton exchange membrane to obtain a water electrolysis membrane electrode structure; or the like, or a combination thereof,
firstly, sequentially preparing a first anode catalyst layer and a second anode catalyst layer on one side of a proton exchange membrane; and preparing a cathode catalyst layer on the other side of the proton exchange membrane to obtain the water electrolysis membrane electrode structure.
Further preferably, the method further comprises a step S3, in which the water electrolysis membrane electrode structure in the step S2 is hot-pressed, and the water electrolysis membrane electrode based on the proton exchange membrane is obtained after pressure and heat are released.
As a preferred technical scheme of the invention, the hot pressing temperature is 80-160 ℃, the hot pressing pressure is 0.1-10 MPa, and the hot pressing time is 1-10 min.
A water electrolysis membrane electrode assembly comprises the water electrolysis membrane electrode, wherein an anode porous transmission layer is arranged on one side of a second anode catalyst layer of the water electrolysis membrane electrode, and a cathode gas diffusion layer is arranged on one side of a cathode catalyst layer of the water electrolysis membrane electrode.
The application of the water electrolysis membrane electrode in a water electrolysis cell comprises the following steps: and respectively placing the porous transmission layer (anode diffusion layer) and the anode gas diffusion layer on the outer layers of the second anode catalyst layer and the cathode catalyst layer of the prepared water electrolysis membrane electrode to form a membrane electrode assembly, and fixing the membrane electrode assembly in an electrolytic bath clamp for carrying out an electrolyzed water test.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the first anode catalyst layer is added between the second anode catalyst layer and the proton exchange membrane, the content of ion exchange resin in the first anode catalyst layer is up to 50 wt% -95 wt%, so that an electrode structure with pore distribution gradient (the porosity is gradually reduced in the direction from a flow field to a PEM) is formed on the anode side together with the second anode catalyst layer and the porous transmission layer, and the transmission of reactants and products is facilitated.
2. The surface of the first anode catalyst layer is of an irregular structure, so that the contact area between the first anode catalyst layer and the anode catalyst layer is increased, the utilization rate of the anode catalyst is improved, and the dosage of the anode catalyst is reduced.
3. The platinum-based catalyst in the first anode catalyst layer is beneficial to catalytic oxidation of hydrogen permeated from the cathode into protons, so that on one hand, reduction of catalytic activity caused by reduction of the anode oxygen evolution catalyst due to the existence of hydrogen can be avoided, and on the other hand, potential safety hazards caused by over-high concentration of hydrogen in oxygen can be avoided.
4. By applying the membrane electrode structure, the hydrogen concentration in the anode product is effectively reduced, the utilization rate of the oxygen evolution catalyst can be improved, and the noble metal loading capacity of the first anode catalyst layer is reduced to 0.2-0.6 mg/cm 2 。
Drawings
FIG. 1 is a schematic view of the structure of a water electrolysis membrane electrode according to the present invention; (wherein 101 denotes a proton exchange membrane, 102 denotes a first anode catalyst layer, 103 denotes a second anode catalyst layer, and 104 denotes a cathode catalyst layer).
FIG. 2 is a schematic view of the structure of a water electrolysis membrane electrode assembly according to the present invention; (wherein 201 denotes a proton exchange membrane, 202 denotes a first anode catalytic layer, 203 denotes a second anode catalytic layer, 204 denotes a cathode catalytic layer, 205 denotes an anode porous transport layer, and 206 denotes a cathode gas diffusion layer).
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The present embodiment provides a water electrolysis membrane electrode, wherein,
the proton exchange membrane adopts Nafion TM 212, having a thickness of 51 μm.
The first anode catalyst layer consists of a platinum carbon catalyst and first ion exchange resin, wherein the content of the first ion exchange resin is 90 wt%; the platinum loading in the first anode catalytic layer was 0.02mg/cm 2 。
The second anode catalytic layer consists of iridium oxide black and second ion exchange resin, wherein the content of the second ion exchange resin is 10 wt%; the iridium loading is 0.5mg/cm 2 ；
The cathode catalyst layer consists of a platinum-carbon catalyst and third ion exchange resin, wherein the content of the third ion exchange resin is 20 wt%; platinum loading was 0.3mg/cm 2 。
The embodiment provides a preparation method of a water electrolysis membrane electrode, which comprises the following steps: the method specifically comprises the following steps:
s1: respectively preparing first anode catalyst slurry, second anode catalyst slurry and cathode catalyst slurry for later use;
s2: the first anode catalyst slurry is coated on Nafion by means of ultrasonic spraying TM 212 deg.C drying, placing in a splint with surface roughness of Ra3.2 μm, pressing under 0.5MPa for 2min to form a first anode catalyst layer with irregular surface, wherein the platinum loading is 0.02mg/cm 2 . Then obtaining a first anode catalyst layer/proton exchange membrane structure;
s3: coating the second anode catalyst slurry on the surface of the irregular first anode catalyst layer formed in the step S1 by ultrasonic spraying, and drying at 80 DEG CForming a second anode catalytic layer after drying, wherein the iridium loading is 0.5mg/cm 2 . Then obtaining a second anode catalyst layer/first anode catalyst layer/proton exchange membrane structure;
s4: coating the cathode catalyst slurry on the other side of the proton exchange membrane by ultrasonic spraying, and drying at 80 ℃ to form a cathode catalyst layer, wherein the platinum loading is 0.3mg/cm 2 . Obtaining a second anode catalyst layer/first anode catalyst layer/proton exchange membrane/cathode catalyst layer structure; as shown in fig. 1;
s5: and (3) hot-pressing the prepared structure of the second anode catalyst layer/the first anode catalyst layer/the proton exchange membrane/the cathode catalyst layer for 5min at 140 ℃ and under 1MPa, and obtaining the water electrolysis membrane electrode based on the proton exchange membrane after releasing pressure and heat.
The titanium felt, the water electrolysis membrane electrode obtained in example 1 and the gas diffusion layer (the carbon paper with the microporous layer) are sequentially stacked in a test fixture (with a sealing gasket) of a single serpentine flow field as shown in fig. 2, and a force of 5N · m is gradually applied to lock the fixture, so that the single cell 1 is obtained. And (3) performing performance test by using a direct current power supply, wherein the water temperature and the battery temperature are both kept at 80 ℃, and the cathode back pressure is 1 MPa.
Example 2
This example provides two types of water electrolyte membrane electrodes, which differ from example 1 only in that: the proton exchange membranes of the water electrolysis membrane electrode are respectively Nafion TM 115 and Nafion TM 117, wherein the proton exchange membrane has a thickness of 127 μm and 183 μm, respectively;
the assembly and testing of the cells were the same as in example 1; respectively designated as cell 2-1 and cell 2-2.
Example 3
This example provides two types of water electrolyte membrane electrodes, which differ from example 1 only in that: in the water electrolysis membrane electrode, the content of the first ion exchange resin is 70 wt% and 50 wt%, respectively.
The assembly and testing of the cells were the same as in example 1; respectively designated as cell 3-1 and cell 3-2.
Example 4
This example provides two types of water electrolyte membrane electrodes, which differ from example 1 only in that: in the water electrolysis membrane electrode, the second anode catalyst layer uses a ruthenium oxide catalyst and an iridium ruthenium alloy catalyst, respectively.
The assembly and testing of the cells were the same as in example 1; respectively designated as cell 4-1 and cell 4-2.
Example 5
This example provides two kinds of water electrolyte membrane electrodes, which are different from the preparation method of example 1 only in step S2:
s2: d2020 ion exchange resin solution is applied to Nafion by ultrasonic spraying TM And drying the surface of the 212 proton exchange membrane at 80 ℃, respectively placing the proton exchange membrane in splints with the surface roughness of Ra1.6 mu m and Ra6.3 mu m, and pressing for 2min under the condition of 0.5MPa to form a resin transition layer with irregular surface. At this point a resin transition layer/proton exchange membrane structure is obtained.
The assembly and testing of the cells were the same as in example 1; respectively designated as cell 5-1 and cell 5-2.
Comparative example 1
The comparative example is a water electrolysis membrane electrode of a conventional anode catalyst layer/proton exchange membrane/cathode catalyst layer structure, in which,
the proton exchange membrane adopts Nafion TM 115 film, 127 μm thick.
The anode catalyst layer consists of iridium oxide black and second ion exchange resin, wherein the content of the second ion exchange resin is 10 wt%; the iridium loading is 1.5mg/cm 2 ；
The cathode catalyst layer consists of a platinum-carbon catalyst and third ion exchange resin, wherein the content of the third ion exchange resin is 20 wt%; platinum loading was 0.3mg/cm 2 。
The preparation method specifically comprises the following steps:
s1: respectively preparing anode catalyst slurry and cathode catalyst slurry for later use;
s2: the anode catalyst slurry is coated on Nafion by an ultrasonic spraying mode TM 212 proton exchange membrane surface, drying at 80 deg.C, wherein the platinum loading is 0.02mg/cm 2 . At this time, anode catalysis is obtainedA layer/proton exchange membrane structure;
s3: coating the cathode catalyst slurry on the other side of the proton exchange membrane by ultrasonic spraying, and drying at 80 ℃ to form a cathode catalyst layer, wherein the platinum loading is 0.3mg/cm 2 . Obtaining an anode catalyst layer/proton exchange membrane/cathode catalyst layer structure;
s4: and (3) hot-pressing the prepared anode catalyst layer/proton exchange membrane/cathode catalyst layer structure for 5min at 140 ℃ under the condition of 1MPa, and obtaining the water electrolysis membrane electrode based on the proton exchange membrane after releasing pressure and heat.
The cell assembly and testing was the same as example 1 and was identified as cell D1.
Comparative example 2
The comparative example is a water electrolysis membrane electrode of an anode catalyst layer/resin transition layer/proton exchange membrane/cathode catalyst layer structure, wherein,
the proton exchange membrane adopts Nafion TM 212 film with a thickness of 51 μm;
the resin transition layer is pure ion exchange resin with the thickness of 10 μm;
the anode catalyst layer consists of iridium oxide black and second ion exchange resin, wherein the content of the second ion exchange resin is 10 wt%; the iridium loading is 0.5mg/cm 2 ；
The cathode catalyst layer consists of a platinum carbon catalyst and third ion exchange resin, wherein the content of the third ion exchange resin is 20 wt%; platinum loading was 0.3mg/cm 2 。
The preparation method specifically comprises the following steps:
s1: respectively preparing anode catalyst slurry and cathode catalyst slurry for later use;
s2: d2020 ion exchange resin solution is applied to Nafion by ultrasonic spraying TM Drying the surface of the 212 proton exchange membrane at 80 ℃ to obtain a resin transition layer/proton exchange membrane structure;
s3: coating the anode catalyst slurry on the surface of the resin transition layer formed in the step S1 in an ultrasonic spraying manner, and drying at 80 ℃ to obtain an anode catalyst layer/resin transition layer/proton exchange membrane structure;
s4: coating the cathode catalyst slurry on the other side of the proton exchange membrane by ultrasonic spraying, and drying at 80 ℃ to form a cathode catalyst layer, wherein the platinum loading is 0.3mg/cm 2 . Obtaining an anode catalyst layer/resin transition layer/proton exchange membrane/cathode catalyst layer structure;
s5: and (3) hot-pressing the prepared anode catalyst layer/resin transition layer/proton exchange membrane/cathode catalyst layer structure for 5min at 140 ℃ and 1MPa, and obtaining the water electrolysis membrane electrode based on the proton exchange membrane after releasing pressure and heat.
The assembly and testing of the cells were the same as in example 1; denoted as cell D2.
Comparative example 3
The present comparative example provides a water electrolyte membrane electrode, which is different from the preparation method of comparative example 2 only in step S2:
s2: d2020 ion exchange resin solution is applied to Nafion by ultrasonic spraying TM And drying the surface of the 212 proton exchange membrane at 80 ℃, putting the proton exchange membrane into a splint with the surface roughness of Ra3.2, and pressing for 2min under the condition of 0.5MPa to form a resin transition layer with an irregular surface. At this point a resin transition layer/proton exchange membrane structure is obtained.
The assembly and testing of the cells were the same as in example 1; denoted as cell D3.
Comparative example 4
The present comparative example provides a water electrolysis membrane electrode, which is different from the preparation method of example 1 only in step S2:
s2: the first anode catalyst slurry is coated on Nafion by means of ultrasonic spraying TM 212 deg.C drying to form a first anode catalyst layer with platinum loading of 0.02mg/cm 2 . At the moment, a first anode catalyst layer/proton exchange membrane structure is obtained;
assembly and testing of cells as in example 1; and is referred to as cell D4.
Table 1 shows structural information of the water electrolysis membrane electrodes prepared in examples 1 to 5 and comparative examples 1 to 4
Table 1 shows composition information of the water electrolysis membrane electrodes prepared in examples 1 to 5 and comparative examples 1 to 4. Wherein example 1 employs Nafion with a thickness of 51 μm TM 115 film, the platinum loading and the resin content in the catalytic transition layer are respectively 0.02mg/cm 2 And 90 wt%, the loading amount of iridium ruthenium in the anode catalytic layer is 0.5mg/cm 2 . Example 2, based on example 1, only varied the thickness of the proton exchange membrane, using Nafion with a thickness of 127 μm and 183 μm, respectively TM 115 and Nafion TM 117 a film; example 3 only the second ion exchange resin content was changed to 70 wt% and 50 wt%; example 4 only changing the oxygen evolution catalyst species to ruthenium oxide and iridium ruthenium alloy, respectively; example 5 only the roughness of the first anode catalytic layer was changed to ra1.6 μm and ra6.3 μm, respectively. Comparative example 1 did not contain the first anode catalytic layer, compared to example 1; the first anode catalytic layer of comparative example 2 had a resin content of 100 wt%, and the first anode catalytic layer was not provided with surface roughness; the first anode catalytic layer resin content in comparative example 3 was 100 wt%; comparative example 4 the first anode catalytic layer was not provided with surface roughness.
The above examples and comparative examples were subjected to membrane electrode performance tests. The results are shown in table 2 below:
TABLE 2 Performance data of Water electrolyte Membrane electrodes prepared in examples 1 to 5 and comparative examples 1 to 4
Table 2 shows performance data of the membrane electrodes prepared in examples 1 to 5 and comparative examples 1 to 4. Except for example 4, the other water electrolysis membrane electrodes adopt the same catalyst, and the voltage (@10 mA/cm) of the small current region 2 ) Close to each other, all lie in the 1.48V regionAnd (4) approaching. Example 4-1 the lowest voltage @10mA/cm due to the use of the more active ruthenium oxide catalyst 2 Example 4-2 has the highest voltage @10mA/cm due to the use of the less active iridium-ruthenium alloy catalyst 2 . As can be seen from a comparison between example 1 and example 2, reducing the thickness of the proton exchange membrane contributes to improving the performance of the water electrolysis membrane electrode. As can be seen from the comparison between example 1 and comparative example 1, the addition of the first anode catalyst layer with irregular surface between the proton exchange membrane and the anode catalyst layer can significantly reduce the amount of the oxygen evolution catalyst and improve the performance of the water electrolysis membrane electrode. As can be seen from the comparison between example 1 and comparative example 4, the roughness is arranged on the surface of the first anode catalyst layer, so that the contact area with the second anode catalyst layer is increased, on one hand, the contact resistance between the layers is reduced, and on the other hand, the utilization rate of the oxygen evolution catalyst is also improved.
TABLE 3 hydrogen concentration (volume percentage) on oxygen side of water electrolyte membrane electrodes prepared in examples 1 to 5 and comparative examples 1 to 4 at different current densities
| 0.5A/cm 2 | 1A/cm 2 | 2A/cm 2 | |
| Example 1 | - | 0.02Vol％ | 0.06Vol％ |
| Example 2-1 | - | - | 0.02Vol％ |
| Examples 2 to 2 | - | - | - |
| Example 3-1 | - | - | 0.03Vol％ |
| Examples 3 to 2 | - | - | - |
| Example 4-1 | - | 0.01Vol％ | 0.05Vol％ |
| Example 4 to 2 | - | 0.02Vol％ | 0.05Vol％ |
| Example 5-1 | - | - | 0.05Vol％ |
| Examples 5 and 2 | - | 0.01Vol％ | 0.04Vol％ |
| Comparative example 1 | 0.62Vol％ | 0.87Vol％ | 0.92Vol％ |
| Comparative example 2 | 1.27Vol％ | 1.44Vol％ | 1.57Vol％ |
| Comparative example 3 | 1.35Vol％ | 1.39Vol％ | 1.62Vol％ |
| Comparative example 4 | - | - | 0.04Vol％ |
Table 3 shows performance data of the membrane electrodes prepared in examples 1 to 5 and comparative examples 1 to 4. For all membrane electrodes, the hydrogen concentration on the oxygen side increased with increasing current density. Comparison of examples 1 to 5 with comparative examples 1 to 3 shows that the first anode catalyst layer composed of a platinum-carbon catalyst and a first ion exchange resin is effective in eliminating hydrogen gas on the anode side. By combining the consideration of the performance and the cost of the membrane electrode, the purposes of improving the performance of the membrane electrode, reducing the consumption of the oxygen evolution catalyst and eliminating the hydrogen content on the anode side can be simultaneously achieved by adopting a thinner proton exchange membrane and additionally arranging the first anode catalyst layer with an irregular surface.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A water electrolysis membrane electrode is characterized in that a first anode catalyst layer and a second anode catalyst layer are sequentially arranged on one side of a proton exchange membrane, and a cathode catalyst layer is arranged on the other side of the proton exchange membrane;
the first anode catalytic layer comprises a platinum-based catalyst and a first ion exchange resin; the content of the first ion exchange resin is 50-95 wt%;
the second anode catalyst layer comprises an oxygen evolution catalyst and second ion exchange resin, and the content of the second ion exchange resin is not more than 30 wt%.
2. The water electrolysis membrane electrode assembly according to claim 1, wherein the thickness of the first anode catalytic layer is no more than 20 μm, preferably the thickness of the first anode catalytic layer is no more than 15 μm.
3. The water electrolysis membrane electrode assembly according to claim 1, wherein the surface roughness of the first anode catalytic layer ranges from Ra 0.1 μm to Ra12.5 μm.
4. The water electrolysis membrane electrode assembly according to claim 1, wherein the platinum-based catalyst in the first anode catalyst layer comprises any one or a combination of several of platinum black, carbon-supported platinum catalyst, platinum-based binary metal catalyst, platinum-based multi-element metal catalyst, platinum-based core-shell binary catalyst or platinum-based core-shell multi-element catalyst.
5. The water electrolysis membrane electrode assembly according to claim 4, wherein the platinum loading in the first anode catalyst layer is 0.01-0.1 mg/cm 2 。
6. The water electrolysis membrane electrode assembly according to claim 1, wherein in the second anode catalytic layer, the oxygen evolution catalyst comprises any one or combination of iridium black, ruthenium black, iridium oxide, ruthenium oxide, platinum iridium alloy, iridium ruthenium oxide, and supported catalysts containing the above materials;
the noble metal loading amount in the second anode catalyst layer is 0.2-0.6 mg/cm 2 。
7. The water electrolysis membrane electrode assembly according to claim 1, wherein the proton exchange membrane is any one of a perfluorosulfonic acid resin membrane, a modified perfluorosulfonic acid resin membrane and a reinforced perfluorosulfonic acid resin membrane, and the thickness of the proton exchange membrane is not more than 150 μm; preferably, the thickness of the proton exchange membrane is not more than 100 μm.
8. The preparation method of the water electrolysis membrane electrode according to any one of claims 1 to 7, characterized by comprising the following steps:
s1: respectively preparing first anode catalyst slurry, second anode catalyst slurry and cathode catalyst slurry for later use;
s2: preparing a cathode catalyst layer on one side of a proton exchange membrane, and sequentially preparing a first anode catalyst layer and a second anode catalyst layer on the other side of the proton exchange membrane to obtain a water electrolysis membrane electrode; or the like, or, alternatively,
firstly, sequentially preparing a first anode catalyst layer and a second anode catalyst layer on one side of a proton exchange membrane; and preparing a cathode catalyst layer on the other side of the proton exchange membrane to obtain the water electrolysis membrane electrode.
9. A water electrolysis membrane electrode assembly comprising the water electrolysis membrane electrode according to any one of claims 1 to 7, wherein an anode porous transmission layer is provided on the second anode catalyst layer side of the water electrolysis membrane electrode, and a cathode gas diffusion layer is provided on the cathode catalyst layer side of the water electrolysis membrane electrode.
10. Use of a water electrolysis membrane electrode assembly as claimed in claim 9 in a water electrolyser.
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