CN110942922A - 一步法合成多孔MnO/C微球用于超级电容器电极材料 - Google Patents
一步法合成多孔MnO/C微球用于超级电容器电极材料 Download PDFInfo
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Abstract
本专利涉及一种用于超级电容器电极材料的碳负载氧化锰的制备方法，针对实施例1附图2中的产物形貌，所得的MnO/C电极材料是具有许多纳米颗粒包覆构成的多孔微球结构，构成多孔微球结构的纳米微球直径约为2.5μm，电化学测试结果表明，在电流密度为0.1 A·g‑1时，单电极的比容量达到104.9 mAh·g‑1，当电流密度为1 A·g‑1时，经过500次循环充放电，电极比容量的保持率为96.4%。
Description
技术领域
本发明属于超级电容器器件技术领域，具体涉及一步法合成多孔MnO微球用于超级电容器电极材料。
背景技术
随着人类对能源的需求，科学家开发了各种先进的能量转换和存储装置，如锂离子电池、燃料电池和超级电容器。在各种类型的储能设备中，电化学超级电容器，引起了广泛的关注。超级电容器具有寿命长、充放电速度快、功率密度高等优点具有许多潜在的应用前景，其中电极材料是影响性能的关键，具有赝电容特性的金属氧化物已其价格低廉、自然丰度高、环境友好、理论比容量高等优点成为最近研究的热点，其中RuO2电极材料的比电容可达788 F/g。但是由于材料价格过高，应用受到严重限制。
Mn系氧化物具有自然含量丰富及价格较低、环保友好等优点，有望替代RuO2成为新型赝电容电极材料。其中二价锰系氧化物的开发在国内刚刚起步，Wang 等人采用一种简单的凝胶状薄膜辅助法，在碳布上制备了平均粒径为80、41、20、15和9 nm的均匀可调的MnO颗粒并探索出中等粒径的纳米粒子(20 nm)表现出最好的性能，而且优化后的MnO/碳布电极具有良好的柔韧性和较高的导电性与稳定性，在功率密度可达到450 W/kg。尽管如此，锰氧化物材料存在利用率低，离子/电子导电性差，小颗粒的团聚易造成低比表面积等缺陷。为解决上述问题，一种有效的策略是利用碳质基体构建纳米复合材料，可以大大改善材料的导电特性，降低内阻，从而提高电容性能。
申请公开号为CN201610470858.3的发明专利公开一种利用激光一步原位还原氧化石墨烯、分解锰化合物制备石墨烯/氧化锰柔性电极的方法，具体公开了将氧化石墨烯的水溶液与锰的氧化物均匀混合，涂布在柔性基底上，在惰性气氛保护下利用激光照射，使氧化石墨烯被激光还原成石墨烯的同时,锰化合物受热分解得到氧化锰材料。上述专利的目的都在于提高锰氧化物材料的比容量，但制备的方法复杂，所得产物比表面积受限等缺陷仍是限制高性能电极材料进一步应用的关键。本发明以多巴胺为碳源，一步实现锰前驱体碳酸锰和聚多巴胺的合成，并经过惰性气体N2保护下，煅烧实现碳掺杂的MnO的制备。
发明内容
本发明以MnSO4为锰源，以NaHCO3为沉淀剂，室温下快速合成MnCO3，通过多巴胺的修饰高温煅烧碳化得到MnO/C多孔分级结构微球，制备的MnO/C应用于超级电容器电极材料，为二价锰材料应用于超级电容器电极提供数据和制备方法。
为解决上述技术问题，本发明采取如下技术方案：本发明的基于一种用于超级电容器电极材料的碳负载氧化锰的制备方法，具体包括如下步骤：（1）将0.75 mmol MnSO4溶于70 mL 蒸馏水和7 mL 无水乙醇混合溶液中，加入0.03 g多巴胺（DA）溶解，将10 mmol/L三羟甲基氨基甲烷（Tris-buffer）逐滴加入上述混合溶液中，磁力搅拌均匀后，将7.8 mmolNaHCO3溶于70 mL 蒸馏水后缓慢加入到上述溶液中反应3 h。得到溶液离心分离后用蒸馏水、乙醇洗涤，干燥后得MnCO3/PDA。
（2）将MnCO3/PDA粉末转移至高温管式炉内，在氮气保护下，进行煅烧碳化，升温速率为5 ℃/min下煅烧2 h，得到MnO/C多孔微球复合材料。
所得的MnO/C多孔微球粒径为0.8-1 µm，由50-70 nm的纳米颗粒构成，表面粗糙，且颗粒间有明显的空隙和孔道，有利于电解液的渗透和内部材料的充分利用，电化学测试结果表明，在电流密度为0.1 A·g-1时，单电极比容量达到104.9 mAh·g-1，当电流密度为1A·g-1时，经过500次循环充放电，电极比容量的保持率为96.4 %。
附图说明
图1是实施例1中所制备的MnO/C材料XRD曲线。
图2是实施例1中所制备的MnO/C材料扫描电镜照片。
图3是实施例1中所制备的MnO/C材料扫描电镜的放大照片。
图4是实施例1中所制备的MnO/C材料不同扫描速率的循环伏安曲线。
图5是实施例1中所制备的MnO/C材料不同电流密度的充放电曲线。
具体实施方式
下面结合实施例对本发明的技术方案及效果作进一步描述。但是，所使用的具体方法、配方和说明并不是对本发明的限制。
实施例1：将0.75 mmol MnSO4溶于70 mL 蒸馏水和7 mL 无水乙醇混合溶液中，加入0.03 g多巴胺溶解，将10 mmol/L Tris-buffer逐滴加入上述混合溶液中，磁力搅拌均匀后，将7.8 mmol NaHCO3溶于70 mL 蒸馏水后缓慢加入到上述溶液中反应3 h。得到溶液离心分离后用蒸馏水、乙醇洗涤，干燥后得MnCO3/PDA；将MnCO3/PDA粉末转移至高温管式炉内，在氮气保护下，进行600 ℃高温煅烧碳化，升温速率为5 ℃/min下煅烧2 h，得到MnO/C多孔微球复合材料。
实施例2：将0.75 mmol MnSO4溶于70 mL 蒸馏水和7 mL 无水乙醇混合溶液中，加入0.03 g多巴胺溶解，将10 mmol/L Tris-buffer逐滴加入上述混合溶液中，磁力搅拌均匀后，将7.8 mmol NaHCO3溶于70 mL 蒸馏水后缓慢加入到上述溶液中反应3 h。得到溶液离心分离后用蒸馏水、乙醇洗涤，干燥后得MnCO3/PDA；将MnCO3/PDA粉末转移至高温管式炉内，在氮气保护下，进行800 ℃高温煅烧碳化，升温速率为5 ℃/min下煅烧2 h，得到MnO/C多孔微球复合材料。
实施例3：将0.75 mmol MnSO4溶于70 mL 蒸馏水和7 mL 无水乙醇混合溶液中，加入0.04 g多巴胺溶解，将10 mmol/L Tris-buffer逐滴加入上述混合溶液中，磁力搅拌均匀后，将7.8 mmol NaHCO3溶于70 mL 蒸馏水后缓慢加入到上述溶液中反应3 h。得到溶液离心分离后用蒸馏水、乙醇洗涤，干燥后得MnCO3/PDA；将MnCO3/PDA粉末转移至高温管式炉内，在氮气保护下，进行600 ℃高温煅烧碳化，升温速率为5 ℃/min下煅烧2 h，得到MnO/C多孔微球复合材料。
实施例4：将0.75 mmol MnSO4溶于70 mL 蒸馏水和7 mL 无水乙醇混合溶液中，加入0.03 g多巴胺溶解，将10 mmol/L Tris-buffer逐滴加入上述混合溶液中，磁力搅拌均匀后，将7.8 mmol NaHCO3溶于70 mL 蒸馏水后缓慢加入到上述溶液中反应2 h。得到溶液离心分离后用蒸馏水、乙醇洗涤，干燥后得MnCO3/PDA；将MnCO3/PDA粉末转移至高温管式炉内，在氮气保护下，进行600 ℃高温煅烧碳化，升温速率为5 ℃/min下煅烧2 h，得到MnO/C多孔微球复合材料。
实施例5：将0.65 mmol MnSO4溶于70 mL 蒸馏水和7 mL 无水乙醇混合溶液中，加入0.03 g多巴胺溶解，将10 mmol/L Tris-buffer逐滴加入上述混合溶液中，磁力搅拌均匀后，将6.8 mmol NaHCO3溶于70 mL 蒸馏水后缓慢加入到上述溶液中反应3 h。得到溶液离心分离后用蒸馏水、乙醇洗涤，干燥后得MnCO3/PDA；将MnCO3/PDA粉末转移至高温管式炉内，在氮气保护下，进行600 ℃高温煅烧碳化，升温速率为5 ℃/min下煅烧2 h，得到MnO/C多孔微球复合材料。
Claims (2)
1.一种用于超级电容器电极材料的碳负载氧化锰材料，其特征在于，所述电极材料以多巴胺为碳源，一步实现锰前驱体碳酸锰和聚多巴胺的合成，并经过惰性气体N2保护下，煅烧实现碳掺杂的MnO的制备，所得的MnO/C多孔微球粒径为0.8-1 µm，由50-70 nm的纳米颗粒构成，表面粗糙，且颗粒间有明显的空隙和孔道。
2.一种用于超级电容器电极材料的碳负载氧化锰的制备方法，其特征在于，包括如下步骤：将0.169 g的MnSO4溶于70 mL蒸馏水与7 mL乙醇的混合溶液中，充分溶解后加入15-30 mg DA,再加入Tris溶液（0.093 g,500μL蒸馏水），搅拌30 min，将0.84 g NaHCO3加入70mL 蒸馏水，待充分溶解后，缓慢加入至上述溶液中，50℃下磁力搅拌3 h(300r)，用蒸馏水和乙醇分别洗涤3次，60℃干燥，得到MnO粉末，在管式炉内600-800℃氮气保护下退火2h，得到MnO/C电极材料，利用MnO/C微球型多孔结构，提升离子传输速率，来实现电极材料的高电化学性能。
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