CN107393730A - 一种石墨烯/钴‑镍双金属氢氧化物的制备方法 - Google Patents
一种石墨烯/钴‑镍双金属氢氧化物的制备方法 Download PDFInfo
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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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
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Abstract
本发明公开一种石墨烯/钴‑镍双金属氢氧化物的制备方法，包括以下步骤：选取一定粒度的石墨粉末，对其进行氧化处理、过滤清洗获得石墨粉末，然后对石墨粉末进行微波膨化后，获得膨胀蠕虫石墨粉末，并将其放入N‑甲基吡咯烷酮溶剂中，经超声震荡、离心分离，取上层悬浮液，将一定摩尔比的钴盐和镍盐加入其中，获得一定浓度的前驱体，并将前驱体放入高压反应釜密封加热，冷却后将反应产物过滤、洗涤、干燥后即获得石墨烯/钴‑镍双金属氢氧化物。本发明的复合材料具有原料易得、廉价，成本低，电极储能特性效果好等特点，可以应用在超级电容器电极材料和电化学催化方面。
Description
技术领域
本发明涉及功能复合功能材料制备领域，主要是涉及一种生产成本低、重量轻、储能效果好的复合纳米材料制备方法。
背景技术
超级电容器从储能机理上分的话，超级电容器分为双电层电容器和赝电容器。是一种新型储能装置，它具有功率密度高、充电时间短、使用寿命长、温度特性好、节约能源和绿色环保等特点。按其储能机理可以分为双电层型超级电容器和赝电容型超级电容器，双电层型超级电容器主要是采用活性碳，碳纤维，碳气凝胶，碳纳米管或石墨烯作为电极材料的，通过电场吸附电荷储存能量的机制。赝电容型超级电容器包括金属氧化物电极材料与聚合物电极材料，金属氧化物包括NiOx、MnO2、V2O5等作为正极材料，活性炭作为负极材料制备的超级电容器，导电聚合物材料包括PPY、PTH、PANi等掺杂制取电极。其中新近发现的具有高储能特性的水滑石类化合物，其主体一般由两种金属的氢氧化物构成，又称为层状双羟基复合金属氧化物或双金属氢氧化物，它们是一类具有高电化学储能特性的化合物。
然而双金属氢氧化物自身导电特性差，使得其循环稳定性和倍率性能会有所下降，一个有效的提高上述缺点的方法就是将其与具有高导电特性的物质复合，例如碳纳米管、石墨烯等，获得一类复合材料，不仅能发挥氢氧化物高储能的特性，也能通过碳材料提高其电导率，实现高的综合性能。
发明内容
针对超级电容器电极材料存在的问题和不足，本发明的目的是提供一种具有高储能特性及电化学稳定性的复合电极材料的制备方法，选用具有水滑石结构的钴-镍双金属氢氧化物和石墨烯原位复合，通过化学一步法实现二者的组合，为高性能超级电容器提供优质电极材料。
一种石墨烯/钴-镍双金属氢氧化物的制备方法，包括以下步骤：
(1)选取粒度为1～100微米的石墨粉末，依次对其进行浓硝酸和高锰酸钾氧化处理，过滤后用大量水清洗石墨粉末；
(2)然后将(1)中所得的石墨粉末放入微波炉微波膨化后，获得膨胀蠕虫石墨粉末；
(3)将(2)中的膨胀石墨粉末放入N-甲基吡咯烷酮溶剂中，经2小时以上超声波震荡、并离心分离，取浓度为1～10mg/mL上层悬浮液，将其用作多层石墨烯；
(4)把1:9-9:1摩尔比的钴盐和镍盐加入到(3)中获得的多层石墨烯悬浮液中，钴盐和镍盐的总摩尔量为0.01～0.1mol，室温下搅拌均匀，即获得0.1～1mol/L前驱体；
(5)将(4)中的前驱体放入聚四氟乙烯为内衬的高压反应釜中，填充率为70％～85％，密封反应釜后，将其加热到180～200度反应1～2小时；
(6)将(5)中的反应釜自然冷却到室温后，取出反应产物经过过滤、洗涤、干燥后即获得石墨烯/钴-镍双金属氢氧化物。
进一步地，所述的钴盐为四水合醋酸钴和六水合硝酸钴中的一种或它们的混合物。
进一步地，所述的镍盐为四水合醋酸镍和六水合硝酸镍中的一种或它们的混合物。
本发明所制备的石墨烯/钴-镍双金属氢氧化物具有以下优点：
(1)原料来源广、价格便宜，产品比电容高，循环稳定性好；
(2)复合材料一次工艺获得，工艺简单，生产周期短；
(3)对制备设备要求低，便于批量化规模化制备。
具体实施方式
实施例1
选取平均粒径5微米的天然高纯石墨粉末，依次对其进行浓硝酸和高锰酸钾氧化处理，过滤后用大量水清洗石墨粉末；然后将石墨粉末放入微波炉微波膨化后，获得膨胀蠕虫石墨粉末；加入N-甲基吡咯烷酮中超声震荡超声波震荡、并离心分离后，取出5mg/mL上层悬浊液100mL，加入0.025mol四水合醋酸钴和0.075mol四水合醋酸镍，搅拌均匀后，装入总体积120mL的反应釜中，经过180度反应1小时后，冷却，过滤，洗涤，干燥后获得石墨烯/钴-镍双金属氢氧化物。在2mol/L KOH水溶液中，单电极测试其比电容为1185F/g，经过10000次充放电循环后，比电容保留率为92％。
实施例2
选取平均粒径1微米的天然高纯石墨粉末，依次对其进行浓硝酸和高锰酸钾氧化处理，过滤后用大量水清洗石墨粉末；然后将石墨粉末放入微波炉微波膨化后，获得膨胀蠕虫石墨粉末；加入N-甲基吡咯烷酮中超声震荡超声波震荡、并离心分离后，取出1mg/mL上层悬浊液100mL，加入0.001mol六水合硝酸钴和0.009mol六水合硝酸镍，搅拌均匀后，装入总体积140mL的反应釜中，经过200度反应2小时后，冷却，过滤，洗涤，干燥后获得石墨烯/钴-镍双金属氢氧化物。在2mol/L KOH水溶液中，单电极测试其比电容为1476F/g，经过5000次充放电循环后，比电容保留率为95％。
实施例3
选取平均粒径100微米的天然高纯石墨粉末，依次对其进行浓硝酸和高锰酸钾氧化处理，过滤后用大量水清洗石墨粉末；然后将石墨粉末放入微波炉微波膨化后，获得膨胀蠕虫石墨粉末；加入N-甲基吡咯烷酮中超声震荡超声波震荡、并离心分离后，取出10mg/mL上层悬浊液100mL，加入0.009mol四水合醋酸钴和0.001mol四水合醋酸镍，搅拌均匀后，装入总体积125mL的反应釜中，经过200度反应2小时后，冷却，过滤，洗涤，干燥后获得石墨烯/钴-镍双金属氢氧化物。在2mol/L KOH水溶液中，单电极测试其比电容为1064F/g，经过10000次充放电循环后，比电容保留率为97％。
Claims (3)
1.一种石墨烯/钴-镍双金属氢氧化物的制备方法，包括以下步骤：
(1)选取粒度为1～100微米的石墨粉末，对其依次进行浓硝酸和高锰酸钾氧化处理，过滤后用大量水清洗石墨粉末；
(2)然后将(1)中所得的石墨粉末放入微波炉微波膨化后，获得膨胀蠕虫石墨粉末；
(3)将(2)中的膨胀石墨粉末放入N-甲基吡咯烷酮溶剂中，经2小时以上超声波震荡、并离心分离，取浓度为1～10mg/mL上层悬浮液，将其用作多层石墨烯；
(4)把1:9～9:1摩尔比的钴盐和镍盐加入到(3)中获得的多层石墨烯悬浮液中，钴盐和镍盐的总摩尔量为0.01～0.1mol，室温下搅拌均匀，即获得0.1～1mol/L前驱体。
(5)将(4)中的前驱体放入聚四氟乙烯为内衬的高压反应釜中，填充率为70％～85％，密封反应釜后，将其加热到180～200度反应1～2小时；
(6)将(5)中的反应釜自然冷却到室温后，取出反应产物经过过滤、洗涤、干燥后即获得石墨烯/钴-镍双金属氢氧化物。
2.如权利要求1所述的制备方法，其特征在于，步骤(4)中所述的钴盐为四水合醋酸钴和六水合硝酸钴中的一种或它们的混合物。
3.如权利要求1所述的制备方法，其特征在于，步骤(4)中所述的镍盐为四水合醋酸镍和六水合硝酸镍中的一种或它们的混合物。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN109513440A (zh) * | 2018-11-12 | 2019-03-26 | 上海今海新材料科技有限公司 | 一种花状石墨烯担载的氧化铜复合粉体的制备方法 |
| CN110289178A (zh) * | 2019-05-13 | 2019-09-27 | 江苏大学 | 两步法制备氧化镍/四氧化三钴/氮掺杂碳点超薄纳米片电极材料及其应用 |
| CN110676069A (zh) * | 2019-10-15 | 2020-01-10 | 西华大学 | 一种石墨烯-金属氧化物/氮化物复合储能材料及其制备方法 |
| CN111001375A (zh) * | 2019-12-29 | 2020-04-14 | 福建工程学院 | 一种层状双氢氧化物复合吸附材料的制备方法 |
| CN111001375B (zh) * | 2019-12-29 | 2023-03-14 | 福建工程学院 | 一种层状双氢氧化物复合吸附材料的制备方法 |
| CN111199834A (zh) * | 2020-01-08 | 2020-05-26 | 杭州电子科技大学 | 一种硫化钴/多层石墨烯复合材料及其制备方法 |
| CN113231023A (zh) * | 2021-05-17 | 2021-08-10 | 黑龙江省科学院高技术研究院 | 一种膨胀石墨基钴铟双金属氢氧化物层间复合材料的制备方法及应用 |
| CN113231023B (zh) * | 2021-05-17 | 2022-06-28 | 黑龙江省科学院高技术研究院 | 一种膨胀石墨基钴铟双金属氢氧化物层间复合材料的制备方法及应用 |
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