CN113224275A - 一种石墨烯/粘土纳米复合电极材料及其制备方法 - Google Patents
一种石墨烯/粘土纳米复合电极材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯/粘土纳米复合电极材料制备方法，主要包括如下步骤：将焦糖、层状粘土和水混合并搅拌制得前驱物；将前驱物放入管式炉中，在惰性气体氛围中按照一定的升温速率加热至800‑1000℃，保持3‑5小时；混合物取出磨粉，即可获得石墨烯复合纳米电极材料。本发明的石墨烯/粘土纳米复合电极材料综合了石墨烯材料优良的导电性能和绿脱石良好的化学性能稳定性，形成了ABAB型堆叠层状结构，极大的提高了充放电过程中，锂离子在正负极材料之间的穿梭能力和穿梭效率，具备优良的充放电性能和高循环次数。同时，该电极材料制备工艺简单，易于工业化。
Description
技术领域
本发明属于电极材料技术领域，涉及一种粘土石墨烯/粘土纳米复合材料及其制备方法。
背景技术
锂离子电池以其比能量高、功率密度高、循环寿命长、自放电小、性能价格比高等优点已经成为当今便携式电子产品的可再充式电源的主要选择对象。与此同时，为缓解环境压力.世界各国竞相开发电池和机械动力并用的混合电动汽车(HEV)。在锂离子电池的发展过程中，正极材料可能会成为制约其大规模推广应用的瓶颈，所以开发性能优越、价格便宜的正极材料是锂离子电池商业化进程中的关键性因素。
锂离子电池的正极是含金属锂的化合物，一般为锂铁磷酸盐(如磷酸铁锂LiFePO4、磷酸钴锂LiCoO2等)，负极是石墨或炭(一般多用石墨)，正负极之间使用有机溶剂作为电解质。在对电池进行充电时，正极上分解生成锂离子，锂离子通过电解质进入电池负极，嵌入负极碳层的微孔中。在电池的使用过程中(相当于放电)，嵌在负极微孔中的锂离子又运动回正极。回到正极的锂离子越多，放电容量就越高，我们平时所指的电池容量就是放电容量。这样，在电池充放电过程中，锂离子不断地在正负极之间来回奔跑，所以锂离子电池也被称为摇椅式电池。电化学反应方程式如下：
正极：Li0.33Fe(3+)2〔(Al，Si)4O10〕(OH)2·nH2O<＝>
Li0.33-xFe(2+)2〔(Al，Si)4O10〕(OH)2·nH2O+xLi++xe-
负极：xLi+xe-+6C<＝>LixC6
总反应：Li0.33Fe(3+)2〔(Al，Si)4O10〕(OH)2·nH2O+6xC<＝>Li0.33·FePO4+LixC6
石墨烯是只有一层碳原子厚度的二维晶体。石墨烯本不具备储电的能力，是一种导电性能优越的新型纳米材料。在充放电过程中，加速了石墨烯锂离子在石墨烯表面和电极之间的穿梭运动。
粘土不具备非常好的导电性能，但其结构稳定性能优越，尤其是含有二价铁绿脱石，可通过在电池的中的电化学氧化还原，引导锂离子脱嵌。
粘土石墨烯复合纳米电极材料，即利用石墨烯优越的导电性能和綠脱石稳定的化学性能，可制得的一种新型电极材料，具备良好的充放电性能和较高的循环效率。
发明内容
本发明的目的在于提供一种能够同时具有优良的导电性能和化学稳定性的电极材料。
为了实现上述目的，本发明采用以下技术方案：
一种石墨烯/粘土纳米复合电极材料的制备方法，其特征在于，包括如下步骤：
(1)按照m焦糖∶m层状粘土∶m水＝1∶2～3∶5～8的比例将焦糖、层状粘土和水混合并搅拌2-5小时，制得前驱物；
(2)将步骤(1)获得的前驱物放入管式炉中，在惰性气体氛围中按照5-10℃/分钟的升温速率加热至800-1000℃，保持3-5小时；
(3)将步骤(2)获得的混合物取出磨粉，即可获得石墨烯复合纳米电极材料。
进一步地，步骤(1)中的层状粘土为绿脱石粉体，粒度为200-400目。
进一步地，步骤(1)中的水为去离子水。
进一步地，步骤(2)中惰性气体为氮气。
进一步地，步骤(3)中将混合物磨成目数为200-400目的粉末。
本发明的另一个目的在于提供上述制备方法制备得到的石墨烯/粘土纳米复合电极材料，其特征在于，所述石墨烯/粘土纳米复合电极材料结构为锂离子掺杂的ABAB型堆叠层状材料。
进一步地，锂离子掺杂区域为石墨烯所在的层间域区域。
本发明的石墨烯/粘土纳米复合电极材料综合了石墨烯材料优良的导电性能和绿脱石良好的化学性能稳定性，形成了ABAB型堆叠层状结构(如图1所示)，极大的提高了充放电过程中，锂离子在正负极材料之间的穿梭能力和穿梭效率，具备优良的充放电性能和高循环次数。同时，该电极材料制备工艺简单，易于工业化。
附图说明
图1是本发明石墨烯复合纳米电极材料的结构图。
具体实施方式
实施例1
取10g焦糖，20g粒度为200目的绿脱石粉末和50g的去离子水，混合并置于高速搅拌机中搅拌2.5个小时，制得前驱体；
将前驱体置于管式炉中，充入氮气，以5℃/min的升温速率升温至800℃，并继续保持3个小时；
取出获得的混合物，磨碎至200目，即得到石墨烯/粘土纳米复合电极材料。
石墨烯/粘土纳米复合电极材料结构如图1所示，具备ABAB型层状结构，锂离子掺杂区域为石墨烯层间区域。
获得材料充放电性能如下表所示：
实施例2
取20g焦糖，40g粒度为200目的绿脱石粉末和120g的去离子水，混合并置于高速搅拌机中搅拌3.5个小时，制得前驱体；
将前驱体置于管式炉中，充入氮气，以8℃/min的升温速率升温至800℃，并继续保持3个小时；
取出获得的混合物，磨碎至300目，即得到石墨烯/粘土纳米复合电极材料。
石墨烯/粘土纳米复合电极材料结构如图1所示，具备ABAB型层状结构，锂离子掺杂区域为石墨烯层间区域。
获得材料充放电性能如下表所示：
实施例3
取40g焦糖，80g粒度为200目的绿脱石粉末和320g的去离子水，混合并置于高速搅拌机中搅拌5个小时，制得前驱体；
将前驱体置于管式炉中，充入氮气，以5℃/min的升温速率升温至900℃，并继续保持5个小时；
取出获得的混合物，磨碎至400目，即得到石墨烯/粘土纳米复合电极材料。
石墨烯/粘土纳米复合电极材料结构如图1所示，具备ABAB型层状结构，锂离子掺杂区域为石墨烯层间区域。
获得材料充放电性能如下表所示：
以上试验证明，本发明的石墨烯/粘土纳米复合电极材料综合了石墨烯材料优良的导电性能和绿脱石良好的化学性能稳定性，极大的提高了充放电过程中，锂离子在正负极材料之间的穿梭能力和穿梭效率，具备优良的充放电性能和高循环次数。
Claims (7)
1.一种石墨烯/粘土纳米复合电极材料的制备方法，其特征在于，包括如下步骤：
(1)按照m焦糖∶m层状粘土∶m水＝1∶2～3∶5～8的比例将焦糖、层状粘土和水混合并搅拌2-5小时，制得前驱物；
(2)将步骤(1)获得的前驱物放入管式炉中，在惰性气体氛围中按照5-10℃/分钟的升温速率加热至800-1000℃，保持3-5小时；
(3)将步骤(2)获得的混合物取出磨粉，即可获得石墨烯复合纳米电极材料。
2.如权利要求1所述的制备方法，其特征在于，步骤(1)中的层状粘土为绿脱石粉体，粒度为200-400目。
3.如权利要求1所述的制备方法，其特征在于，步骤(1)中的水为去离子水。
4.如权利要求1所述的制备方法，其特征在于，步骤(2)中惰性气体为氮气。
5.如权利要求1所述的制备方法，其特征在于，步骤(3)中将混合物磨成目数为200-400目的粉末。
6.由权利要求1～5任一所述制备方法制备得到的石墨烯/粘土纳米复合电极材料，其特征在于，所述石墨烯/粘土纳米复合电极材料的结构为锂离子掺杂的ABAB型堆叠层状材料。
7.根据权利要求6所述的石墨烯/粘土纳米复合电极材料，其特征在于，锂离子掺杂区域为石墨烯所在的层间域区域。
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| CN102157736A (zh) * | 2011-03-23 | 2011-08-17 | 中银（宁波）电池有限公司 | 一次锂电池二硫化铁/碳复合正极材料及其制备方法和应用 |
| WO2013103537A1 (en) * | 2012-01-04 | 2013-07-11 | Momentive Performance Materials Inc. | Silicone adhesive compositions |
| CN103950914A (zh) * | 2014-04-04 | 2014-07-30 | 西安理工大学 | 一种类石墨烯结构的导电碳材料的制备方法 |
| CN107128903A (zh) * | 2017-06-02 | 2017-09-05 | 扬州大学 | 以卷曲层状结构的埃洛石纳米管制备石墨烯的方法 |
| US20180366280A1 (en) * | 2017-06-14 | 2018-12-20 | Nanotech Energy, Inc | Electrodes and electrolytes for aqueous electrochemical energy storage systems |
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| CN102157736A (zh) * | 2011-03-23 | 2011-08-17 | 中银（宁波）电池有限公司 | 一次锂电池二硫化铁/碳复合正极材料及其制备方法和应用 |
| WO2013103537A1 (en) * | 2012-01-04 | 2013-07-11 | Momentive Performance Materials Inc. | Silicone adhesive compositions |
| CN103950914A (zh) * | 2014-04-04 | 2014-07-30 | 西安理工大学 | 一种类石墨烯结构的导电碳材料的制备方法 |
| CN107128903A (zh) * | 2017-06-02 | 2017-09-05 | 扬州大学 | 以卷曲层状结构的埃洛石纳米管制备石墨烯的方法 |
| US20180366280A1 (en) * | 2017-06-14 | 2018-12-20 | Nanotech Energy, Inc | Electrodes and electrolytes for aqueous electrochemical energy storage systems |
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Denomination of invention: A graphene/clay nanocomposite electrode material and its preparation method Granted publication date: 20220719 Pledgee: Agricultural Bank of China Limited Yangyuan County Branch Pledgor: YANGYUAN COUNTY RENHENG FINE CLAY Co.,Ltd. Registration number: Y2024980003041 |