CN107032312B - 一种多孔CoP电极材料的制备方法 - Google Patents
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
本发明涉及一种多孔CoP电极材料的制备方法,包括:将Co(NO3)2·6H2O,CO(NH2)2和NH4F溶解于去离子水中并充分搅拌,得到混合溶液;将上述混合溶液加入反应釜中并放入基底材料,在90‑150℃水热条件下反应3‑12h,冷却至室温,洗涤,干燥,得到长有前驱体的基底材料,然后和NaH2PO2进行煅烧,即得。本发明所制备的多孔CoP电极材料展现出优异的电化学性能,具有实际应用前景。
Description
技术领域
本发明属于电极材料的制备领域,特别涉及一种多孔CoP电极材料的制备方法。
背景技术
随着全球经济的快速发展、化石能源的不断消耗、环境污染的日益严重,研究一种高效、低成本、环境友好、高性能的能源转换和储存系统已经显得越来越重要。超级电容器由于具有高的功率密度,快速充放电速率和长的循环寿命等优点而被认为是最有前景的下一代能量转换和储存设备。研究表明,电极材料是决定超级电容器性能的关键因素之一。因此,开发新型高性能电极材料对于提高超级电容器的性能显得尤为必要。过渡金属磷化物由于具有金属特性、超高的电导率和高的比电容而受到广大科研人员的关注。本发明制备了多孔CoP电极材料,展现出优异的电化学性能,具有很重要的应用前景。
发明内容
本发明所要解决的技术问题是提供一种多孔CoP电极材料的制备方法,本发明所制备的CoP电极材料面积比电容高达1.89F/cm2,经过4000次循环测试比电容只有~3%损失,而且具有较高的库伦效率。
本发明的一种多孔CoP电极材料的制备方法,包括:
(1)将Co(NO3)2·6H2O,CO(NH2)2和NH4F溶解于去离子水中并充分搅拌,得到混合溶液;其中Co(NO3)2·6H2O、CO(NH2)2、NH4F的摩尔比为1-5:5-20:1-10;
(2)将上述混合溶液加入反应釜中并放入基底材料,反应釜放入鼓风干燥箱中,90-150℃水热条件下反应3-12h,冷却反应釜至室温,洗涤,干燥,得到长有前驱体的基底材料;
(3)将上述长有前驱体的基底材料和NaH2PO2进行煅烧,即得多孔CoP电极材料。优选步骤(1)中Co(NO3)2·6H2O摩尔量为1-5mmol,CO(NH2)2摩尔量为5-20mmol和NH4F摩尔量为1-10mmol。
所述步骤(2)中反应釜为聚四氟乙烯水热反应釜。
所述步骤(2)中基底材料为碳布、碳纸、泡沫镍、钛片中的一种。
所述步骤(2)中基底材料为清洗过的基底材料。
所述步骤(2)中洗涤为用去离子水和乙醇洗涤。
步骤(1)中的Co(NO3)2·6H2O和步骤(3)中NaH2PO2的比例为1-5mmol:5-100mg。
所述步骤(3)中NaH2PO2质量为5-100mg。
所述步骤(3)中煅烧为:管式炉中煅烧,煅烧温度为200-500℃,煅烧时间为60-300min。
有益效果
本发明所制备的CoP电极材料面积比电容高达1.89F/cm2,经过4000次循环测试比电容只有~3%损失,而且具有较高的库伦效率;
本发明所制备的多孔CoP电极材料展现出优异的电化学性能,具有实际应用前景。
附图说明
图1是本发明中实施例1制备的多孔CoP材料的扫描电镜(a,b)和透射电镜图(c,d);
图2是本发明中实施例1制备的多孔CoP电极材料的循环伏安(a),充放电(b),面积比电容(c)和循环稳定性和库伦效率(d)
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
1)称取2mmol Co(NO3)2·6H2O,10mmol CO(NH2)2和5mmol NH4F溶解于去离子水中并充分搅拌。
2)将上述混合溶液倒入聚四氟乙烯水热反应釜中并放入一块已经清洗过的碳布,将反应釜放入鼓风干燥箱中,120℃水热条件下反应5小时,反应结束后冷却反应釜至室温,并取出长有前驱体的基底材料,分别用去离子水和乙醇溶剂洗涤,并干燥。
3)将上述制备的材料和NaH2PO2(10mg)置于管式炉中煅烧,煅烧温度为300℃,煅烧时间为120分钟,保护气体为氩气。
对附图1材料的形貌及大小进行描述;对附图2中电化学性能进行分析说明。图一表明所制备的CoP纳米线长度约为3-8μm,且为多孔结构。电化学测试结果表明,该电极材料的面积比电容为1.89F/cm2,经过4000次循环测试后比电容仅下降~3%。
实施例2
1)称取1mmolCo(NO3)2·6H2O,5mmol CO(NH2)2和2.5mmol NH4F溶解于去离子水中并充分搅拌。
2)将上述混合溶液倒入聚四氟乙烯水热反应釜中并放入一块已经清洗过的碳布,将反应釜放入鼓风干燥箱中,120℃水热条件下反应5小时,反应结束后冷却反应釜至室温,并取出长有前驱体的基底材料,分别用去离子水和乙醇溶剂洗涤,并干燥。
3)将上述制备的材料和NaH2PO2(100mg)置于管式炉中煅烧,煅烧温度为300℃,煅烧时间为120分钟,保护气体为氩气。
Claims (5)
1.一种多孔CoP电极材料的制备方法,包括:
(1)将Co(NO3)2·6H2O,CO(NH2)2和NH4F溶解于去离子水中并充分搅拌,得到混合溶液;其中Co(NO3)2·6H2O、CO(NH2)2、NH4F的摩尔比为2:10:5;
(2)将上述混合溶液加入反应釜中并放入基底材料,反应釜放入鼓风干燥箱中, 90-150℃水热条件下反应3-12h,冷却至室温,洗涤,干燥,得到长有前驱体的基底材料;其中基底材料为碳布;
(3)将上述长有前驱体的基底材料和NaH2PO2进行煅烧,即得多孔CoP电极材料;其中制备得到的CoP纳米线长度为3 - 8 μm;其中步骤(1)中Co(NO3)2·6H2O和步骤(3)中NaH2PO2的比例为2 mmol:10 mg;其中煅烧为:保护气体条件下,管式炉中煅烧,煅烧温度为200-500℃,煅烧时间为60-300min。
2.根据权利要求1所述的一种多孔CoP电极材料的制备方法,其特征在于:所述步骤(2)中反应釜为聚四氟乙烯水热反应釜。
3.根据权利要求1所述的一种多孔CoP电极材料的制备方法,其特征在于:所述步骤(2)中基底材料为清洗过的基底材料。
4.根据权利要求1所述的一种多孔CoP电极材料的制备方法,其特征在于:所述步骤(2)中洗涤为用去离子水和乙醇洗涤。
5.根据权利要求1所述的一种多孔CoP电极材料的制备方法,其特征在于:所述步骤(3)中保护气体为氩气。
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CN109821561A (zh) * | 2019-03-22 | 2019-05-31 | 黑龙江大学 | 一种自支撑磷化钴铁纳米微球电催化剂的制备方法 |
CN111060575A (zh) * | 2019-12-25 | 2020-04-24 | 广州钰芯传感科技有限公司 | 一种用于葡萄糖无酶检测的多孔Co-P复合电极及其制备方法与应用 |
CN112044458B (zh) * | 2020-08-21 | 2021-07-20 | 广东工业大学 | 一种多层级金属磷化物及其制备方法和应用 |
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CN104941674A (zh) * | 2015-06-18 | 2015-09-30 | 西南大学 | 一种活性炭上负载磷化钴的催化剂及其制备方法和应用 |
CN105403606A (zh) * | 2015-11-10 | 2016-03-16 | 西安建筑科技大学 | 一种基于磷化钴/血红蛋白修饰的碳布电极的制备方法 |
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KR20120100108A (ko) * | 2011-03-03 | 2012-09-12 | 성균관대학교산학협력단 | CoP 합금 박막의 제조방법 및 수직자기 기록매체 |
CN104941674A (zh) * | 2015-06-18 | 2015-09-30 | 西南大学 | 一种活性炭上负载磷化钴的催化剂及其制备方法和应用 |
CN105403606A (zh) * | 2015-11-10 | 2016-03-16 | 西安建筑科技大学 | 一种基于磷化钴/血红蛋白修饰的碳布电极的制备方法 |
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