CN105702958B - 一种二氧化锡量子点溶液及其复合材料的制备方法与应用 - Google Patents
一种二氧化锡量子点溶液及其复合材料的制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种高稳定性二氧化锡(SnO2)量子点水溶液的简易制备方法，量子点粒径尺寸在2～5nm范围内。该方法利用SnCl2·2H2O的水解特性，引入硫脲作为催化剂和稳定剂，在常温下通过持续磁力搅拌12‑24小时，即可得到黄色澄清透明的SnO2量子点溶液。该方法制备的SnO2量子点粒径小和结晶性好，具有良好的稳定性和分散性；通过简单地混合SnO2量子点溶液和碳纳米材料，即可进一步得到均匀负载SnO2量子点的碳基复合纳米材料。以其作为锂离子电池的负极材料，表现出了优异的电化学特性。本发明的制备方法步骤简单，成本低廉，便于工业化应用。
Description
技术领域
本发明涉及一种SnO2量子点溶液及其复合材料的简易制备方法与应用，属于锂离子电池电极材料的制备与应用领域。
背景技术
在当今能源危机和能源革命的时代，二次化学电源扮演着十分重要的角色。被广泛应用的二次电源的发展经历了铅酸电池、镍镉电池、镍氢电池、锂离子电池等几个阶段。由于锂离子电池具有更高的比能量、比功率等突出优势，自20世纪90年代初开发成功以来，已成为目前综合性能最好的电池体系，支撑着现代和未来生活的发展。目前，商业化的锂离子电池负极材料一般为石墨类材料或者以碳作为基质的材料。然而，商用的锂离子电池存在着比容量低，首次充放电效率低，有机溶剂共嵌入等不足，随着大功率用电设备如电动车、混合动力汽车及太阳能风能等储电设备的发展，已经不能满足高容量及高倍率性能要求，制约了锂离子电池的进一步发展。因此，亟需开发高能量密度化学电源，开发容量密度高、循环寿命长、安全性能好的锂离子电池负极材料成为当前能源领域的重要研究方向。
目前，在被研究的各种锂离子电池负极材料中，锡基负极材料具有质量与体积比能量高，价格便宜，无毒副作用，加工合成相对容易等优点，受到了研究者的广泛关注。锡基负极材料包括金属锡、氧化锡、氧化亚锡及其锡基复合氧化物，与商用的石墨碳材料(理论比容量372mAh/g)相比，锡基材料的比容量要大得多(SnO2：～790mAh/g；SnO：～875mAh/g；Sn：～990mAh/g)。研究工作表明，Sn的氧化物具有合金型储锂机理，以氧化锡SnO2为例，其储锂过程分为两步：第一步是SnO2+4Li++4e-→Sn+2Li2O，SnO2被Li金属还原生成金属Sn和Li2O，这一步是不可逆的；第二步是可逆的
这是SnO2的电化学储锂机制。然而，锡基合金化的储锂机制导致其首次不可逆容量很大，这主要是由于储锂第一步中Li2O的生成及SEI膜的形成；而第二步造成了材料在脱嵌锂的过程中，产生了巨大的体积形变导致电极材料的粉化，从而造成材料比容量衰减和循环性能的下降，限制了该类材料的商业化应用。为改善锡基负极材料的电化学性能，研究思路主要集中在材料的纳米化、掺杂改性、包覆处理、与新型纳米碳(如碳纳米管和石墨烯)复合等方面。电极材料的尺寸降到纳米范围时，比表面积增大，锂离子在其中扩散距离显著降低，所以对于同种成分的电极材料而言，纳米材料具有更好的倍率特性。除此之外，颗粒尺寸的降低可以增加储锂位，缩短锂离子扩散距离，从而提高材料的可逆比容量。然而由于其颗粒尺寸小、比表面积及表面能大，容易吸附杂质元素或者不可避免地发生颗粒之间的团聚。因此，单独的某种材料都不能完全满足实际需要。碳材料虽然有很好的循环性能，但比容量低；锡基材料虽然比容量高，但首次不可逆损失很高且体积形变严重；纳米颗粒虽然体积小，但是容易团聚。这样看来，综合各种材料的优点，有目的的地将各种材料复合，避免各自存在的不足，形成复合负极材料是一个合理的选择。目前，与新型纳米碳(如碳纳米管和石墨烯)复合是最行之有效的方法之一。碳纳米管作为负极材料不仅可以嵌脱锂离子，而且碳纳米管相互交错构筑的网络结构，可以作为骨架材料负载锡基负极材料，避免颗粒之间的团聚，同时可有效缓解脱嵌锂过程中体积膨胀-收缩带来的应力变化，进而克服锡基材料在充放电过程中的粉化问题。另外，碳纳米管良好的导电性有利于离子运输和电子传导，可以改善电极材料的电导性，从而提高了材料的综合电化学性能。例如，上海交通大学研究组通过水热、高温煅烧手段合成了具有中空碳包覆结构的SnO2@CNT@C复合材料，在200mA/g电流密度下，经过350次充放电循环后容量为～700mAh/g；北京大学研究组利用葡萄糖改性后的碳纳米管，通过水热法制备了纳米棒自组装结构的CNT@SnO2，在720mA/g电流密度下，经过40次循环后仍能保持～980mAh/g的容量。华中科技大学研究组通过一步溶剂热法制备了graphene@CNT@SnO2，在200mA/g电流密度下，经过100次充放电循环后容量为～840mAh/g；然而，研究成果最终需要转化成实际应用才有研究意义。传统的水热，湿化学合成方法，往往需要高温，昂贵的原材料，特殊的烧结气氛和复杂的过程，不利于实际发展。所以如何在满足性能要求的前提下，最大化减少成本，利于商业化、产业化发展，真正应用于实际，同样是重中之重的任务。
发明内容
本发明旨在提出一种简单，高效，低成本的合成方法。仅在常温下，成功制备了均匀分散的稳定的SnO2量子点溶液(平均粒径小于5nm)；通过简易吸附原理，实现了超细SnO2量子点在多壁碳纳米管上的沉积与均匀分布。将其作为锂离子电池负极材料，表现出了优异的电化学性能。
本发明通过如下技术方案实现，具体步骤为：
1.将称量好的SnCl2·2H2O和CH4N2S粉末倒入放有去离子水的锥形瓶中，持续搅拌后即可得到SnO2量子点溶液(溶液1)；
2.将称量好的碳纳米管分散于去离子水中后，与溶液1混合，搅拌一段时间后得到SnO2@CNT溶液。
附图说明
图1是本发明的实施例1中制备的SnO2量子点的高分辨透射电镜图。
图2是本发明的实施例1中SnO2量子点和碳纳米管的高分辨透射电镜图。
具体实施方式
为便于理解本发明，下面通过实施例对本发明作详细描述，但并不限于本发明的内容。
实施例1
将0.9gSnCl2·2H2O和0.3gCH4N2S粉末混合并放入于装有30mL去离子水的锥形瓶中，形成乳白色悬浮液。在常温下连续搅拌12-24h后，得到呈黄色澄清状的SnO2量子点溶液；将20mg碳纳米管分散于25mL去离子水中，搅拌1小时，得到分散均匀的碳纳米管水溶液，将制备的SnO2量子点溶液加入上述水溶液并持续搅拌，一段时间后，得到黑色的SnO2@CNTs溶液。
实施例2
分别以SnO2和SnO2@CNTs作为锂离子负极材料，与乙炔黑和聚丙烯酸(PAA)按质量比8∶1∶1混合，加水制备成均匀浆料，涂在铜箔上，并于120℃下干燥12h以上。以锂片作为对电极，美国celgard2400为锂电池隔膜，电解液为1MLiPF6，溶剂为EC+DEC(体积比1∶1)，组装成2025钮扣式电池。电池充放电测试在深圳新威电池测试系统上进行。组装成的电池在100mA/g电流密度下，SnO2电池经过40次循环容量保持在290mAh/g左右；SnO2@CNTs电池经过90次循环，容量保持在875mAh/g左右。
Claims (2)
1.一种SnO2@CNTs复合材料的制备方法，其特征是：以无机锡盐SnCl2·2H2O作为锡源，硫脲为催化剂和稳定剂，在常温下通过磁力搅拌得到黄色澄清状的SnO2量子点溶液；随后以碳纳米管CNTs作为载体，在常温下通过搅拌一定时间即可得到SnO2@CNTs复合材料。
2.如权利要求1所述方法制备的SnO2@CNTs复合材料在锂离子电池负极材料与超级电容器、透明导电膜领域中的应用。
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| CN106784329B (zh) * | 2017-01-12 | 2019-10-11 | 武汉大学 | 一种SnO2量子点电子传输层钙钛矿太阳能电池及其制备方法 |
| CN110161009B (zh) * | 2019-06-27 | 2021-09-03 | 大连海事大学 | 二氧化锡量子点检测污水中重金属离子的应用及检测方法 |
| CN110726759A (zh) * | 2019-10-31 | 2020-01-24 | 大连海事大学 | 一种二氧化锡量子点的制备方法、气体传感器及其制备方法 |
| CN113267476B (zh) * | 2021-04-30 | 2022-11-25 | 大连海事大学 | 一种应用二氧化锡量子点检测船用燃油中硫含量的方法 |
| CN114113238A (zh) * | 2021-11-17 | 2022-03-01 | 中国兵器工业集团第二一四研究所苏州研发中心 | 一种基于三维多孔石墨烯@量子点复合材料的气敏传感器及其制备方法 |
| CN115939332A (zh) * | 2022-09-09 | 2023-04-07 | 厦门理工学院 | 一种锡基负极材料、制备方法及其应用 |
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