CN111408725A - 一种具有梯度孔径的spe电解槽用气体扩散层制备方法 - Google Patents
一种具有梯度孔径的spe电解槽用气体扩散层制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,首先将钛粉与溶剂、粘结剂和增塑剂机械搅拌混合获得料液;其次将得到的料液在流延机内流延成型,获得平板状生胚;然后将得到的平板状生胚转移至真空炉中,进行程序升温烧结,获得微孔扩散层;最后通过真空等离子喷涂法在获得微孔扩散层上喷涂钛粉制备大孔扩散层,由此制得具有梯度孔径的SPE电解槽用气体扩散层。本发明制备的气体扩散层尺寸、幅面可调,具有梯度孔径,能够促进电解小室内气液传质,提高电解槽的性能。
Description
技术领域
本发明涉及电解水制氢领域,具体涉及一种具有梯度孔径的SPE电解槽用气体扩散层制备方法。
背景技术
电解制氢可以通过氢气存储实现大规模、低成本的能源消纳利用,是最有前景的可再生能源消纳方式之一,在世界上获得了普遍认可。电解制氢技术主要包括传统的碱性电解水制氢和新兴的固态电解质(SPE)电解水制氢。与碱性电解槽相比,SPE电解槽具有效率高、装置紧凑、产品氢气纯度高等特点,同时启动和停机迅速,能够在宽负荷范围内操作,因此在消纳间歇、波动性可再生能源的应用场景内展现出独特的竞争力。
SPE电解槽主要由双极板、阴/阳极气体扩散层、阴/阳极催化层、离子交换膜等关键部件组成。气体扩散层通常为导电的多孔材料,起到支撑膜电极、收集电流和气液传输等多重作用,是影响电解槽性能的关键部件之一。因为水电解时阳极产生的强氧化性活性氧及酸性环境下的腐蚀,商用SPE电解槽多采用烧结钛板作为阳极气体扩散层。多孔烧结钛板的孔径能够显著影响其内部的气液传质特性,因此优化扩散层孔径成为提升电解槽性能的重要手段。
商用烧结钛板采用先将钛粉冲压成型再高温煅烧的方法生产。气体扩散层的尺寸受到冲压器械和模具尺寸的限制,现有产品逐渐难以满足电解槽规模大型化的需求。同时传统工艺生产的气体扩散层孔径单一,难以有效促进电解槽内气液传质。
发明内容
本发明提供一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,以克服现有技术的不足,本发明制备的气体扩散层尺寸、幅面可调,具有梯度孔径,能够促进电解小室内气液传质,提高电解槽的性能。
为达到上述目的,本发明采用如下技术方案:
一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)料液制备:将钛粉与溶剂、粘结剂和增塑剂机械搅拌混合获得料液;
(2)流延成胚:将步骤(1)得到的料液在流延机内流延成型,获得平板状生胚;
(3)真空烧结:将步骤(2)得到的平板状生胚转移至真空炉中,进行程序升温烧结,获得微孔扩散层;
(4)喷涂:通过真空等离子喷涂法在步骤(3)获得微孔扩散层上喷涂钛粉制备大孔扩散层,由此制得具有梯度孔径的SPE电解槽用气体扩散层。
进一步地,所述的步骤(1)中,钛粉为球形雾化钛粉,钛粉粒径为30~80μm。
进一步地,所述的步骤(1)中,溶剂为乙醇、甲苯或甲醇,粘结剂为聚乙烯醇缩丁醛树脂或丙烯酸树脂,增塑剂为PEG400。
进一步地,所述的步骤(1)中,钛粉质量分数为65%~85%,溶剂质量分数为10%~30%:粘结剂质量分数为1%~2%:增塑剂质量分数为3%~4%。
进一步地,所述的步骤(1)中,机械搅拌时间为8~24h。
进一步地,所述的步骤(2)中,流延成型时,流延速度为200~400mm/min,流延宽度为0.5~2m,流延厚度为200~800μm。
进一步地,所述的步骤(3)中,程序升温烧结具体为:在Ar气流中由室温升温至400~500℃,压力为10~20mbar,保持恒温10~60min;在真空中继续升温至800~1200℃,真空度为10-4~10-5mbar,保持恒温120~240min;整个过程中升温速率为1~5℃/min。
进一步地,所述的步骤(4)中,真空等离子喷涂法使用涂料为无规则形状的氢化脱氢钛粉,粉末粒径为100~200μm;等离子焓为10~20MJ/kg;喷涂速度为300~500mm/s;喷涂前基体预热至200~300℃;喷涂压力为30~50mbar;喷涂厚度为100~400μm。
与现有技术相比,本发明具有以下有益的技术效果:
本发明所述的具有梯度孔径的SPE电解槽用气体扩散层制备方法,采用流延法制造微孔扩散层,操作流程简单,可实现宽幅面生产;采用真空等离子喷涂法在微孔层表面制造大孔层,既保证了层间结合强度,又在扩散层内形成梯度孔径;微孔结构有利于抑制膜电极表面气泡的聚集生长,大孔结构有利于液体由双极板侧向电极表面传输,两种孔结构结合促进气液质量传递,降低电解水制氢能耗。
附图说明
图1为具有梯度孔径的SPE电解槽用气体扩散层示意图。
其中,1-气体扩散层,2-微孔层,3-大孔层,4-催化层,5-双极板。
具体实施方式
为了更好的理解本发明,下面对本发明进行进一步详细描述。
一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)料液制备:以质量分数计,将65%~85%钛粉与10%~30%溶剂、1%~2%粘结剂和3%~4%增塑剂机械搅拌8~24h混合获得料液;其中,钛粉为球形雾化钛粉,钛粉粒径为30~80μm,溶剂为乙醇、甲苯或甲醇,粘结剂为聚乙烯醇缩丁醛(PVB)树脂或丙烯酸树脂,增塑剂为PEG400。
(2)流延成胚:将步骤(1)得到的料液在流延机内流延成型,流延速度为200~400mm/min,流延宽度为0.5~2m,流延厚度为200~800μm,获得平板状生胚;
(3)真空烧结:将步骤(2)得到的平板状生胚转移至真空炉中,进行程序升温烧结,程序升温烧结具体为:在Ar气流中由室温升温至400~500℃,压力为10~20mbar,保持恒温10~60min;在真空中继续升温至800~1200℃,真空度为10-4~10-5mbar,保持恒温120~240min;整个过程中升温速率为1~5℃/min,获得微孔扩散层;
(4)喷涂:通过真空等离子喷涂法在步骤(3)获得微孔扩散层上喷涂钛粉制备大孔扩散层,真空等离子喷涂法使用涂料为无规则形状的氢化脱氢钛粉,粉末粒径为100~200μm;等离子焓为10~20MJ/kg;喷涂速度为300~500mm/s;喷涂前基体预热至200~300℃;喷涂压力为30~50mbar;喷涂厚度为100~400μm,由此制得具有梯度孔径的SPE电解槽用气体扩散层。
下面结合实施例对本发明做进一步详细描述:
实施例1
本发明所述的具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)将质量分数为70%的粒径为45μm的球形雾化钛粉、25%的乙醇、1.2%的聚乙烯醇缩丁醛树脂和3.8%PEG400机械搅拌12h混合获得料液;
(2)将步骤(1)中料液在流延机内流延成型,流延速度为250mm/min,流延宽度为1m,流延厚度为400μm,获得平板状生胚;
(3)将步骤(2)中生胚转移至真空炉中,在Ar气流中以2℃/min速度由室温升温至500℃,压力为15mbar,保持恒温30min;停止通入Ar气流,在真空中继续以2℃/min速度升温至1000℃,真空度为10-5mbar,保持恒温120min;自然冷却后获得微孔扩散层;
(4)将步骤(3)获得微孔扩散层预热至250℃作为基体;采用真空等离子喷涂法将粒径为150μm的无规则形状的氢化脱氢钛粉喷涂在基体表面;等离子焓设定为10MJ/kg;喷涂速度为350mm/s;喷涂压力为50mbar;喷涂厚度为200μm;由此制得所述梯度孔径气体扩散层。
制备的梯度孔径气体扩散层1的微孔层2平均孔径为4.2μm,孔隙率为35%,大孔层3平均孔径为15.3μm,孔隙率为24%;商用气体扩散层平均孔径为10μm,孔隙率为30%。将自制的梯度孔径气体扩散层和商用气体扩散层分别安装在催化层4和双极板5之间,用于组装酸性质子交换膜电解槽进行电解制氢实验;在电流密度为2A/cm2条件下,装备自制梯度孔径气体扩散层的电解槽电解电压为1.92V,装备商用气体扩散层的电解槽电解电压为1.98V。
实施例2
本发明所述的具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)将质量分数为80%的粒径为35μm球形雾化钛粉、15%的乙醇、2%的聚乙烯醇缩丁醛树脂和3%PEG400机械搅拌16h混合获得料液;
(2)将步骤(1)中料液在流延机内流延成型,流延速度为200mm/min,流延宽度为2m,流延厚度为300μm,获得平板状生胚;
(3)将步骤(2)中生胚转移至真空炉中,在Ar气流中以2℃/min速度由室温升温至450℃,压力为20mbar,保持恒温45min;停止通入Ar气流,在真空中继续以2℃/min速度升温至950℃,真空度为10-4mbar,保持恒温150min;自然冷却后获得微孔扩散层;
(4)将步骤(3)获得微孔扩散层预热至200℃作为基体;采用真空等离子喷涂法将粒径为200μm的无规则形状的氢化脱氢钛粉喷涂在基体表面;等离子焓设定为12MJ/kg;喷涂速度为300mm/s;喷涂压力为50mbar;喷涂厚度为300μm;由此制得所述梯度孔径气体扩散层。
制备的梯度孔径气体扩散层1的微孔层2平均孔径为4.8μm,孔隙率为37%,大孔层3平均孔径为16.5μm,孔隙率为21%;商用气体扩散层平均孔径为10μm,孔隙率为30%。将自制的梯度孔径气体扩散层和商用气体扩散层分别用于组装酸性质子交换膜电解槽进行电解制氢实验;在电流密度为2A/cm2条件下,装备自制梯度孔径气体扩散层的电解槽电解电压为1.89V,装备商用气体扩散层的电解槽电解电压为1.98V。
实施例3
本发明所述的具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)将质量分数为80%的粒径为30μm球形雾化钛粉、15%的甲醇、1.0%的聚乙烯醇缩丁醛树脂和4.0%PEG400机械搅拌24h混合获得料液;
(2)将步骤(1)中料液在流延机内流延成型,流延速度为350mm/min,流延宽度为1.0m,流延厚度为600μm,获得平板状生胚;
(3)将步骤(2)中生胚转移至真空炉中,在Ar气流中以3℃/min速度由室温升温至475℃,压力为10mbar,保持恒温60min;停止通入Ar气流,在真空中继续以3℃/min速度升温至1200℃,真空度为10-5mbar,保持恒温120min;自然冷却后获得微孔扩散层;
(4)将步骤(3)获得微孔扩散层预热至275℃作为基体;采用真空等离子喷涂法将粒径为100μm的无规则形状的氢化脱氢钛粉喷涂在基体表面;等离子焓设定为18MJ/kg;喷涂速度为500mm/s;喷涂压力为45mbar;喷涂厚度为200μm;由此制得所述梯度孔径气体扩散层。
制备的梯度孔径气体扩散层1的微孔层2平均孔径为4.6μm,孔隙率为37%,大孔层3平均孔径为13.7μm,孔隙率为26%;商用气体扩散层平均孔径为10μm,孔隙率为30%。将自制的梯度孔径气体扩散层和商用气体扩散层分别安装在催化层4和双极板5之间,用于组装碱性阴离子交换膜电解槽进行电解制氢实验;在电流密度为2A/cm2条件下,装备自制梯度孔径气体扩散层的电解槽电解电压为2.05V,装备商用气体扩散层的电解槽电解电压为2.13V。
实施例4
本发明所述的具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)将质量分数为65%的粒径为80μm的球形雾化钛粉、30%的甲苯、1.5%的丙烯酸树脂和3.5%PEG400机械搅拌8h混合获得料液;
(2)将步骤(1)中料液在流延机内流延成型,流延速度为400mm/min,流延宽度为0.5m,流延厚度为800μm,获得平板状生胚;
(3)将步骤(2)中生胚转移至真空炉中,在Ar气流中以5℃/min速度由室温升温至400℃,压力为15mbar,保持恒温30min;停止通入Ar气流,在真空中继续以5℃/min速度升温至1000℃,真空度为10-5mbar,保持恒温120min;自然冷却后获得微孔扩散层;
(4)将步骤(3)获得微孔扩散层预热至300℃作为基体;采用真空等离子喷涂法将粒径为150μm的无规则形状的氢化脱氢钛粉喷涂在基体表面;等离子焓设定为10MJ/kg;喷涂速度为450mm/s;喷涂压力为50mbar;喷涂厚度为100μm;由此制得所述梯度孔径气体扩散层。
制备的梯度孔径气体扩散层1的微孔层2平均孔径为3.9μm,孔隙率为42%,大孔层3平均孔径为15.7μm,孔隙率为21%;商用气体扩散层平均孔径为10μm,孔隙率为30%。将自制的梯度孔径气体扩散层和商用气体扩散层分别安装在催化层4和双极板5之间,用于组装酸性质子交换膜电解槽进行电解制氢实验;在电流密度为2A/cm2条件下,装备自制梯度孔径气体扩散层的电解槽电解电压为1.90V,装备商用气体扩散层的电解槽电解电压为1.98V。
实施例5
本发明所述的具有梯度孔径的SPE电解槽用气体扩散层制备方法,包括以下步骤:
(1)将质量分数为85%的粒径为50μm的球形雾化钛粉、10%的乙醇、1.2%的丙烯酸树脂和3.8%PEG400机械搅拌12h混合获得料液;
(2)将步骤(1)中料液在流延机内流延成型,流延速度为250mm/min,流延宽度为1m,流延厚度为200μm,获得平板状生胚;
(3)将步骤(2)中生胚转移至真空炉中,在Ar气流中以1℃/min速度由室温升温至500℃,压力为15mbar,保持恒温10min;停止通入Ar气流,在真空中继续以1℃/min速度升温至800℃,真空度为10-5mbar,保持恒温240min;自然冷却后获得微孔扩散层;
(4)将步骤(3)获得微孔扩散层预热至250℃作为基体;采用真空等离子喷涂法将粒径为100μm的无规则形状的氢化脱氢钛粉喷涂在基体表面;等离子焓设定为20MJ/kg;喷涂速度为350mm/s;喷涂压力为30mbar;喷涂厚度为400μm;由此制得所述梯度孔径气体扩散层。
制备的梯度孔径气体扩散层1的微孔层2平均孔径为5.1μm,孔隙率为39%,大孔层3平均孔径为16.1μm,孔隙率为25%;商用气体扩散层平均孔径为10μm,孔隙率为30%。将自制的梯度孔径气体扩散层和商用气体扩散层分别安装在催化层4和双极板5之间,用于组装碱性阴离子交换膜电解槽进行电解制氢实验;在电流密度为2A/cm2条件下,装备自制梯度孔径气体扩散层的电解槽电解电压为2.01V,装备商用气体扩散层的电解槽电解电压为2.13V。
Claims (8)
1.一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,包括以下步骤:
(1)料液制备:将钛粉与溶剂、粘结剂和增塑剂机械搅拌混合获得料液;
(2)流延成胚:将步骤(1)得到的料液在流延机内流延成型,获得平板状生胚;
(3)真空烧结:将步骤(2)得到的平板状生胚转移至真空炉中,进行程序升温烧结,获得微孔扩散层;
(4)喷涂:通过真空等离子喷涂法在步骤(3)获得微孔扩散层上喷涂钛粉制备大孔扩散层,由此制得具有梯度孔径的SPE电解槽用气体扩散层。
2.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(1)中,钛粉为球形雾化钛粉,钛粉粒径为30~80μm。
3.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(1)中,溶剂为乙醇、甲苯或甲醇,粘结剂为聚乙烯醇缩丁醛树脂或丙烯酸树脂,增塑剂为PEG400。
4.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(1)中,钛粉质量分数为65%~85%,溶剂质量分数为10%~30%:粘结剂质量分数为1%~2%:增塑剂质量分数为3%~4%。
5.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(1)中,机械搅拌时间为8~24h。
6.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(2)中,流延成型时,流延速度为200~400mm/min,流延宽度为0.5~2m,流延厚度为200~800μm。
7.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(3)中,程序升温烧结具体为:在Ar气流中由室温升温至400~500℃,压力为10~20mbar,保持恒温10~60min;在真空中继续升温至800~1200℃,真空度为10-4~10-5mbar,保持恒温120~240min;整个过程中升温速率为1~5℃/min。
8.根据权利要求1所述的一种具有梯度孔径的SPE电解槽用气体扩散层制备方法,其特征在于,所述的步骤(4)中,真空等离子喷涂法使用涂料为无规则形状的氢化脱氢钛粉,粉末粒径为100~200μm;等离子焓为10~20MJ/kg;喷涂速度为300~500mm/s;喷涂前基体预热至200~300℃;喷涂压力为30~50mbar;喷涂厚度为100~400μm。
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