CN113789663A - 一种n,f掺杂碳材料双功能“一体式”催化剂的制备方法与应用 - Google Patents

一种n,f掺杂碳材料双功能“一体式”催化剂的制备方法与应用 Download PDF

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CN113789663A
CN113789663A CN202110964248.XA CN202110964248A CN113789663A CN 113789663 A CN113789663 A CN 113789663A CN 202110964248 A CN202110964248 A CN 202110964248A CN 113789663 A CN113789663 A CN 113789663A
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王春莲
陈继民
袁艳萍
周堃
董国臣
相世博
郭馨阳
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Beijing University of Technology
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Abstract

一种N,F掺杂碳材料双功能“一体式”催化剂的制备方法与应用属于制备合成技术领域。本发明以飞秒激光辐照微加工技术，通过飞秒激光辐照在复合碳布上制备一种杂元素掺杂的碳膜，用于锌空气电池正极氧气反应催化剂。本发明作为锌‑空气电池正极催化剂的全电池循环性能优良。

Description

一种N,F掺杂碳材料双功能“一体式”催化剂的制备方法与 应用
技术领域
本发明设计一种锌空气电池正极用N,F掺杂双功能“一体式”催化剂的制备方法，以飞秒激光辐照微加工技术，通过飞秒激光辐照在复合碳布上制备一种杂元素掺杂的碳膜，用于锌空气电池正极氧气反应催化剂。本发明提供一种杂元素掺杂碳简便的制备方法，属于制备合成技术领域。
背景技术
随着经济水平的不断发展，全球对于能源的需求量越来越多，煤炭石油天然气等不可再生资源的全球储量日益减少，开发安全可靠清洁可二次使用的能源成为全球人民面临的重大难题。可充电电池成为解决这个难题的有效措施，其中锌空气电池，由于锌储量比较大且正极活性物质是空气中的氧气成为有潜力的能源储备。其中锌空气电池正极氧气反应是制约锌空气全电池性能的重要因素，在电池充放电的过程中伴随着的氧气的氧化反应和氧气析出反应直接影响电池的循环性能的放电性能，因此开发高效清洁的催化剂是发展锌空气电池的必须解决的问题之一。组成、形貌以及制备方法各异的清洁催化剂，各式各样的碳材料由于其较高的比表面积、催化活性、无毒无害等优点成为锌空气电池正价催化剂的研究热点。但是，碳材料传统的制备方法是基于化学法，制备过程繁琐而且涉及不同的化学试剂，影响了它的大规模制备与应用。激光先进制造是上个世纪伴随着激光技术的日益成熟而产生的高效简便的材料加工制备工艺，依托激光的优点，激光制造技术成为传统物理方法或者化学方法无法达到的水平，可操作性强、不受加工件尺寸与形状影响、加工精度高等优点。飞秒激光属于超短脉冲激光，在加工制造领域更是收到了很大的青睐。利用飞秒激光辐照技术制备碳材料，可以实现一步完成，而且单纯通过调节激光能量可以实现对碳材料成分的调控，从而实现对锌空气电池正极催化性能的调控。因此，本文利用飞秒激光辐照技术制备“一体式”N,F掺杂的双功能碳膜的催化剂。
发明内容
本发明通过飞秒激光辐照技术制备“一体式”N,F双掺杂掺杂的双催化功能碳膜的催化剂。本发明技术的方案如下：
一种N,F掺杂碳材料双功能“一体式”催化剂的制备方法，其特征在于，包括以下步骤：
(1)用天平称取0.01-1.01g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入0.01-10.01mL的N-甲基吡咯烷酮溶液；
(3)在转速是100-5000r/min下持续搅拌0.01-3.0h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是1-500μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干0.3-3h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在1-1000Hz，功率在1-100mW的激光光源，在三轴联动的位移台以加工速度是0.01-10mm/s完成加工的；即可得到N，F掺杂的碳材料；
(8)将步骤(7)得到碳布裁剪成作为锌-空气电池正极材料组装全电池测试电化学性能。
作为优选，步骤(1)称取聚偏氟乙烯乙烯粉末质量为0.1-0.3g；
作为优选，步骤(2)加入N-甲基吡咯烷酮溶液的体积是1-3mL；
作为优选，步骤(3)搅拌过程中转速是2000r/min，搅拌时间是1h；
作为优选，步骤(4)涂覆层的厚度是100-200μm；
作为优选，步骤(7)重复频率是1000Hz，功率是30-40mW。
附图说明
图1不同激光功率加工的碳扫描图。
图2N,F掺杂碳的XPS结果图。
图3N,F掺杂碳作为锌-空气电池正极催化剂的全电池循环性能图。
图4N,F杂掺杂碳作为锌-空气电池正极催化剂的全电池循环性能图。图5N,F双元素掺杂碳作为锌-空气电池正极催化剂的全电池循环性能图。
具体实施方式
结合附图，分别对步骤中的各个参数进行优选，具体实施案例如下：
实施案例1
(1)用天平称取0.1g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入1mL的N-甲基吡咯烷酮溶液；
(3)在转速是1000r/min下持续搅拌0.5h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是50μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干0.3h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在1000Hz，功率在20mW的激光光源，在三轴联动的位移台以加工速度是0.1mm/s完成加工的；即可得到N，F掺杂的碳材料；
(8)将步骤(7)得到碳布裁剪作为锌-空气电池正极材料组装全电池测试电化学性能。
实施案例2
(1)用天平称取0.2g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入2mL的N-甲基吡咯烷酮溶液；
(3)在转速是2000r/min下持续搅拌1h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是100μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干0.5h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在800Hz，功率在30mW的激光光源，在三轴联动的位移台以加工速度是0.5mm/s完成加工的；即可得到N，F掺杂的碳材料；
(8)将步骤(7)得到碳布裁剪作为锌-空气电池正极材料组装全电池测试电化学性能。
实施案例3
(1)用天平称取0.4g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入4mL的N-甲基吡咯烷酮溶液；
(3)在转速是3000r/min下持续搅拌2.0h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是200μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干1h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在1000Hz，功率在40mW的激光光源，在三轴联动的位移台以加工速度是1mm/s完成加工的；即可得到N，F掺杂的碳材料；
(8)将步骤(7)得到碳布裁剪作为锌-空气电池正极材料组装全电池测试电化学性能。
实施案例4
(1)用天平称取0.5g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入5mL的N-甲基吡咯烷酮溶液；
(3)在转速是2500r/min下持续搅拌2.5h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是300μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干2h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在200Hz，功率在50mW的激光光源，在三轴联动的位移台以加工速度是2mm/s完成加工的；即可得到N，F掺杂的碳材料；
(8)将步骤(7)得到碳布裁剪作为锌-空气电池正极材料组装全电池测试电化学性能。
实施案例5
(1)用天平称取0.6g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入6mL的N-甲基吡咯烷酮溶液；
(3)在转速是1500r/min下持续搅拌3.0h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是500μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干3h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在1000Hz，功率在120mW的激光光源，在三轴联动的位移台以加工速度是5mm/s完成加工的；即可得到N，F掺杂的碳材料；
(8)将步骤(7)得到碳布裁剪作为锌-空气电池正极材料组装全电池测试电化学性能。

Claims (7)

1.一种N,F掺杂碳材料双功能“一体式”催化剂的制备方法，其特征在于，包括以下步骤：
(1)用天平称取0.01-1.01g的聚偏氟乙烯粉末，放入烧杯中；
(2)向步骤(1)烧杯中加入0.01-10.01mL的N-甲基吡咯烷酮；
(3)在转速是100-5000r/min下持续搅拌0.01-3.0h直至混合均匀得到透明的粘稠状分散体系；
(4)在洁净的玻璃板上粘附一层疏水碳布，后将步骤(3)得到的粘稠状分散体系用涂覆工具均匀涂覆在碳布上，形成涂层厚度是1-500μm厚度的涂覆层；
(5)将步骤(4)得到的有涂覆层的碳布在50℃的恒温烘箱中烘干0.3-3h直至液体完全挥发得到干燥的碳布；
(6)用裁纸刀选取步骤(5)中均匀的碳布，粘在载玻片上；
(7)利用波长是800nm，脉宽是35fs，重复频率在1-1000Hz，功率在1-100mW的激光光源，在三轴联动的位移台以加工速度是0.01-10mm/s完成加工得到催化剂。
2.如权利要求1所述的方法，其特征在于，步骤(1)称取聚偏氟乙烯乙烯粉末质量为0.1-0.3g。
3.如权利要求1所述的方法，其特征在于，步骤(2)加入N-甲基吡咯烷酮溶液的体积是1-3mL。
4.如权利要求1所述的方法，其特征在于，步骤(3)搅拌过程中转速是2000r/min，搅拌时间是1h。
5.如权利要求1所述的方法，其特征在于，步骤(4)涂覆层的厚度是100-200μm。
6.如权利要求1所述的方法，其特征在于，步骤(7)重复频率是1000Hz，功率是30-40mW。
7.应用如权利要求1所述的方法所制备的一种N,F掺杂碳材料双功能“一体式”催化剂在锌空气电池的中的应用。
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JP2011255336A (ja) * 2010-06-10 2011-12-22 Toyota Motor Corp 触媒担持担体の製造方法および電極触媒の製造方法
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