CN108922793A - 一种二维层状Ti2CTx柔性纸的制备方法 - Google Patents
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Abstract
本发明公开了一种二维层状Ti2CTx柔性纸的制备方法,步骤如下:将Ti粉、Al粉和TiC粉混合,球磨混料4‑6h,置于在真空热压炉中烧结,得Ti2AlC粉末;在聚乙烯塑料瓶中,将盐酸加入除气的去离子水中,在搅拌下加入氟化锂,并缓慢加入Ti2AlC粉末,密封聚乙烯塑料瓶,并将磁力搅拌器升温至32‑36℃反应47‑49h,反应结束后,洗涤离心,将底层沉淀直接加入到装有除气的去离子水中,密封瓶盖并超声4‑5h,离心,得到含有少层或单层Ti2CTx纳米片的悬浮液,用硝基纤维素膜抽滤,干燥即得。该方法制备的二维层状Ti2CTx柔性纸可直接裁剪并用于超级电容器电极材料,并表现出了优异的电学性能。
Description
技术领域
本发明涉及一种二维层状Ti2CTx柔性纸的制备方法。
背景技术
自石墨烯被发现以来,便以其优异的性能引起了各界的广泛关注。但是由于其制备过程复杂、产率较低且代价较高,使得寻找一种新型的类石墨烯材料变得更为重要。自MXene材料被发现,成为了二维材料家族中新的一员。MXene材料是由三元层状碳氮化物MAX相(通式为Mn+1AXn,M是过渡金属元素,A主要是Ⅲ和Ⅳ主族元素,X是碳或/和氮元素,n=1、2或3)为前躯体,通过HF等选择性刻蚀出其中的A(Al)层后得到的一类二维过渡族金属碳(氮)化物。其化学组成可表示为Mn+1XnTx(T代表Al被腐蚀去除后Mn+1Xn层表面结合的OH、O、F等官能团),简称MXene,以反映其相对于MAX相的组成特点和类石墨烯的二维结构。此外,MXene材料的化学组成及其表面官能团赋予了其良好的亲水性及金属导电性和优异的力学性能,其性质可通过元素组成和表面官能团的改变而进行调控。因此MXene在电化学储能材料、传感器、电子器件材料、化工领域的催化剂、聚合物的导电增强相、环境治理以及储氢等许多领域展现出良好的应用前景。当MXene材料在用作超级电容器、锂离子电池、钠离子电池等的电极时,表现出了优异的性能,如Ti3C2Tx柔性纸作为锂离子电池负极和超级电容器电极的质量比容量和体积比容量分别高达410mAh/g和900F/cm3,并具有良好的充放电循环稳定性。
目前,MXene材料的制备主要是以HF作为刻蚀剂,将前躯体MAX相刻蚀得到相应的多层MXene,再通过插层剥离从而得到少层或单层的MXene。但由于HF的毒性、强腐蚀性以及工艺复杂、流程长等因素严重限制了MXene的研究、大规模制备及应用。
Ti3C2Tx是研究最多的MXene材料,每层Ti3C2Tx由3层Ti原子和2层C原子组成。相比之下Ti2CTx每层只含有2层Ti原子和1层C原子,原子数更少其质量比容量更大,理论预测其应具有更优的电化学性能。
发明内容
本发明的目的在于提供一种二维层状Ti2CTx柔性纸的制备方法。
本发明通过下面技术方案实现:
一种二维层状Ti2CTx柔性纸的制备方法,包括如下步骤:将10-20份Ti粉、14-18份Al粉和10-20份TiC粉混合,球磨混料4-6h,置于在真空热压炉中在1100-1200℃烧结2-3h,高能球磨破碎并过500目筛得Ti2AlC粉末;在聚乙烯塑料瓶中,将25-35份浓度为10mol/L的盐酸加入40-50份除气的去离子水中,在磁力搅拌下,加入5-15份氟化锂,充分搅拌至完全溶解,继续磁力搅拌,并缓慢加入10-20份Ti2AlC粉末,密封聚乙烯塑料瓶,并将磁力搅拌器升温至32-36℃充分反应47-49h,反应结束后,将产物用除气的去离子水洗涤离心直至上层清液pH值大于6.5,弃去上层液体,将底层沉淀直接加入到装有90-100份除气的去离子水中,密封瓶盖并超声4-5h,随后在3000rad/min的转速下离心10-15min,得到含有少层或单层Ti2CTx纳米片的悬浮液,用孔径为0.22μm的硝基纤维素膜抽滤,在34-36℃下真空干燥,干燥后Ti2CTx柔性纸可自动脱膜;各原料均为重量份。
优选地,所述的制备方法中,置于在真空热压炉中在1150℃烧结2.5h。
优选地,所述的制备方法中,将磁力搅拌器升温至34℃充分反应48h。
优选地,所述的制备方法中,密封瓶盖并超声4.5h。
优选地,所述的制备方法中,在3000rad/min的转速下离心12min。
优选地,所述的制备方法中,在35℃下真空干燥。
本发明技术效果:
该方法简便、快捷、易操作,制备的二维层状Ti2CTx柔性纸可直接裁剪并用于超级电容器电极材料,并表现出了优异的电学性能。
具体实施方式
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种二维层状Ti2CTx柔性纸的制备方法,包括如下步骤:将15份Ti粉、16份Al粉和15份TiC粉混合,球磨混料5h,置于在真空热压炉中在1150℃烧结2.5h,高能球磨破碎并过500目筛得Ti2AlC粉末;在聚乙烯塑料瓶中,将30份浓度为10mol/L的盐酸加入45份除气的去离子水中,在磁力搅拌下,加入10份氟化锂,充分搅拌至完全溶解,继续磁力搅拌,并缓慢加入15份Ti2AlC粉末,密封聚乙烯塑料瓶,并将磁力搅拌器升温至34℃充分反应48h,反应结束后,将产物用除气的去离子水洗涤离心直至上层清液pH值大于6.5,弃去上层液体,将底层沉淀直接加入到装有95份除气的去离子水中,密封瓶盖并超声4.5h,随后在3000rad/min的转速下离心12min,得到含有少层或单层Ti2CTx纳米片的悬浮液,用孔径为0.22μm的硝基纤维素膜抽滤,在35℃下真空干燥,干燥后Ti2CTx柔性纸可自动脱膜;各原料均为重量份。
实施例2
一种二维层状Ti2CTx柔性纸的制备方法,包括如下步骤:将10份Ti粉、14份Al粉和10份TiC粉混合,球磨混料4h,置于在真空热压炉中在1100℃烧结2h,高能球磨破碎并过500目筛得Ti2AlC粉末;在聚乙烯塑料瓶中,将25份浓度为10mol/L的盐酸加入40份除气的去离子水中,在磁力搅拌下,加入5份氟化锂,充分搅拌至完全溶解,继续磁力搅拌,并缓慢加入10份Ti2AlC粉末,密封聚乙烯塑料瓶,并将磁力搅拌器升温至32℃充分反应47h,反应结束后,将产物用除气的去离子水洗涤离心直至上层清液pH值大于6.5,弃去上层液体,将底层沉淀直接加入到装有90份除气的去离子水中,密封瓶盖并超声4h,随后在3000rad/min的转速下离心10min,得到含有少层或单层Ti2CTx纳米片的悬浮液,用孔径为0.22μm的硝基纤维素膜抽滤,在34℃下真空干燥,干燥后Ti2CTx柔性纸可自动脱膜;各原料均为重量份。
实施例3
一种二维层状Ti2CTx柔性纸的制备方法,包括如下步骤:将20份Ti粉、18份Al粉和20份TiC粉混合,球磨混料6h,置于在真空热压炉中在1200℃烧结3h,高能球磨破碎并过500目筛得Ti2AlC粉末;在聚乙烯塑料瓶中,将35份浓度为10mol/L的盐酸加入50份除气的去离子水中,在磁力搅拌下,加入15份氟化锂,充分搅拌至完全溶解,继续磁力搅拌,并缓慢加入20份Ti2AlC粉末,密封聚乙烯塑料瓶,并将磁力搅拌器升温至36℃充分反应49h,反应结束后,将产物用除气的去离子水洗涤离心直至上层清液pH值大于6.5,弃去上层液体,将底层沉淀直接加入到装有100份除气的去离子水中,密封瓶盖并超声5h,随后在3000rad/min的转速下离心15min,得到含有少层或单层Ti2CTx纳米片的悬浮液,用孔径为0.22μm的硝基纤维素膜抽滤,在36℃下真空干燥,干燥后Ti2CTx柔性纸可自动脱膜;各原料均为重量份。
该方法简便、快捷、易操作,制备的二维层状Ti2CTx柔性纸可直接裁剪并用于超级电容器电极材料,并表现出了优异的电学性能。
Claims (6)
1.一种二维层状Ti2CTx柔性纸的制备方法,其特征在于包括如下步骤:将10-20份Ti粉、14-18份Al粉和10-20份TiC粉混合,球磨混料4-6h,置于在真空热压炉中在1100-1200℃烧结2-3h,高能球磨破碎并过500目筛得Ti2AlC粉末;在聚乙烯塑料瓶中,将25-35份浓度为10mol/L的盐酸加入40-50份除气的去离子水中,在磁力搅拌下,加入5-15份氟化锂,充分搅拌至完全溶解,继续磁力搅拌,并缓慢加入10-20份Ti2AlC粉末,密封聚乙烯塑料瓶,并将磁力搅拌器升温至32-36℃充分反应47-49h,反应结束后,将产物用除气的去离子水洗涤离心直至上层清液pH值大于6.5,弃去上层液体,将底层沉淀直接加入到装有90-100份除气的去离子水中,密封瓶盖并超声4-5h,随后在3000rad/min的转速下离心10-15min,得到含有少层或单层Ti2CTx纳米片的悬浮液,用孔径为0.22μm的硝基纤维素膜抽滤,在34-36℃下真空干燥,干燥后Ti2CTx柔性纸可自动脱膜;各原料均为重量份。
2.根据权利要求1所述的制备方法,其特征在于:置于在真空热压炉中在1150℃烧结2.5h。
3.根据权利要求1所述的制备方法,其特征在于:将磁力搅拌器升温至34℃充分反应48h。
4.根据权利要求1所述的制备方法,其特征在于:密封瓶盖并超声4.5h。
5.根据权利要求1所述的制备方法,其特征在于:在3000rad/min的转速下离心12min。
6.根据权利要求1所述的制备方法,其特征在于:在35℃下真空干燥。
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109692581A (zh) * | 2019-01-15 | 2019-04-30 | 山东理工大学 | 二维层状Ti3C2膜及其制备方法与应用 |
CN113066673A (zh) * | 2021-03-24 | 2021-07-02 | 同济大学 | Ti3C2Tx-TiO2纳米管阵列自支撑薄膜电极材料及其制备方法和应用 |
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CN114838851A (zh) * | 2021-01-30 | 2022-08-02 | 苏州北科纳米科技有限公司 | 一种MXene柔性微力传感器的制备方法 |
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2018
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109692581A (zh) * | 2019-01-15 | 2019-04-30 | 山东理工大学 | 二维层状Ti3C2膜及其制备方法与应用 |
CN113772619A (zh) * | 2020-06-10 | 2021-12-10 | 宝山钢铁股份有限公司 | 一种微孔通道膜及其制备方法 |
CN113772619B (zh) * | 2020-06-10 | 2023-07-11 | 宝山钢铁股份有限公司 | 一种微孔通道膜及其制备方法 |
CN114804883A (zh) * | 2021-01-27 | 2022-07-29 | 中国科学院金属研究所 | 一种基于Ti2CTx迈科烯的高倍率锂离子电池负极材料制备方法 |
CN114804883B (zh) * | 2021-01-27 | 2023-11-10 | 中国科学院金属研究所 | 一种基于Ti2CTx迈科烯的高倍率锂离子电池负极材料制备方法 |
CN114843433A (zh) * | 2021-01-30 | 2022-08-02 | 苏州北科纳米科技有限公司 | 一种MXene导电纸及纸电池的制备方法 |
CN114838851A (zh) * | 2021-01-30 | 2022-08-02 | 苏州北科纳米科技有限公司 | 一种MXene柔性微力传感器的制备方法 |
CN114838851B (zh) * | 2021-01-30 | 2024-04-02 | 苏州北科纳米科技有限公司 | 一种MXene柔性微力传感器的制备方法 |
CN113066673A (zh) * | 2021-03-24 | 2021-07-02 | 同济大学 | Ti3C2Tx-TiO2纳米管阵列自支撑薄膜电极材料及其制备方法和应用 |
CN114184308A (zh) * | 2021-11-30 | 2022-03-15 | 西安电子科技大学 | 基于激光雕刻的一体化全柔性离电式传感器及制备方法 |
CN115538209A (zh) * | 2022-10-08 | 2022-12-30 | 哈尔滨工业大学 | 一种MXene纤维无纺布及其制备方法 |
CN115538209B (zh) * | 2022-10-08 | 2023-11-14 | 哈尔滨工业大学 | 一种MXene纤维无纺布及其制备方法 |
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