CN117594811A - A kind of thermal pressure-assisted reinforced fuel cell membrane electrode and its preparation method - Google Patents
A kind of thermal pressure-assisted reinforced fuel cell membrane electrode and its preparation method Download PDFInfo
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Abstract
Description
技术领域Technical field
本发明属于质子交换膜燃料电池技术领域,具体涉及一种热压辅助增强燃料电池膜电极及其制备方法。The invention belongs to the technical field of proton exchange membrane fuel cells, and specifically relates to a thermal pressure-assisted enhanced fuel cell membrane electrode and a preparation method thereof.
背景技术Background technique
质子交换膜燃料电池(PEMFC)是一种先进的能源转换技术,它可以直接将化学能转变为电能,而无需通过传统的燃烧过程。这种电池具有高效能量转换、零排放特性,并且可以在相对较低的温度下迅速启动,因此在多个领域具有广泛的应用前景。在质子交换膜燃料电池中,膜电极组件(MEA)扮演着关键的角色,它直接影响着燃料电池的性能表现。MEA包括质子交换膜、阳极和阴极催化层,以及分别位于阳极和阴极上的气体扩散层。这些组成部分共同协作,影响着膜电极的整体功能。Proton exchange membrane fuel cell (PEMFC) is an advanced energy conversion technology that directly converts chemical energy into electrical energy without going through a traditional combustion process. This kind of battery has high-efficiency energy conversion, zero emission characteristics, and can start quickly at relatively low temperatures, so it has broad application prospects in many fields. In proton exchange membrane fuel cells, the membrane electrode assembly (MEA) plays a key role, which directly affects the performance of the fuel cell. The MEA includes a proton exchange membrane, anode and cathode catalytic layers, and gas diffusion layers located on the anode and cathode respectively. These components work together to influence the overall function of the membrane electrode.
膜电极中的催化层一般由催化剂和树脂组成,其中催化剂起到了主要的电催化作用,促使氢气(在阳极)和氧气(在阴极)的电化学反应。铂碳催化剂是常见的催化剂类型,其中碳载体在整个反应过程中起到支持和导电的作用。碳载体可以采用导电炭黑、碳纤维、碳纳米管等材料。这些碳载体具有良好的电导性质,有助于将电子传递到催化剂上,从而促使气体分子的电化学反应。The catalytic layer in a membrane electrode is generally composed of a catalyst and resin. The catalyst plays the main electrocatalytic role, promoting the electrochemical reaction of hydrogen (at the anode) and oxygen (at the cathode). Platinum carbon catalyst is a common catalyst type in which the carbon support plays a supporting and conductive role throughout the reaction process. The carbon carrier can use materials such as conductive carbon black, carbon fiber, and carbon nanotubes. These carbon supports have good electrical conductivity properties and help transfer electrons to the catalyst, thereby promoting the electrochemical reaction of gas molecules.
碳纳米管相对于导电炭黑,在传导电子方面展现出明显的优势,此外,碳纳米管的化学稳定性也使其能够在长时间内保持卓越的电导性能。上述优势使碳纳米管负载的燃料电池催化剂具有广泛的应用前景。专利文献CN111244480B公开了一种碳载钯基合金燃料电池膜电极及其制备方法,采用负载钯基合金的多壁碳纳米管或单壁碳纳米管载体作为第一催化层,负载铂催化剂的多壁碳纳米管或单壁碳纳米管载体作为第二催化层,分别将其喷涂于质子交换膜的两个表面制备质子交换膜燃料电池膜电极。然而碳纳米管呈现管状结构并具有较大的比表面积,因此,在催化剂负载过程中,通常会形成相对松散的排列,从而导致堆积密度较低,此时层与层之间的碳纳米管无法形成有效的导电通路,从而无法使碳纳米管负载的铂碳催化剂性能无法得到有效的发挥。Compared with conductive carbon black, carbon nanotubes show obvious advantages in conducting electrons. In addition, the chemical stability of carbon nanotubes also enables them to maintain excellent conductivity properties over a long period of time. The above advantages make carbon nanotube-supported fuel cell catalysts have broad application prospects. Patent document CN111244480B discloses a carbon-supported palladium-based alloy fuel cell membrane electrode and its preparation method. It uses multi-walled carbon nanotubes or single-walled carbon nanotube carriers supporting palladium-based alloys as the first catalytic layer, and multi-walled carbon nanotubes supporting platinum catalysts. The wall carbon nanotube or single-wall carbon nanotube carrier is used as the second catalytic layer, which is sprayed on both surfaces of the proton exchange membrane to prepare a proton exchange membrane fuel cell membrane electrode. However, carbon nanotubes exhibit a tubular structure and have a large specific surface area. Therefore, during the catalyst loading process, they usually form a relatively loose arrangement, resulting in a low packing density. At this time, the carbon nanotubes between layers cannot An effective conductive path is formed, so that the performance of the carbon nanotube-supported platinum carbon catalyst cannot be effectively exerted.
发明内容Contents of the invention
本发明的目的在于提供一种热压辅助增强燃料电池膜电极及其制备方法,以解决碳纳米管排列松散、堆积密度较低,以及层与层之间无法形成有效导电通路,导致膜电极电化学性能较差的问题The purpose of the present invention is to provide a hot-pressure-assisted enhanced fuel cell membrane electrode and a preparation method thereof to solve the problem of loose arrangement of carbon nanotubes, low packing density, and inability to form effective conductive paths between layers, resulting in membrane electrode electrical conductivity. The problem of poor chemical performance
本发明的目的可以通过以下技术方案实现:The object of the present invention can be achieved through the following technical solutions:
第一方面,一种热压辅助增强燃料电池膜电极的制备方法,包括如下步骤:In the first aspect, a method for preparing a thermal pressure-assisted reinforced fuel cell membrane electrode includes the following steps:
S1.制备催化层浆料:碳纳米管负载的铂催化剂(Pt/CNTs)中加入水和异丙醇,在30W的超声功率中搅拌,再加入全氟磺酸树脂溶液,常温条件下(25-30℃)混合均匀,得到均匀分散的墨水状催化剂浆料;S1. Preparation of catalytic layer slurry: add water and isopropyl alcohol to the carbon nanotube-supported platinum catalyst (Pt/CNTs), stir at 30W ultrasonic power, then add the perfluorosulfonic acid resin solution, and mix at room temperature (25 -30°C) and mix evenly to obtain a uniformly dispersed ink-like catalyst slurry;
S2.喷涂:质子交换膜置于加热板上,催化层浆料依次喷涂于质子交换膜的两侧,得到同时具有阳极催化层和阴极催化层的催化膜;S2. Spraying: The proton exchange membrane is placed on the heating plate, and the catalytic layer slurry is sprayed on both sides of the proton exchange membrane in sequence to obtain a catalytic membrane with both an anode catalytic layer and a cathode catalytic layer;
S3.一次热压:先将PTFE(聚四氟乙烯)薄膜分别贴在催化剂膜两侧得到组装体a,再将多孔PEFT薄膜分别贴在组装体a两侧得到组装体b,最后将薄铜片分别装配在组装体b两侧,对其进行支撑和保护得到组装体c;对组装体c进行一次热压,热压完成后分别剥离两侧的薄铜片、多孔PTFE薄膜和PTFE薄膜,得到半成品热压辅助增强的催化膜;S3. One-time hot pressing: first stick PTFE (polytetrafluoroethylene) films on both sides of the catalyst membrane to obtain assembly a, then stick porous PEFT films on both sides of assembly a to get assembly b, and finally put thin copper The sheets are respectively assembled on both sides of the assembly b to support and protect them to obtain the assembly c; the assembly c is hot-pressed once, and after the hot-pressing is completed, the thin copper sheets, porous PTFE films and PTFE films on both sides are peeled off. A semi-finished hot-pressing-assisted reinforced catalytic membrane is obtained;
S4.二次热压:将气体扩散层置于半成品热压辅助增强的催化膜的两侧,进行二次热压,得到燃料电池膜电极。S4. Secondary hot pressing: Place the gas diffusion layer on both sides of the semi-finished hot-pressing-assisted and enhanced catalytic membrane, and perform a second hot-pressing to obtain the fuel cell membrane electrode.
进一步地,所述S1中搅拌速率为500rpm,搅拌时间为30min。Further, the stirring rate in S1 is 500 rpm, and the stirring time is 30 min.
进一步地,所述S1中采用搅拌的方式进行混合,所述搅拌的速率为10000rpm,搅拌的时间为30min。Further, in S1, mixing is performed by stirring, the stirring rate is 10,000 rpm, and the stirring time is 30 minutes.
进一步地,所述S1中碳纳米管负载的铂催化剂铂的质量百分比为10%。Further, the mass percentage of platinum catalyst supported on carbon nanotubes in S1 is 10%.
进一步地,所述S1中全氟磺酸树脂溶液的质量百分比为20wt%。Further, the mass percentage of the perfluorosulfonic acid resin solution in S1 is 20wt%.
进一步地,所述S1中催化剂浆料的溶剂为水和异丙醇,所述水和异丙醇的体积比为0.5-1.5:8.5-9.5。Further, the solvents of the catalyst slurry in S1 are water and isopropyl alcohol, and the volume ratio of water and isopropyl alcohol is 0.5-1.5:8.5-9.5.
进一步地,所述S1中催化剂浆料的溶质为Pt/CNTs和全氟磺酸树脂,所述溶质的质量百分比为1-2%。Further, the solute of the catalyst slurry in S1 is Pt/CNTs and perfluorosulfonic acid resin, and the mass percentage of the solute is 1-2%.
进一步地,所述溶质中全氟磺酸树脂和Pt/CNTs中碳纳米管的质量比为0.7-0.8:1。Further, the mass ratio of perfluorosulfonic acid resin and carbon nanotubes in Pt/CNTs in the solute is 0.7-0.8:1.
进一步地,所述S2中催化膜两侧阳极催化层和阴极催化层的总铂载量为0.5mg/cm2。Further, the total platinum loading of the anode catalytic layer and the cathode catalytic layer on both sides of the catalytic membrane in S2 is 0.5 mg/cm 2 .
进一步地,所述阳极催化层和阴极催化层铂载量之比为1:4,也即催化膜两侧阳极催化层和阴极催化层的铂载量分别为0.1mg/cm2,0.4mg/cm2。Further, the ratio of the platinum loading of the anode catalytic layer and the cathode catalytic layer is 1:4, that is, the platinum loading of the anode catalytic layer and the cathode catalytic layer on both sides of the catalytic membrane are 0.1mg/cm 2 and 0.4mg/ cm 2 .
进一步地,所述S2中质子交换膜的厚度为12μm。Further, the thickness of the proton exchange membrane in S2 is 12 μm.
进一步地,所述S2中加热板的温度为90℃。Further, the temperature of the heating plate in S2 is 90°C.
进一步地,所述S2中催化层浆料喷涂于质子交换膜的一侧后,置于40℃下放置1h,挥发多余溶剂,得到单侧催化层催化膜后,再将催化层浆料喷涂于质子交换膜的另一侧,同样置于40℃下放置1h,得到同时具有阳极催化层和阴极催化层的催化膜。Further, after the catalytic layer slurry in S2 is sprayed on one side of the proton exchange membrane, it is placed at 40°C for 1 hour to evaporate excess solvent to obtain a single-sided catalytic layer catalytic membrane, and then the catalytic layer slurry is sprayed on The other side of the proton exchange membrane was also placed at 40°C for 1 hour to obtain a catalytic membrane with both an anode catalytic layer and a cathode catalytic layer.
进一步地,所述S3中PTFE薄膜厚度为0.4-0.8mm,铜片厚度为1mm。Further, the thickness of the PTFE film in the S3 is 0.4-0.8mm, and the thickness of the copper sheet is 1mm.
进一步地,所述S3中多孔PTFE薄膜的孔隙率为20-40%。Further, the porosity of the porous PTFE film in S3 is 20-40%.
进一步地,所述S3中一次热压条件为在100-120℃,0.4-0.6MPa压力下热压80-120s。Further, the hot pressing conditions in S3 are hot pressing at 100-120°C and 0.4-0.6MPa pressure for 80-120 seconds.
进一步地,所述S4中气体扩散层的厚度为220μm。Further, the thickness of the gas diffusion layer in S4 is 220 μm.
进一步地,所述S4中二次热压条件在140℃,3MPa压力下热压120s。Furthermore, the second hot pressing conditions in S4 are hot pressing at 140°C and 3MPa pressure for 120 seconds.
第二方面,本发明提供一种热压辅助增强燃料电池膜电极,所述热压辅助增强燃料电池膜电极由第一方面所述的热压辅助增强燃料电池膜电极的制备方法制备而成:In a second aspect, the present invention provides a hot-pressure-assisted reinforced fuel cell membrane electrode, which is prepared by the preparation method of a hot-pressure-assisted reinforced fuel cell membrane electrode described in the first aspect:
所述热压辅助增强燃料电池膜电极包括质子交换膜,质子交换膜的一侧设置有阴极催化层,质子交换膜的另一侧设置有阳极催化层,阴极催化层和阳极催化层的外侧均设置有气体扩散层;所述阴极催化层和阳极催化层中包括碳纳米管负载的铂催化剂和全氟磺酸树脂。The thermal pressure-assisted enhanced fuel cell membrane electrode includes a proton exchange membrane. One side of the proton exchange membrane is provided with a cathode catalytic layer, and the other side of the proton exchange membrane is provided with an anode catalytic layer. The outer sides of the cathode catalytic layer and the anode catalytic layer are both A gas diffusion layer is provided; the cathode catalytic layer and the anode catalytic layer include a carbon nanotube-supported platinum catalyst and a perfluorosulfonic acid resin.
本发明的有益效果:Beneficial effects of the present invention:
本发明提供了一种热压辅助增强燃料电池膜电极及其制备方法,通过喷涂工艺将碳纳米管负载的铂碳催化剂及全氟磺酸树脂负载于质子交换膜上得到疏松的催化层,再通过热压的方法使疏松的碳纳米管的层与层之间形成更加致密的导电通路,有效提高催化层中催化剂的堆积密度,从而提高膜电极的电化学性能。The invention provides a hot-pressing-assisted reinforced fuel cell membrane electrode and a preparation method thereof. The carbon nanotube-supported platinum carbon catalyst and perfluorosulfonic acid resin are loaded on a proton exchange membrane through a spraying process to obtain a loose catalytic layer. Through the hot pressing method, denser conductive paths are formed between the layers of loose carbon nanotubes, which effectively increases the packing density of the catalyst in the catalytic layer, thereby improving the electrochemical performance of the membrane electrode.
附图说明Description of drawings
下面结合附图对本发明作进一步的说明。The present invention will be further described below in conjunction with the accompanying drawings.
图1是本发明热压辅助增强燃料电池膜电极的结构示意图;Figure 1 is a schematic structural diagram of a membrane electrode of a fuel cell assisted by hot pressing in accordance with the present invention;
图2是本发明实施例5中实施例2和对比例1的极化曲线示意图;Figure 2 is a schematic diagram of the polarization curves of Example 2 and Comparative Example 1 in Example 5 of the present invention;
图3是本发明实施例5中实施例2和对比例1的扫描电镜表征图;Figure 3 is a scanning electron microscope characterization diagram of Example 2 and Comparative Example 1 in Example 5 of the present invention;
图中:1、质子交换膜;2、阴极催化层;3、阳极催化层;4、气体扩散层。In the picture: 1. Proton exchange membrane; 2. Cathode catalytic layer; 3. Anode catalytic layer; 4. Gas diffusion layer.
具体实施方式Detailed ways
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.
实施例1Example 1
请参阅图1所示,一种热压辅助增强燃料电池膜电极,所述热压辅助增强燃料电池膜电极包括质子交换膜1,质子交换膜1的一侧设置有阴极催化层2,质子交换膜1的另一侧设置有阳极催化层3,阴极催化层2和阳极催化层3的外侧均设置有气体扩散层4。Please refer to Figure 1, a thermo-pressure-assisted enhanced fuel cell membrane electrode. The thermo-pressed-assisted enhanced fuel cell membrane electrode includes a proton exchange membrane 1. A cathode catalytic layer 2 is provided on one side of the proton exchange membrane 1. The proton exchange membrane electrode An anode catalytic layer 3 is provided on the other side of the membrane 1 , and a gas diffusion layer 4 is provided outside both the cathode catalytic layer 2 and the anode catalytic layer 3 .
实施例2Example 2
一种热压辅助增强燃料电池膜电极的制备方法,包括如下步骤:A method for preparing a thermal pressure-assisted reinforced fuel cell membrane electrode, including the following steps:
S1.制备催化层浆料:0.5g Pt/CNTs(铂的质量百分比为10%)中加入5.25mL蒸馏水和29.75mL异丙醇,在30W超声波清洗器中以500rpm速度搅拌30min,再加入1.0g全氟磺酸树脂溶液(质量百分比为20wt%),常温条件下以10000rpm搅拌30min,得到均匀分散的墨水状催化剂浆料;催化剂浆料的溶剂为水和异丙醇,水和异丙醇的体积比为1.5:8.5;溶质为Pt/CNTs和全氟磺酸树脂,溶质的质量百分比为2%,全氟磺酸树脂和Pt/CNTs中碳纳米管的质量比为0.8:1。S1. Prepare the catalytic layer slurry: add 5.25mL distilled water and 29.75mL isopropyl alcohol to 0.5g Pt/CNTs (the mass percentage of platinum is 10%), stir in a 30W ultrasonic cleaner at 500rpm for 30min, and then add 1.0g Perfluorosulfonic acid resin solution (mass percentage is 20wt%), stir at 10000rpm for 30 minutes at room temperature to obtain a uniformly dispersed ink-like catalyst slurry; the solvent of the catalyst slurry is water and isopropyl alcohol, and the solvent of water and isopropyl alcohol is The volume ratio is 1.5:8.5; the solute is Pt/CNTs and perfluorosulfonic acid resin, the mass percentage of the solute is 2%, and the mass ratio of carbon nanotubes in perfluorosulfonic acid resin and Pt/CNTs is 0.8:1.
S2.喷涂:将12μm厚度的质子交换膜置于90℃的加热板上,催化层浆料倒入喷枪中喷涂于质子交换膜的一侧后,置于40℃下放置1h,挥发多余溶剂,得到单侧催化层催化膜后,再将催化层浆料喷涂于质子交换膜的另一侧,同样置于40℃下放置1h,得到同时具有阳极催化层和阴极催化层的催化膜;催化膜两侧阳极催化层和阴极催化层的总铂载量为0.5mg/cm2,阳极催化层和阴极催化层的铂载量之比为1:4。S2. Spraying: Place a proton exchange membrane with a thickness of 12 μm on a heating plate at 90°C. Pour the catalytic layer slurry into a spray gun and spray it on one side of the proton exchange membrane. Place it at 40°C for 1 hour to evaporate excess solvent. After obtaining the single-sided catalytic layer catalytic membrane, spray the catalytic layer slurry on the other side of the proton exchange membrane, and place it at 40°C for 1 hour to obtain a catalytic membrane with both an anode catalytic layer and a cathode catalytic layer; catalytic membrane The total platinum loading of the anode catalytic layer and the cathode catalytic layer on both sides is 0.5 mg/cm 2 , and the ratio of the platinum loading of the anode catalytic layer and the cathode catalytic layer is 1:4.
S3.一次热压:先将厚度为0.8mm的PTFE薄膜分别贴在催化剂膜两侧得到组装体a,再将孔隙率为40%的多孔PEFT薄膜分别贴在组装体a两侧得到组装体b,最后将厚度为1mm薄铜片分别装配在组装体b两侧,得到组装体c;组装体c在120℃,0.6MPa压力下进行一次热压,热压时间为120s;热压完成后分别并依次剥离两侧的薄铜片、多孔PTFE薄膜和PTFE薄膜,得到半成品热压辅助增强的催化膜;S3. One-time hot pressing: First, attach PTFE films with a thickness of 0.8mm to both sides of the catalyst membrane to obtain assembly a, and then attach porous PEFT films with a porosity of 40% to both sides of assembly a to obtain assembly b. , finally, 1mm thick copper sheets are assembled on both sides of assembly b to obtain assembly c; assembly c is hot-pressed once at 120°C and 0.6MPa pressure, and the hot-pressing time is 120s; after the hot-pressing is completed, respectively And peel off the thin copper sheets, porous PTFE film and PTFE film on both sides in sequence to obtain a semi-finished hot-pressing-assisted reinforced catalytic membrane;
S4.二次热压:将厚度为220μm的气体扩散层置于半成品热压辅助增强的催化膜的两侧,装入热压机的模具中,在140℃和3MPa压力下进行二次热压,热压时间为120s,得到燃料电池膜电极。S4. Secondary hot pressing: Place the gas diffusion layer with a thickness of 220 μm on both sides of the semi-finished hot-pressed auxiliary reinforced catalytic membrane, put it into the mold of the hot press, and perform secondary hot pressing at 140°C and 3MPa pressure. , the hot pressing time is 120s, and the fuel cell membrane electrode is obtained.
实施例3Example 3
一种热压辅助增强燃料电池膜电极的制备方法,包括如下步骤:A method for preparing a thermal pressure-assisted reinforced fuel cell membrane electrode, including the following steps:
S1.制备催化层浆料:0.5g Pt/CNTs(铂的质量百分比为10%)中加入3.375mL蒸馏水和64.125mL异丙醇,在30W超声波清洗器中以500rpm速度搅拌30min,再加入0.875g全氟磺酸树脂溶液(质量百分比为20wt%),常温条件下以10000rpm搅拌30min,得到均匀分散的墨水状催化剂浆料;催化剂浆料的溶剂为水和异丙醇,水和异丙醇的体积比为0.5:9.5;溶质为Pt/CNTs和全氟磺酸树脂,溶质的质量百分比为1%,全氟磺酸树脂和Pt/CNTs中碳纳米管的质量比为0.7:1。S1. Prepare the catalytic layer slurry: add 3.375mL distilled water and 64.125mL isopropyl alcohol to 0.5g Pt/CNTs (the mass percentage of platinum is 10%), stir in a 30W ultrasonic cleaner at 500rpm for 30min, and then add 0.875g Perfluorosulfonic acid resin solution (mass percentage is 20wt%), stir at 10000rpm for 30 minutes at room temperature to obtain a uniformly dispersed ink-like catalyst slurry; the solvent of the catalyst slurry is water and isopropyl alcohol, and the solvent of water and isopropyl alcohol is The volume ratio is 0.5:9.5; the solute is Pt/CNTs and perfluorosulfonic acid resin, the mass percentage of the solute is 1%, and the mass ratio of carbon nanotubes in perfluorosulfonic acid resin and Pt/CNTs is 0.7:1.
S2.喷涂:将12μm厚度的质子交换膜置于90℃的加热板上,催化层浆料倒入喷枪中喷涂于质子交换膜的一侧后,置于40℃下放置1h,挥发多余溶剂,得到单侧催化层催化膜后,再将催化层浆料喷涂于质子交换膜的另一侧,同样置于40℃下放置1h,得到同时具有阳极催化层和阴极催化层的催化膜;催化膜两侧阳极催化层和阴极催化层的总铂载量为0.5mg/cm2,阳极催化层和阴极催化层的铂载量之比为1:4。S2. Spraying: Place a proton exchange membrane with a thickness of 12 μm on a heating plate at 90°C. Pour the catalytic layer slurry into a spray gun and spray it on one side of the proton exchange membrane. Place it at 40°C for 1 hour to evaporate excess solvent. After obtaining the single-sided catalytic layer catalytic membrane, spray the catalytic layer slurry on the other side of the proton exchange membrane, and place it at 40°C for 1 hour to obtain a catalytic membrane with both an anode catalytic layer and a cathode catalytic layer; catalytic membrane The total platinum loading of the anode catalytic layer and the cathode catalytic layer on both sides is 0.5 mg/cm 2 , and the ratio of the platinum loading of the anode catalytic layer and the cathode catalytic layer is 1:4.
S3.一次热压:先将厚度为0.4mm的PTFE薄膜分别贴在催化剂膜两侧得到组装体a,再将孔隙率为20%的多孔PEFT薄膜分别贴在组装体a两侧得到组装体b,最后将厚度为1mm薄铜片分别装配在组装体b两侧,得到组装体c;组装体c在100℃,0.4MPa压力下进行一次热压,热压时间为80s;热压完成后分别并依次剥离两侧的薄铜片、多孔PTFE薄膜和PTFE薄膜,得到半成品热压辅助增强的催化膜;S3. One-time hot pressing: first stick PTFE films with a thickness of 0.4mm on both sides of the catalyst membrane to obtain assembly a, and then stick porous PEFT films with a porosity of 20% on both sides of assembly a to obtain assembly b. , and finally, 1mm thick copper sheets are assembled on both sides of assembly b to obtain assembly c; assembly c is hot-pressed once at 100°C and 0.4MPa pressure, and the hot-pressing time is 80s; after the hot-pressing is completed, respectively And peel off the thin copper sheets, porous PTFE film and PTFE film on both sides in sequence to obtain a semi-finished hot-pressing-assisted reinforced catalytic membrane;
S4.二次热压:将厚度为220μm的气体扩散层置于半成品热压辅助增强的催化膜的两侧,装入热压机的模具中,在140℃和3MPa压力下进行二次热压,热压时间为120s,得到燃料电池膜电极。S4. Secondary hot pressing: Place the gas diffusion layer with a thickness of 220 μm on both sides of the semi-finished hot-pressed auxiliary reinforced catalytic membrane, put it into the mold of the hot press, and perform secondary hot pressing at 140°C and 3MPa pressure. , the hot pressing time is 120s, and the fuel cell membrane electrode is obtained.
实施例4Example 4
一种热压辅助增强燃料电池膜电极的制备方法,包括如下步骤:A method for preparing a thermal pressure-assisted reinforced fuel cell membrane electrode, including the following steps:
S1.制备催化层浆料:0.5g Pt/CNTs(铂的质量百分比为10%)中加入4.58mL蒸馏水和41.25mL异丙醇,在30W超声波清洗器中以500rpm速度搅拌30min,再加入0.9375g全氟磺酸树脂溶液(质量百分比为20wt%),常温条件下以10000rpm搅拌30min,得到均匀分散的墨水状催化剂浆料;催化剂浆料的溶剂为水和异丙醇,水和异丙醇的体积比为1:9;溶质为Pt/CNTs和全氟磺酸树脂,溶质的质量百分比为1.5%,全氟磺酸树脂和Pt/CNTs中碳纳米管的质量比为0.75:1。S1. Prepare the catalytic layer slurry: add 4.58mL distilled water and 41.25mL isopropyl alcohol to 0.5g Pt/CNTs (the mass percentage of platinum is 10%), stir in a 30W ultrasonic cleaner at 500rpm for 30min, and then add 0.9375g Perfluorosulfonic acid resin solution (mass percentage is 20wt%), stir at 10000rpm for 30 minutes at room temperature to obtain a uniformly dispersed ink-like catalyst slurry; the solvent of the catalyst slurry is water and isopropyl alcohol, and the solvent of water and isopropyl alcohol is The volume ratio is 1:9; the solute is Pt/CNTs and perfluorosulfonic acid resin, the mass percentage of the solute is 1.5%, and the mass ratio of carbon nanotubes in perfluorosulfonic acid resin and Pt/CNTs is 0.75:1.
S2.喷涂:将12μm厚度的质子交换膜置于90℃的加热板上,催化层浆料倒入喷枪中喷涂于质子交换膜的一侧后,置于40℃下放置1h,挥发多余溶剂,得到单侧催化层催化膜后,再将催化层浆料喷涂于质子交换膜的另一侧,同样置于40℃下放置1h,得到同时具有阳极催化层和阴极催化层的催化膜;催化膜两侧阳极催化层和阴极催化层的总铂载量为0.5mg/cm2,阳极催化层和阴极催化层的铂载量之比为1:4。S2. Spraying: Place a proton exchange membrane with a thickness of 12 μm on a heating plate at 90°C. Pour the catalytic layer slurry into a spray gun and spray it on one side of the proton exchange membrane. Place it at 40°C for 1 hour to evaporate excess solvent. After obtaining the single-sided catalytic layer catalytic membrane, spray the catalytic layer slurry on the other side of the proton exchange membrane, and place it at 40°C for 1 hour to obtain a catalytic membrane with both an anode catalytic layer and a cathode catalytic layer; catalytic membrane The total platinum loading of the anode catalytic layer and the cathode catalytic layer on both sides is 0.5 mg/cm 2 , and the ratio of the platinum loading of the anode catalytic layer and the cathode catalytic layer is 1:4.
S3.一次热压:先将厚度为0.6mm的PTFE薄膜分别贴在催化膜两侧得到组装体a,再将孔隙率为30%的多孔PEFT薄膜分别贴在组装体a两侧得到组装体b,最后将厚度为1mm薄铜片分别装配在组装体b两侧,得到组装体c;组装体c在110℃,0.5MPa压力下进行一次热压,热压时间为100s;热压完成后分别并依次剥离两侧的薄铜片、多孔PTFE薄膜和PTFE薄膜,得到半成品热压辅助增强的催化膜;S3. One-time hot pressing: first stick PTFE films with a thickness of 0.6mm on both sides of the catalytic membrane to obtain assembly a, and then stick porous PEFT films with a porosity of 30% on both sides of assembly a to obtain assembly b. , and finally, 1mm thick copper sheets are assembled on both sides of assembly b to obtain assembly c; assembly c is hot-pressed once at 110°C and 0.5MPa pressure, and the hot-pressing time is 100s; after the hot-pressing is completed, respectively And peel off the thin copper sheets, porous PTFE film and PTFE film on both sides in sequence to obtain a semi-finished hot-pressing-assisted reinforced catalytic membrane;
S4.二次热压:将厚度为220μm的气体扩散层置于半成品热压辅助增强的催化膜的两侧,装入热压机的模具中,在140℃和3MPa压力下进行二次热压,热压时间为120s,得到燃料电池膜电极。S4. Secondary hot pressing: Place the gas diffusion layer with a thickness of 220 μm on both sides of the semi-finished hot-pressed auxiliary reinforced catalytic membrane, put it into the mold of the hot press, and perform secondary hot pressing at 140°C and 3MPa pressure. , the hot pressing time is 120s, and the fuel cell membrane electrode is obtained.
对比例1Comparative example 1
一种热压辅助增强燃料电池膜电极的制备方法,包括如下步骤:A method for preparing a thermal pressure-assisted reinforced fuel cell membrane electrode, including the following steps:
S1.制备催化层浆料:0.5g Pt/CNTs(铂的质量百分比为10%)中加入5.25mL蒸馏水和29.75mL异丙醇,在30W超声波清洗器中以500rpm速度搅拌30min,再加入1.0g全氟磺酸树脂溶液(质量百分比为20wt%),常温条件下以10000rpm搅拌30min,得到均匀分散的墨水状催化剂浆料;催化剂浆料的溶剂为水和异丙醇,水和异丙醇的体积比为1.5:8.5;溶质为Pt/CNTs和全氟磺酸树脂,溶质的质量百分比为2%,全氟磺酸树脂和Pt/CNTs中碳纳米管的质量比为0.8:1。S1. Prepare the catalytic layer slurry: add 5.25mL distilled water and 29.75mL isopropyl alcohol to 0.5g Pt/CNTs (the mass percentage of platinum is 10%), stir in a 30W ultrasonic cleaner at 500rpm for 30min, and then add 1.0g Perfluorosulfonic acid resin solution (mass percentage is 20wt%), stir at 10000rpm for 30 minutes at room temperature to obtain a uniformly dispersed ink-like catalyst slurry; the solvent of the catalyst slurry is water and isopropyl alcohol, and the solvent of water and isopropyl alcohol is The volume ratio is 1.5:8.5; the solute is Pt/CNTs and perfluorosulfonic acid resin, the mass percentage of the solute is 2%, and the mass ratio of carbon nanotubes in perfluorosulfonic acid resin and Pt/CNTs is 0.8:1.
S2.喷涂:将12μm厚度的质子交换膜置于90℃的加热板上,催化层浆料倒入喷枪中喷涂于质子交换膜的一侧后,置于40℃下放置1h,挥发多余溶剂,得到单侧催化层催化膜后,再将催化层浆料喷涂于质子交换膜的另一侧,同样置于40℃下放置1h,得到同时具有阳极催化层和阴极催化层的催化膜;催化膜两侧阳极催化层和阴极催化层的总铂载量为0.5mg/cm2,阳极催化层和阴极催化层的铂载量之比为1:4。S2. Spraying: Place a proton exchange membrane with a thickness of 12 μm on a heating plate at 90°C. Pour the catalytic layer slurry into a spray gun and spray it on one side of the proton exchange membrane. Place it at 40°C for 1 hour to evaporate excess solvent. After obtaining the single-sided catalytic layer catalytic membrane, spray the catalytic layer slurry on the other side of the proton exchange membrane, and place it at 40°C for 1 hour to obtain a catalytic membrane with both an anode catalytic layer and a cathode catalytic layer; catalytic membrane The total platinum loading of the anode catalytic layer and the cathode catalytic layer on both sides is 0.5 mg/cm 2 , and the ratio of the platinum loading of the anode catalytic layer and the cathode catalytic layer is 1:4.
S3.热压:将厚度为220μm的气体扩散层置于催化膜的两侧,装入热压机的模具中,在140℃和3MPa压力下进行热压,热压时间为120s,得到燃料电池膜电极。S3. Hot pressing: Place the gas diffusion layer with a thickness of 220 μm on both sides of the catalytic membrane, put it into the mold of the hot press, and perform hot pressing at 140°C and 3MPa pressure. The hot pressing time is 120s to obtain the fuel cell. membrane electrode.
实施例5Example 5
膜电极电性能测试Membrane electrode electrical performance testing
采用燃料电池测试系统,该系统使用的反应物为压缩空气和高纯氢,系统配置外部增湿系统,通过控制增湿器温度来得到不同的气体增湿效果。测试前,先对MEA进行活化,其目的是使质子交换膜以及催化层所含的Nafion树脂含有充足的水,以保证足够的电导率。待工作条件稳定后,控制电池不同的放电电流或电压,测试结束后,导出实验数据。燃料电池的单体电池由膜电极、极板、密封垫片和端板等组成。极板采用尺寸为50×50×3mm的不透气硬石墨板,内侧设计为平行的蛇形三流道;密封垫片采用普通塑料垫片;用不锈钢板作为端板。各部件间紧装配以减小电池内阻。自制单体电池中膜电极的有效面积为25cm2。将电极有效面积为25cm2的膜电极装入单体实验电池后,在测试台上进行单体电池性能测试。膜电极的电化学性能测试条件中氢气和氧气的湿度都是50%RH,将氢压和氧压分别调至0.28MPa和0.30MPa,将单体电池与外接恒流恒压电源相连接,电池温度升至80℃,测量电池的电压-电流曲线。A fuel cell test system is used. The reactants used in this system are compressed air and high-purity hydrogen. The system is equipped with an external humidification system, and different gas humidification effects are obtained by controlling the temperature of the humidifier. Before the test, the MEA is first activated. The purpose is to make the proton exchange membrane and the Nafion resin contained in the catalytic layer contain sufficient water to ensure sufficient conductivity. After the working conditions are stable, control the different discharge currents or voltages of the battery. After the test is completed, export the experimental data. The single cell of a fuel cell is composed of membrane electrodes, plates, sealing gaskets and end plates. The electrode plate is made of an air-impermeable hard graphite plate with a size of 50×50×3mm, and the inside is designed with a parallel serpentine three-flow channel; the sealing gasket is an ordinary plastic gasket; a stainless steel plate is used as the end plate. The components are tightly assembled to reduce the internal resistance of the battery. The effective area of the membrane electrode in the self-made single cell is 25cm 2 . After the membrane electrode with an electrode effective area of 25cm2 is installed into the single experimental battery, the single battery performance test is performed on the test bench. In the electrochemical performance test conditions of the membrane electrode, the humidity of hydrogen and oxygen is both 50% RH. Adjust the hydrogen pressure and oxygen pressure to 0.28MPa and 0.30MPa respectively. Connect the single cell to an external constant current and constant voltage power supply. The battery The temperature rises to 80°C and the voltage-current curve of the battery is measured.
对实施例2-4和对比例1所制备的膜电极按照上述测试系统进行测试,并对实施例2中经过S3.一次热压得到半成品热压辅助增强的催化膜和对比例1中经过S2.喷涂得到同时具有阳极催化层和阴极催化层的催化膜进行扫描电镜(SEM)形貌表征;The membrane electrodes prepared in Examples 2-4 and Comparative Example 1 were tested according to the above test system, and the semi-finished hot-pressing-assisted enhanced catalytic membrane obtained by S3 and one hot pressing in Example 2 and S2 in Comparative Example 1 were .Spray coating to obtain a catalytic film with both anode catalytic layer and cathode catalytic layer for scanning electron microscopy (SEM) morphology characterization;
实施例3和实施例4的测试结果如表1所示:The test results of Example 3 and Example 4 are shown in Table 1:
表1Table 1
实施例2和对比例1的极化曲线如图2所示,由表1和图2可知,对比例1中没有对喷涂后的Pt/CNT催化膜进行热压增强处理,两种膜电极的初始活化极化基本相同,因为活化极化只与催化剂的本征性能有关,实施例2和对比例1所用的催化剂相同,所以活化极化也基本相同;在电流密度提高时,实施例2的电池电压和功率密度更高,这是因为经过热压增强辅助处理的碳纳米管更容易在层与层之间形成导电通路;进一步的,图3为实施例2和对比例1的SEM图,其中图3A为实施例2中经过S3.一次热压得到半成品热压辅助增强的催化膜的表面形貌,图3B为对比例1中经过S2.喷涂得到同时具有阳极催化层和阴极催化层的催化膜的表面形貌,热压处理后催化层的表面形貌比未经过热压处理催化剂更加光滑,说明了更多导电通路的形成,可以减少膜电极的欧姆阻抗和欧姆极化,从而提高了膜电极的燃料电池电化学性能。The polarization curves of Example 2 and Comparative Example 1 are shown in Figure 2. It can be seen from Table 1 and Figure 2 that in Comparative Example 1, the sprayed Pt/CNT catalytic membrane was not subjected to hot pressure enhancement treatment. The initial activation polarization is basically the same, because the activation polarization is only related to the intrinsic performance of the catalyst. The catalyst used in Example 2 and Comparative Example 1 is the same, so the activation polarization is also basically the same; when the current density increases, the The battery voltage and power density are higher because the carbon nanotubes that have been assisted by thermal pressure enhancement are more likely to form conductive paths between layers; further, Figure 3 is the SEM image of Example 2 and Comparative Example 1. Figure 3A shows the surface morphology of the semi-finished hot-pressing-assisted catalytic membrane obtained through S3. One hot pressing in Example 2, and Figure 3B shows the catalytic film having both an anode catalytic layer and a cathode catalytic layer obtained through S2. spraying in Comparative Example 1. The surface morphology of the catalytic membrane, the surface morphology of the catalytic layer after hot-pressing treatment is smoother than that of the catalyst without hot-pressing treatment, indicating the formation of more conductive paths, which can reduce the ohmic impedance and ohmic polarization of the membrane electrode, thereby improving The electrochemical performance of membrane electrodes in fuel cells.
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that these entities or operations are mutually exclusive. any such actual relationship or sequence exists between them. Furthermore, the terms "comprises," "comprises," or any other variations thereof are intended to cover a non-exclusive inclusion such that a process, method, article, or apparatus that includes a list of elements includes not only those elements, but also those not expressly listed other elements, or elements inherent to the process, method, article or equipment.
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art will understand that various changes, modifications, and substitutions can be made to these embodiments without departing from the principles and spirit of the invention. and modifications, the scope of the invention is defined by the appended claims and their equivalents.
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WO2022170717A1 (en) * | 2021-02-10 | 2022-08-18 | 华东理工大学 | Ccm membrane electrode, preparation method therefor and use thereof |
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CN110459774A (en) * | 2019-08-12 | 2019-11-15 | 南京大学昆山创新研究院 | A kind of preparation method of fuel cell membrane electrode |
WO2022170717A1 (en) * | 2021-02-10 | 2022-08-18 | 华东理工大学 | Ccm membrane electrode, preparation method therefor and use thereof |
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