CN112323510A - 一种连续涂敷低成本制备气体扩散层碳纸的方法 - Google Patents
一种连续涂敷低成本制备气体扩散层碳纸的方法 Download PDFInfo
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Abstract
本发明提出一种连续涂敷低成本制备气体扩散层碳纸的方法,所述气体扩散层碳纸是将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂混合制成的浆料喷涂于氢氧化铝溶胶挂膜的聚四氟乙烯无纺布表面,连续通过酸处理、氨处理得到喷涂层凝固化的无纺布,最后将疏水剂超声雾化喷涂于表面后干燥而制得。本发明提供的方法制得碳纸,导电碳材料与无纺布粘结牢固,碳材料分散均匀并被气凝胶的网络固定,制得的碳纸在导电性、强度、柔性和孔径均匀分布方面保持了较佳的性能,并且制备工艺简单,易于规模化连续生产,能耗低,成本低。
Description
技术领域
本发明涉及燃料电池技术领域,特别是涉及一种连续涂敷低成本制备气体扩散层碳纸的方法。
背景技术
燃料电池是一种将燃料与氧化剂的化学能通过电化学反应直接转换成电能的发电装置。主要由正极、负极、电解质和辅助设备组成。由于燃料电池具有效率高、启动快、污染小等优点,被认为是继风力、水力和太阳能之后有希望大量提供电能的第四种发电技术,是一种绿色能源技术,可有效缓解目前世界面临的“能源短缺”和“环境污染”这两大难题,实现能源的多元化。质子交换膜燃料电池属于低温燃料电池,除了具备燃料电池的一般特定之外,还具有工作温度低、启动快、无电解液流失、无腐蚀、能量转化率高、寿命长、重量轻、体积小等特点,是便携式电源、分布式电站、未来电动汽车的理想替代电源。
质子交换膜燃料电池由于具有高的功率密度、高的能量转换效率、低温启动、无污染、体积轻巧、对压力变化不敏感及电池寿命长等诸多优点,被认为是首选的洁净、高效的发电装置。在新能源汽车领域具有巨大的应用潜力。燃料电池中,膜电极组件(MEA)是核心元件,其不但原料成本高,而且制备复合工艺要求高。膜电极组件是以质子交换膜为夹层中心,在两侧分别复合催化层、气体扩散层而形成的扩散层-催化层-质子交换膜-催化层、扩散层结构的组合件。
燃料电池扩散层是影响电池性能的关键部件,在电极中起支撑催化剂层和稳定电极结构的作用, 还具备为电极反应提供气体通道、电子通道和排水通道等多种功能。用于制备扩散层的是碳材料, 包括碳纤维纸、碳纤维布、碳纤维毡等。采用的技术路线主要是将碳纤维、聚合物纤维、粘合剂复合后,制备成纸,进一步在高温碳化处理得到碳纤维纸,该碳纸脆性大难以连续生产,碳纸石墨化工序大多只能采用间歇式工艺, 极大地限制了碳纤维纸规模化生产,而且成本高,能耗高。也有将碳纤维分散于制浆,抄纸干燥,得到碳纸,但该碳纸强度差、耐折性差,疏水性差,需要进行二次涂敷。而对于新型碳纸的研究和应用受到人们广泛关注。
中国发明专利申请号200710019376.7公开了燃料电池气体扩散层的制备方法,将碳黑粉末、蒸馏水、分散剂混合均匀,然后将PTFE或PVDF乳液均匀加入上述所述的碳黑粉末分散体系中,并继续混合;混合方法采用超声波、机械高速剪切或机械搅拌;将碳纸或碳布放入上述的分散体系中浸渍后取出晾干,并放入干燥箱干,得到载有碳黑和PTFE或PVDF的碳纸或碳布。中国发明专利申请号201721695602.9公开了一种碳纤维纸,该气体扩散层碳纸包括:碳纤维层、微孔导电涂层,碳纤维层中分布有纳米碳纤维和短切碳纤维,碳纤维层上下为石墨烯和PETE组成的微孔导电涂层。
为了保证燃料电池气体扩散层碳纸具有良好的柔性、导电性、强度和均匀分布的孔径,有必要提出一种新型气体扩散层碳纸,进而提高燃料电池气体扩散层的使用性能的同时,简化了制备工艺,实现了规模化生产。
发明内容
针对现有的燃料电池气体扩散层采用的碳纸存在制备工艺复杂、生产能耗高、成本高、发脆、难以批量化生产供应等缺陷,本发明提出一种连续涂敷低成本制备气体扩散层碳纸的方法,从而在改善碳纸机械性能和电学性能的同时,实现了低能耗、规模化生产。
为解决上述问题,本发明采用以下技术方案:
一种连续涂敷低成本制备气体扩散层碳纸的方法,所述气体扩散层碳纸是将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂混合制成的浆料喷涂于氢氧化铝溶胶挂膜的聚四氟乙烯无纺布表面,连续通过酸处理、氨处理得到喷涂层凝固化的无纺布,最后将疏水剂超声雾化喷涂于表面后干燥而制得;具体制备方法如下:
(1)将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂分散均匀,得到浆料;
(2)将聚四氟乙烯无纺布浸入氢氧化铝溶胶中挂膜,然后取出干燥,接着将步骤(1)制得的浆料喷涂于无纺布表面,再经辊筒输送,连续依次送入酸环境和氨环境处理,表面形成二氧化硅凝胶,使得喷涂浆料层凝固化,得到涂布浆料处理的无纺布;
(3)先利用牵引辊将涂布浆料处理的无纺布导入超声雾化室,将疏水剂超声雾化喷涂于无纺布表面,形成纳米级疏水层,然后导入干燥室中干燥处理,进一步平整,即得疏松、柔性的燃料电池多孔碳纸。
优选的,步骤(1)中所述导电碳材料为碳纤维、碳纳米管、介孔碳、炭黑、碳气凝胶、石墨、石墨烯中的一种或两种以上的组合,所述无机纤维为海泡石纤维、玻璃纤维、陶瓷纤维、硅灰石纤维、氢氧化镁纤维中的一种或两种以上的组合,所述增粘剂为质量浓度3%的羟丙基甲基纤维素醚。
优选的,步骤(1)中,乙醇、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、导电碳材料、无机纤维、增粘剂的质量比例为100:5-10:5-10:40-60:20-30:2-4。
氢氧化铝溶胶具有良好的成膜性能,本发明通过先在聚四氟乙烯无纺布预涂氢氧化铝溶胶,使得无纺布可与导电碳材料稳定粘附并均匀分散,保证了所得材料的导电性能。优选的,步骤(2)中所述氢氧化铝溶胶的固含量为20-25%。步骤(2)中所述无纺布在氢氧化铝溶胶中的浸入时间为1-3h。
进一步的,二氧化硅气凝胶是一种由纳米量级粒子聚集并以空气为分散介质的新型非晶固态多孔材料,其具有低密度、高孔隙率、高比表面积、低导热系数、低声波传播速率和低介电常数等一系列特点,是一类具有高比表面积和优异吸附性能的纳米多孔轻质材料,而传统的以正硅酸乙酯为前躯体制备的二氧化硅气凝胶表面连有亲水基团-OH,会导致二氧化硅气凝胶易于吸附水分,存在脆性大、强度低等缺点,而利用甲基三甲氧基硅烷和二甲基二甲氧基硅烷作为硅源,可制得大比表面积的优良柔韧性二氧化硅气凝胶。因此,本发明将甲基三甲氧基硅烷和二甲基二甲氧基硅烷与导电碳材料、无机纤维涂敷无纺布后,通过连续的酸、氨处理,甲基三甲氧基硅烷和二甲基二甲氧基硅烷形成二氧化硅凝胶,将导电碳材料牢固稳定在无纺布,并经干燥形成透气微孔,得到的碳纸柔韧性好,耐折性佳,孔径分布均匀。
优选的,步骤(2)中所述干燥的温度为100-150℃,干燥2-4h。
优选的,步骤(2)中所述酸环境为pH值为4的盐酸溶液、硫酸溶液、硝酸溶液中的一种,温度为50-60℃,酸环境处理时间为1-2h,所述氨环境为pH值为10的氨水,温度为60-80℃,氨环境处理时间为0.5-1.5h。
更进一步的,将聚四氟乙烯与纳米碳粒配制的疏水剂超声雾化喷涂于表面具有二氧化硅凝胶层的无纺布表面,使得碳纸具有适宜的疏水性能,并且进一步提高了导电性。
优选的,步骤(3)中所述疏水剂由质量浓度为12%的聚四氟乙烯乳液、纳米碳粒按照质量比例100:10-15配制而成,所述纳米碳粒为粒径3-5nm的碳粒。
优选的,步骤(3)中所述超声雾化喷涂的超声波频率为40-50kHz,气体压力为1-1.5MPa,超声雾化头振幅为5-10μm,所述疏水层的厚度为40-100nm。
优选的,步骤(3)中所述干燥处理的温度为200-250℃,干燥40-60min,所述碳纸的厚度为0.1-0.2mm。
现有的燃料电池气体扩散层采用碳纸存在柔性差、易发脆、导电性差等缺陷,并且制备工艺复杂、生产能耗高、成本高、难以批量化生产供应,限制了其应用。鉴于此,本发明提出一种连续涂敷低成本制备气体扩散层碳纸的方法,将甲基三甲氧基硅烷和二甲基二甲氧基硅烷与乙醇、导电碳材料、无机纤维、增粘剂分散为浆料;将聚四氟乙烯无纺布浸入氢氧化铝溶胶挂膜,取出后干燥;然后将浆料喷涂在无纺布,经辊筒输送,连续进行酸环境处理、氨环境处理,使得喷涂浆料层凝固化;再将得到的涂布浆料处理的无纺布利用牵引辊导入超声雾化室,将聚四氟乙烯与纳米碳粒配制的疏水剂超声雾化喷涂在表面,形成纳米级疏水层,干燥处理,进一步平整,得到疏松、柔性的燃料电池多孔碳纸。本发明提供的方法制得碳纸,导电碳材料与无纺布粘结牢固,碳材料分散均匀并被气凝胶的网络固定,制得的碳纸在导电性、强度、柔性和孔径均匀分布方面保持了较佳的性能,并且制备工艺简单,易于规模化连续生产,能耗低,成本低。
本发明提出一种连续涂敷低成本制备气体扩散层碳纸的方法,与现有技术相比,其突出的特点和优异的效果在于:
1、本发明的方法不但解决了导电碳材料与无纺布粘结不牢容易脱落的问题,而且通过先涂敷再胶化处理的方法,使碳材料分散均匀,并被气凝胶的网络固定,使得到的碳纸产品在导电性、强度、柔性和孔径均匀分布方面保持了较佳的性能。
2、本发明的方法,制备工艺简单,易于规模化连续生产,能耗低,成本低。
附图说明
图1:实施例1碳纸弯折100次的照片,产品无变形、无开裂。
图2:对比例1碳纸弯折4次的照片,产品发脆、裂开。
具体实施方式
以下通过具体实施方式对本发明作进一步的详细说明,但不应将此理解为本发明的范围仅限于以下的实例。在不脱离本发明上述方法思想的情况下,根据本领域普通技术知识和惯用手段做出的各种替换或变更,均应包含在本发明的范围内。
实施例1
(1)将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂分散均匀,得到浆料;导电碳材料为碳纤维;无机纤维为海泡石纤维;增粘剂为质量浓度为3%的羟丙基甲基纤维素醚;浆料制备中,乙醇、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、导电碳材料、无机纤维、增粘剂的质量比例为100:8:8:50:25:3;
(2)将聚四氟乙烯无纺布浸入氢氧化铝溶胶中挂膜,然后取出干燥,接着将制得的浆料喷涂于无纺布表面,再经辊筒输送,连续依次送入酸环境和氨环境处理,表面形成二氧化硅凝胶,使得喷涂浆料层凝固化,得到涂布浆料处理的无纺布;氢氧化铝溶胶的固含量为22%;无纺布在氢氧化铝溶胶中的浸入时间为2h;干燥的温度为125℃,干燥3h;酸环境为pH值为4的盐酸溶液,温度为55℃,酸环境处理时间为1.5h,所述氨环境为pH值为10的氨水,温度为70℃,氨环境处理时间为1h;
(3)先利用牵引辊将涂布浆料处理的无纺布导入超声雾化室,将疏水剂超声雾化喷涂于无纺布表面,形成纳米级疏水层,然后导入干燥室中干燥处理,进一步平整,即得疏松、柔性的燃料电池多孔碳纸;疏水剂由质量浓度为12%的聚四氟乙烯乳液、纳米碳粒按照质量比例100:10配制而成,,所述纳米碳粒为平均粒径4nm的碳粒;超声雾化喷涂的超声波频率为45kHz,气体压力为1.2MPa,超声雾化头振幅为8μm;疏水层的平均厚度为80nm;干燥处理的温度为225℃,干燥50min,所述碳纸的平均厚度为0.2mm。
测试方法:
将本实施例制备获得的气体扩散层碳纸进行拉伸强度测试,将碳纸制成长45mm、宽5mm的样条,在常温常压下,使用Insron25567型万能拉力试验机测试样品的拉伸强度,测试定长为35mm,拉伸速率为5mm/min,得到结果如表1所示;
将本实施例制备获得的气体扩散层碳纸进行抗弯性能测试,将碳纸制成长200mm、宽25mm的样条,在常温常压下,使用YG(B)022D型自动硬挺度实验仪进行测试,测量角度分4.5°,测试并计算抗弯刚度。测试结果见表1所示。
透气性:采用在80Pa压力差下进行测试,得到本发明制得的气体扩散膜在常温下的透气率;
电阻率:根据四探针法测试;所得数据如表1所示。
耐折性:弯折90°,通过弯折次数衡量耐折性。图1是实施例1碳纸弯折100次的照片,产品无变形、无开裂。
实施例2
(1)将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂分散均匀,得到浆料;导电碳材料为碳纳米管;无机纤维为玻璃纤维;增粘剂质量浓度为3%的羟丙基甲基纤维素醚;浆料制备中,乙醇、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、导电碳材料、无机纤维、增粘剂的质量比例为100:5:5:40:20:2;
(2)将聚四氟乙烯无纺布浸入氢氧化铝溶胶中挂膜,然后取出干燥,接着将制得的浆料喷涂于无纺布表面,再经辊筒输送,连续依次送入酸环境和氨环境处理,表面形成二氧化硅凝胶,使得喷涂浆料层凝固化,得到涂布浆料处理的无纺布;氢氧化铝溶胶的固含量为20%;无纺布在氢氧化铝溶胶中的浸入时间为1h;干燥的温度为100℃,干燥4h;酸环境为pH值为4的硫酸溶液,温度为50℃,酸环境处理时间为2h,所述氨环境为pH值为10的氨水,温度为60℃,氨环境处理时间为1.5h;
(3)先利用牵引辊将涂布浆料处理的无纺布导入超声雾化室,将疏水剂超声雾化喷涂于无纺布表面,形成纳米级疏水层,然后导入干燥室中干燥处理,进一步平整,即得疏松、柔性的燃料电池多孔碳纸;疏水剂由质量浓度为12%的聚四氟乙烯乳液、纳米碳粒按照质量比例100:10配制而成,所述纳米碳粒为平均粒径3nm的碳粒;超声雾化喷涂的超声波频率为40kHz,气体压力为1MPa,超声雾化头振幅为5μm;疏水层的平均厚度为40nm;干燥处理的温度为200℃,干燥60min,所述碳纸的平均厚度为0.1mm。
采用实施例1的方法进行测试,测试结果如表1所示。
实施例3
(1)将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂分散均匀,得到浆料;导电碳材料为介孔碳;无机纤维为陶瓷纤维;增粘剂质量浓度为3%的羟丙基甲基纤维素醚;浆料制备中,乙醇、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、导电碳材料、无机纤维、增粘剂的质量比例为100:10:10:60:30:4;
(2)将聚四氟乙烯无纺布浸入氢氧化铝溶胶中挂膜,然后取出干燥,接着将制得的浆料喷涂于无纺布表面,再经辊筒输送,连续依次送入酸环境和氨环境处理,表面形成二氧化硅凝胶,使得喷涂浆料层凝固化,得到涂布浆料处理的无纺布;氢氧化铝溶胶的固含量为25%;无纺布在氢氧化铝溶胶中的浸入时间为3h;干燥的温度为150℃,干燥2h;酸环境为pH值为4的硝酸溶液,温度为60℃,酸环境处理时间为1h,所述氨环境为pH值为10的氨水,温度为80℃,氨环境处理时间为0.5h;
(3)先利用牵引辊将涂布浆料处理的无纺布导入超声雾化室,将疏水剂超声雾化喷涂于无纺布表面,形成纳米级疏水层,然后导入干燥室中干燥处理,进一步平整,即得疏松、柔性的燃料电池多孔碳纸;疏水剂由质量浓度为12%的聚四氟乙烯乳液、纳米碳粒按照质量比例100:15配制而成,所述纳米碳粒为平均粒径5nm的碳粒;超声雾化喷涂的超声波频率为50kHz,气体压力为1.5MPa,超声雾化头振幅为10μm;疏水层的平均厚度为100nm;干燥处理的温度为250℃,干燥40min,所述碳纸的平均厚度为0.4mm。
采用实施例1的方法进行测试,测试结果如表1所示。
实施例4
(1)将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂分散均匀,得到浆料;导电碳材料为石墨;无机纤维为硅灰石纤维;增粘剂质量浓度为3%的羟丙基甲基纤维素醚;浆料制备中,乙醇、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、导电碳材料、无机纤维、增粘剂的质量比例为100:7:7:48:26:3;
(2)将聚四氟乙烯无纺布浸入氢氧化铝溶胶中挂膜,然后取出干燥,接着将制得的浆料喷涂于无纺布表面,再经辊筒输送,连续依次送入酸环境和氨环境处理,表面形成二氧化硅凝胶,使得喷涂浆料层凝固化,得到涂布浆料处理的无纺布;氢氧化铝溶胶的固含量为23%;无纺布在氢氧化铝溶胶中的浸入时间为1.5h;干燥的温度为130℃,干燥3h;酸环境为pH值为4的盐酸溶液,温度为56℃,酸环境处理时间为1.5h,所述氨环境为pH值为10的氨水,温度为68℃,氨环境处理时间为1h;
(3)先利用牵引辊将涂布浆料处理的无纺布导入超声雾化室,将疏水剂超声雾化喷涂于无纺布表面,形成纳米级疏水层,然后导入干燥室中干燥处理,进一步平整,即得疏松、柔性的燃料电池多孔碳纸;疏水剂由质量浓度为12%的聚四氟乙烯乳液、纳米碳粒按照质量比例100:15配制而成,所述纳米碳粒为平均粒径4nm的碳粒;超声雾化喷涂的超声波频率为46kHz,气体压力为1.3MPa,超声雾化头振幅为7μm;疏水层的平均厚度为70nm;干燥处理的温度为230℃,干燥48min,所述碳纸的平均厚度为0.3mm。
采用实施例1的方法进行测试,测试结果如表1所示。
对比例1
市售中国台湾碳能型号为CDS090的碳纸。
采用实施例1的方法进行测试,测试结果如表1所示。
图2是对比例1碳纸弯折4次的照片,产品发脆、裂开。
表1:
通过测试,本发明的提供的方法制得碳纸,具有良好的机械强度、导电性和透气性,满足燃料电池基本需求。特别是制备工艺简单,易于规模化连续生产,能耗低,成本低。
Claims (10)
1.一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,所述气体扩散层碳纸是将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂混合制成的浆料喷涂于氢氧化铝溶胶挂膜的聚四氟乙烯无纺布表面,连续通过酸处理、氨处理得到喷涂层凝固化的无纺布,最后将疏水剂超声雾化喷涂于表面后干燥而制得;具体制备方法如下:
(1)将甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙醇、导电碳材料、无机纤维、增粘剂分散均匀,得到浆料;
(2)将聚四氟乙烯无纺布浸入氢氧化铝溶胶中挂膜,然后取出干燥,接着将制得的浆料喷涂于无纺布表面,再经辊筒输送,连续依次送入酸环境和氨环境处理,表面形成二氧化硅凝胶,使得喷涂浆料层凝固化,得到涂布浆料处理的无纺布;
(3)先利用牵引辊将涂布浆料处理的无纺布导入超声雾化室,将疏水剂超声雾化喷涂于无纺布表面,形成纳米级疏水层,然后导入干燥室中干燥处理,进一步平整,即得疏松、柔性的燃料电池多孔碳纸。
2.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(1)中所述导电碳材料为碳纤维、碳纳米管、介孔碳、炭黑、碳气凝胶、石墨、石墨烯中的一种或两种以上的组合,所述无机纤维为海泡石纤维、玻璃纤维、陶瓷纤维、硅灰石纤维、氢氧化镁纤维中的一种或两种以上的组合,所述增粘剂为质量浓度3%的羟丙基甲基纤维素醚。
3.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(1)中,乙醇、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、导电碳材料、无机纤维、增粘剂的质量比例为100:5-10:5-10:40-60:20-30:2-4。
4.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(2)中所述氢氧化铝溶胶的固含量为20-25%。
5.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(2)中所述聚四氟乙烯无纺布在氢氧化铝溶胶中的浸入时间为1-3h。
6.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(2)中所述干燥的温度为100-150℃,干燥2-4h。
7.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(2)中所述酸环境为pH值为4的盐酸溶液、硫酸溶液、硝酸溶液中的一种,温度为50-60℃,酸环境处理时间为1-2h,所述氨环境为pH值为10的氨水,温度为60-80℃,氨环境处理时间为0.5-1.5h。
8.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(3)中所述疏水剂由质量浓度为12%的聚四氟乙烯乳液、纳米碳粒按照质量比例100:10-15配制而成,所述纳米碳粒为粒径3-5nm的碳粒。
9.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(3)中所述超声雾化喷涂的超声波频率为40-50kHz,气体压力为1-1.5MPa,超声雾化头振幅为5-10μm,所述疏水层的厚度为40-100nm。
10.根据权利要求1所述的一种连续涂敷低成本制备气体扩散层碳纸的方法,其特征在于,步骤(3)中所述干燥处理的温度为200-250℃,干燥40-60min,所述燃料电池多孔碳纸的厚度为0.1-0.4mm。
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