CN107138172A - 一种电极催化材料的制备方法及其在葡萄糖燃料电池中的应用 - Google Patents
一种电极催化材料的制备方法及其在葡萄糖燃料电池中的应用 Download PDFInfo
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Abstract
本发明公布了一种电极催化材料的制备方法,即一种氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的碳材料。将单氰胺(CN2H2)和六水合硝酸钴(Co(NO3)2.6H2O)混合均匀后进行固‑固反应,制得一种膨松的前驱体,再将前驱体进行高温碳化,得到最终的电极催化材料。单氰胺既是碳源,也是氮源。本发明的优点是:将单氰胺在反应中分解产生的气体作为气体模板构建出三维多孔碳结构,这种三维结构促进了质子和电子的传导效率,石墨化的碳增强了其导电性。该制备方法制备工艺简易,该电极的制备工艺具有潜在应用价值。将这种氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的碳材料分别制备成葡萄糖燃料电池阴极和阳极的催化电极,来催化阴阳极电极反应,从而使其自发进行,带动外加负荷对外输出电能。
Description
技术领域
本发明属于利用一种氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的电极催化材料的制备,以及在葡萄糖燃料电池中的应用。
背景技术
最近几十年中,随着全球环境问题日益突出以及能源危机的加剧,寻找高效率、低成本、清洁的能源转换体统成为了人们的迫切需要。由于燃料电池具有能量转换效率高,反应温度低、产物低污染等优点,因而燃料电池极有可能成为解决环境、能源问题的一种途径。[2]而氧还原是燃料电池技术的核心关键,燃料电池阴极氧还原动力学缓慢,这就限制了燃料电池技术的提高。[3]铂以及铂合金是目前性能最好的氧还原催化剂,但铂金属价格昂贵,且稀缺,加上铂催化剂稳定性差,抗甲醇性能差等缺点使得燃料电池的应用进一步受到了限制,这就需要研究出价格低廉的高活性非贵金属或非金属催化剂来代替铂基催化剂。
多孔碳材料具有较高的比表面积、较好的导电性、高的化学稳定性,且杂原子(例如:N,B,P,S等)掺杂纳米结构碳材料,具有突出的氧还原催化活性,尤其是氮掺杂纳米结构碳材料是其中催化活性最好的。近年来碳材料被广泛研究。最近,多孔碳基负载复合纳米结构过度金属(例如:Co,Fe,Ni等)这类材料,由于协同效应使得整体性能大弧度提高,所以这类材料极有可能代替Pt基催化剂,成为最佳商用氧还原催化剂。
为了进一步提高ORR催化材料的性能,我们发明了一种氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的电极催化材料。大量的Co纳米粒子较均一地修饰在碳纳米片表面,Co纳米粒子负载在高导电性的石墨化碳纳米片上,提高了整体材料的导电性和质荷传导率。这种Co, N双参杂的协同效应,很大程度上提高了材料的催化活性和稳定性。且这种Co,N双掺杂三维多孔碳材料,具有较大的比表面积,提高了大量的活性位点,这有利于改善电催化氧还原反应和葡萄糖氧化反应的催化活性,并有着优异的电催化氧还原和葡萄糖氧化 性能。
发明内容
一种电极催化材料的制备方法及其在燃料电池中的应用,所述电极催化材料为多孔氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的电极催化材料,利用单氰胺作为碳和氮源。其制备方法和在燃料电池中的应用包括以下三个步骤:
1)前驱体材料的制备;将2.37g的Co(NO3)2.6H2O和1.15g的CH2N2碾磨10min, 使其充分混合均匀,再将碾磨后所得的粘稠液倒入烧杯中加热至120°C反应5小时。将所得的蓬松固体碾磨成粉末样品待用;
2)Co/N-MC-750材料的制备;将上述所得的前驱体粉末固体至于管式炉中,惰性气体氛围下高温碳化。将蓬松的黑色固体碾磨成粉末,制备成粉末样。
3)葡萄糖燃料电池的应用: Co/N-MC-750催化材料制备成浆液(水, Naion(5%),乙醇的体积比为420:50:30),将制成的浆液按照2mg/cm2涂在用钛丝串好的碳布上,分别放入葡萄糖燃料电池的阴阳极,外串联一个外加负载,用数据采集仪采集外加负载上的电压。(图5)
步骤(1)中采用的是固态的CN2H2, Co(NO3)2.6H2O与CN2H2质量分数分别为99.9%、95%。
步骤(1)中Co(NO3)2.6H2O与CN2H2两者的质量比为5:4。
步骤(2)中惰性气体为Ar气或者N2。
步骤(2)中碳化温度为750℃,碳化时间为5h。
步骤(2)中CN2H2即作为碳源,又作为氮源。
步骤(2)中CN2H2在低温下聚合的聚合物分解出的气体充当模板,从而形成三维结构的多孔碳纳米片。
步骤(3)中浆液的浓度为10mg/ml。
步骤(3)中外加负荷电阻为150Ω。
本发明的优点是:将单氰胺在反应中分解产生的气体作为气体模板构建出三维多孔碳结构,这种三维结构促进了质子和电子的传导效率,石墨化的碳增强了其导电性。这种碳纳米材料对ORR和GOR都具有非常突出的催化性能,且将这种材料分别作为葡萄糖燃料电池的阴阳极催化电极,能使葡萄糖燃料电池阴极和阳极自发进行反应,带动外加负荷对外输电能。该材料的制备方法制备工艺简易,该电极的制备工艺具有潜在应用价值。
附图说明
图1是本发明Co/N-MC-750材料的XRD图。
图2是本发明Co/N-MC-750材料扫描电镜图。
图3是本发明Co/N-MC-750材料与20% Pt/C氧还原性能对比图。
图4是本发明Co/N-MC-750材料对葡萄糖电流响应效果图。
图5是本发明Co/N-MC-750材料组装成葡萄糖燃料电池的实物图
图6是本发明Co/N-MC-750材料组装成葡萄糖燃料的循环图。
具体实施方式
下面结合附图并通过实施例对本发明作进一步说明,但需要说明的是实施例并不构成对本发明要求保护范围的限定。
实施案例
1. 前驱体材料的合成:将2.37g的Co(NO3)2.6H2O和1.15g的CH2N2碾磨10min, 使其充分混合均匀,再将碾磨后所得的粘稠液倒入烧杯中加热至120°C反应5小时。将所得的蓬松固体碾磨成粉末样品待用。
2.Co/N-MC-750材料的合成:将上述所得的前驱体粉末固体至于管式炉中,于Ar气体氛围下,750°C高温下碳化5h。将蓬松的黑色固体碾磨成粉末,制备成Co/N-MC-750粉末样。
3. 将5mg制得的Co/N-MC-750粉末材料溶于乙醇和Nafion的混合水溶液(乙醇、Nafion溶液和去离子水的体积比为1:1:8)制成浆液涂到玻碳电极或旋转圆盘上,在0.1MKOH的溶液中进行电化学氧还原和葡萄氧化测试,测试的氧还原结果与商用20%的Pt/C作比较,结果如图3所示。
4. 上诉所制得的浆液取100ul涂在碳布上,自然晾干后制成葡萄糖燃料电池的电极材料,组装成燃料电池,如图5。
Claims (8)
1.一种电极催化材料的制备方法,所述电极催化材料为多孔氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的电极催化材料,利用单氰胺作为碳和氮源,包括以下两个步骤:
1)前驱体材料的制备;将2.37g的Co(NO3)2.6H2O和1.15g的CH2N2碾磨10min, 使其充分混合均匀,再将碾磨后所得的粘稠液倒入烧杯中加热至120°C反应5小时;将所得的蓬松固体碾磨成粉末样品待用;
2)Co/N-MC-750材料的制备;将上述所得的前驱体粉末固体至于管式炉中,惰性气体氛围下高温碳化;将蓬松的黑色固体碾磨成粉末,制备成粉末样。
2.根据权利要求1所述的一种电极催化材料的制备方法,其特征在于:步骤(1)中采用的是固态的CN2H2, Co(NO3)2.6H2O与CN2H2质量分数分别为99.9%、95%。
3.根据权利要求1所述的一种电极催化材料的制备方法,其特征在于:步骤(1)中Co(NO3)2.6H2O与CN2H2两者的质量比为5:4。
4.根据权利要求1所述的一种电极催化材料的制备方法,其特征在于:步骤(2)中惰性气体为Ar气或者N2。
5.根据权利要求1所述的一种电极催化材料的制备方法,其特征在于:步骤(2)中碳化温度为750℃,碳化时间为5h。
6.根据权利要求1所述的一种电极催化材料的制备方法,其特征在于:步骤(2)中CN2H2即作为碳源,又作为氮源。
7.根据权利要求1所述的一种电极催化材料的制备方法,其特征在于:步骤(2)中CN2H2在低温下聚合的聚合物分解出的气体充当模板,从而形成三维结构的多孔碳纳米片。
8.根据权利要求1所述所制备的氮参杂碳纳米片包覆Co纳米粒子的三维多孔纳米结构的碳材料,其特征在于:将其分别制备成葡萄糖燃料电池阴极和阳极的催化电极,来催化阴阳极电极反应,能使葡萄糖燃料电池阴极和阳极自发进行反应,带动150Ω的外加负荷,对外输出的最高电流密度可达0.65 mA/cm2。
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