CN107705999A - 金属氧化物核壳纳米片阵列电极材料的制备方法 - Google Patents
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 17
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical class [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 7
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G11/46—Metal oxides
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Abstract
本专利涉及金属氧化物核壳纳米片阵列电极材料的制备方法,所得的四氧化三钴纳米片骨架具有较好的平行多层结构和取向性,复合后的材料具有海绵体的多孔结构,且保持了骨架原有的有规律取向,与普通相互交叉片不同,近乎平行的纳米片提供了长程有序、稳定统一的导电路径,有利于电子的顺利传递。核壳材料的厚度为200‑500 nm,壳层厚度为5‑15 nm,适当的壳层厚度、多孔结构和垂直生长,使得核材料的电化学特性得到充分发挥,电化学测试结果表明,在电流密度为0.5 A·g‑1时,单电极比容量为715 F·g‑1,当电流密度增大到8 A·g‑1时,比容量的保持率为72%。
Description
技术领域
本发明属于超级电容器器件技术领域,具体涉及金属氧化物核壳纳米片阵列电极材料的制备方法。
背景技术
电极材料的电化学活性直接决定器件的电容性能,因此,活性电极材料的开发便成为ECs研究和应用的重点。通常,用于ECs的电极材料包括炭材料、金属氧化物和导电聚合物三大类。炭材料电极通过电解液与电极的界面处形成的双电层存储能量(双电层电容);金属氧化物及导电聚合物材料电极则通过快速可逆的氧化还原反应获得法拉第电容(赝电容),此法拉第电容一般远大于炭材料获得的双电层电容。作为ECs 电极材料使用的贵金属氧化物(如RuO2)具有非常优良的电化学电容性质,但昂贵的价格和剧毒性大大制约其作为电化学电容器电极材料的应用和商品化,研究者尝试通过不同方法制备氧化钴(Co3O4)、氧化镍(NiO)、氧化锡(SnO2)和氧化锰( MnOx)等贱金属氧化物,作为贵金属氧化物的替代品,电极的比容量、充放电效率和长循环寿命显著提高。
申请号为201210438944.8的中国发明专利公开了一种超薄多孔Co3O4纳米片的制备方法,具体公开了向Co(NO3)2溶液中滴加DMSO溶液,采用电沉积法对镍表面进行电化学沉积,得到超薄多孔Co3O4纳米片;申请号为201611255619.2的中国发明专利公开了一种Co3O4多孔纳米片阵列的制备方法。具体公开了将重结晶硝酸钴/碳纤维纸焙烧得生长于碳纤维纸基底的多孔Co3O4纳米片阵列,各种工艺正在提高金属氧化物的比容量,但单一金属氧化物材料的自身缺陷如低电导率,晶型结构有限,比容量较低等缺陷仍是限制高性能电极材料进一步应用的关键。
2D核壳微纳米结构的NiO@Co3O4纳米片阵列,两种金属氧化物以不同的形式有机复合,设计合成的形貌新颖、结构稳定、导电基底原位生长,避免粉体材料在电极制备中需加入的导电性差的粘结剂,从而避免了电极中导电“死区”的出现,同时,利用产生的协同效应,弥补自身缺陷,对实现高效率的能量存储元器件的构筑具有十分重要的意义。
发明内容
本发明将导电集流体原位生长的NiO@Co3O4核壳纳米片阵列应用于超级电容器电极材料,提供一种具有协同增效、较高比容量和优良的倍率特性的超级电容器用复合电极材料的制备方法。
为解决上述技术问题,本发明采取如下技术方案:
本发明的超级电容器电极用NiO@Co3O4核壳纳米片阵列的制备方法,采用两步水热法,首先在导电基底上原位生长四氧化三钴纳米片阵列,并以此为骨架生长边界清晰的NiO核壳阵列,具体包括如下步骤:(1)2.5 mmol 的Co(NO3)2·6H2O,12.5 mmol的Co(NH2)2,溶于30mL蒸馏水中,充分溶解后连同处理过的泡沫镍转移至40 mL水热合成釜中,95℃反应8h,得到均匀生长在泡沫镍表面的碱式碳酸钴纳米片阵列。(2)将0.3-0.8 mmol硝酸镍加入到烧杯中,溶于36mL蒸馏水中,在磁力搅拌器下,加入6-16 mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在95-125℃保持7-13h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在250-400 ℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料。
所得的四氧化三钴纳米片骨架具有较好的平行多层结构和取向性,复合后的材料具有海绵体的多孔结构,且保持了骨架原有的有规律取向,与普通相互交叉片不同,近乎平行的纳米片提供了长程有序、稳定统一的导电路径,有利于电子的顺利传递。核壳材料的厚度为200-500 nm, 壳层厚度为5-15 nm,适当的壳层厚度、多孔结构和垂直生长,使得核材料的电化学特性得到充分发挥,电化学测试结果表明,在电流密度为0.5A·g-1时,单电极比容量为715 F·g-1,当电流密度增大到8 A·g-1时,比容量的保持率为72%。
附图说明
图1是实施例2中所制备的Co3O4 @NiO 核壳纳米片阵列扫描电镜照片。
图2是实施例1中所制备的Co3O4 @NiO 核壳纳米片阵列扫描电镜照片。
图3是实施例3中所制备的Co3O4 @NiO 核壳纳米片阵列扫描电镜照片。
图4是实施例2中所制备的Co3O4 @NiO 核壳纳米片阵列的循环伏安曲线。
图5是实施例2中所制备的Co3O4 @NiO 核壳纳米片阵列的充放电曲线。
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0.5 mmol硝酸镍溶于36mL蒸馏水中,在磁力搅拌器下,加入10 mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在100℃保持7h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在250℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料。
实施例2:将0.5 mmol硝酸镍溶于36mL蒸馏水中,在磁力搅拌器下,加入10 mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在100℃保持10h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在250℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料。
实施例3:将0.5 mmol硝酸镍溶于36mL蒸馏水中,在磁力搅拌器下,加入10 mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在100℃保持13h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在250℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料。
实施例4:将0.6 mmol硝酸镍溶于36mL蒸馏水中,在磁力搅拌器下,加入12 mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在115℃保持10h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在300℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料。
实施例5:将0.7 mmol硝酸镍溶于36mL蒸馏水中,在磁力搅拌器下,加入14 mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在100℃保持12h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在350℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料。
Claims (2)
1.一种金属氧化物核壳纳米片阵列电极材料的制备方法,其特征在于,所述电极活性材料是直接生长在导电集流体泡沫镍上的,所述的二维核壳纳米片具有较好的平行多层结构和取向性,核壳材料的厚度为200-500 nm,壳层厚度为5-15 nm。
2.一种金属氧化物核壳纳米片阵列电极材料的制备方法,其特征在于,包括如下步骤:将0.3-0.8 mmol硝酸镍加入到烧杯中,溶于36mL蒸馏水中,在磁力搅拌器下,加入6-16mmol尿素,搅拌10 min后,将生长片状Co3O4的前驱体和反应溶液转移到40mL密封的聚四氟乙烯内衬的不锈钢高压釜中,在95-125℃保持7-13h,反应结束后,取出泡沫镍基底,超声10min,60℃干燥40min,产物在250-400 ℃煅烧3h,得到Co3O4 @NiO 核壳纳米片阵列复合材料,近乎平行的纳米片提供了长程有序、稳定统一的导电路径,有利于电子的传递和电化学性能的提高。
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