CN115092929B - 一种大片层可控孔洞化MXene纳米片的制备方法 - Google Patents
一种大片层可控孔洞化MXene纳米片的制备方法 Download PDFInfo
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Abstract
本发明公开了一种大片层可控孔洞化MXene纳米片的制备方法，该方法先将Ti3AlC2粉末用氢氟酸刻蚀掉其中的Al元素，得到多层MXene；然后将多层MXene在六亚甲基四胺催化氧化作用下进行水热反应，得到MXene/TiO2复合材料；最后利用过量氢氟酸处理去除TiO2，得到二维孔洞化MXene纳米片。本发明在六亚甲基四胺催化氧化作用下，MXene片层上Ti在水热反应条件下被快速氧化，且可以通过调节反应时间、反应温度控制Ti氧化程度及制备得到不同粒径大小的MXene/TiO2复合材料，并在此基础上制备得到孔径可控、孔分布均匀的二维孔洞化Mxene纳米片材料，有望进一步改善MXene做锂离子电池等储能装置电极材料性质。
Description
技术领域
本发明属于材料技术领域，具体涉及一种大片层可控孔洞化MXene纳米片的制备方法。
背景技术
二维层状材料具有高比表面积、高活性位点及快速离子扩散路径等优势，已经在电催化、超级电容器和二次电池等储能领域被广泛应用。众多二维纳米材料中，过渡金属碳/氮化物材料是一类新型二维晶体，化学通式为Mn+1XnTz(M：过渡金属元素；X：碳或氮元素；T：活性官能团)，具有与石墨烯类似的层状结构，且表面存在F-，OH-，O2-等官能团。由于MAX相种类众多，包含多种元素，在氢氟酸(HF) 的作用下可以选择性刻蚀掉其中的金属原子，自上而下剥离得到类石墨烯结构的二维层状晶体，具有不同的物理化学性质。目前，研究最为普遍的一种物质是Ti3AlC2，在HF酸作用下Al原子被选择性刻蚀，剥离得到Ti3AlC2纳米片。这类材料具有优异的导电性，比表面积较大，活性位点多，具有良好的电学、磁学以及力学性能等，有望应用在储能、催化、吸附等各个领域。
目前，关于制备MXene纳米片的常见方法主要包括两种：一种是自下而上生长制备高质量薄膜技术，但无法获得单层纳米片；另一类是自上而下化学剥离制备单层纳米片。将其应用于储能领域具有导电性好等优势，但其在垂直方向上通过平面的电导率有限，致使材料倍率性能等会有下降，对开发高容量和快速充放电电极材料不利。研究表明采用在片层上形成孔洞化的方式来进行改性，可以克服纳米片层组装的堆叠问题，能够加快离子和电子快速传输到电极结构内部，同时可以提高电解液对电极材料浸润性等。但对于制备可精细调控的孔径均匀MXene纳米片的报道较少，严重影响了孔洞化MXene材料的发展。因此，开发粒径均匀、尺寸可控的二维MXene纳米片层制备新技术具有重要意义。
发明内容
本发明的目的是提供一种操作简单、孔径均匀、尺寸可控的二维孔洞化MXene 纳米片的制备方法。
针对上述目的，本发明所采用的技术方案由下述步骤组成：
(1)将Ti3AlC2粉末加入到氢氟酸中，搅拌充分反应使其中Al元素被完全刻蚀掉，将刻蚀后物质洗至中性后冷冻干燥，得到多层MXene；
(2)将多层MXene加入到蒸馏水和乙醇的混合液中，超声分散30～60分钟后搅拌10～24小时，再加入六亚甲基四胺，在反应釜中120～160℃水热反应5～ 12小时，所得产物用水和乙醇洗涤至中性后真空干燥，得到MXene/TiO2复合材料；
(3)利用过量氢氟酸处理MXene/TiO2复合材料以去除TiO2，得到二维孔洞化 MXene纳米片。
上述步骤(1)和步骤(3)中，所述氢氟酸是质量浓度为25％～35％的氟化氢水溶液。
上述步骤(2)中，优选多层MXene与六亚甲基四胺的质量为1：0.5～0.8。
上述步骤(2)中，优选在反应釜中150℃水热反应5小时。
上述步骤(2)中，所述混合液中蒸馏水和乙醇的体积比为1：1。
本发明的有益效果如下：
本发明在六亚甲基四胺催化氧化作用下，MXene片层上Ti在水热反应条件下被快速氧化，且可以通过调节反应时间、反应温度控制Ti氧化程度及制备得到不同粒径大小的MXene/TiO2复合材料，并在此基础上制备得到孔径可控、孔分布均匀的二维孔洞化Mxene纳米片材料，有望进一步改善MXene做锂离子电池等储能装置电极材料性质。
附图说明
图1是多层MXene在空气中放置12h后、不添加CHN进行水热反应后以及添加CHN进行水热反应后的X射线衍射对比图。
图2是多层MXene在空气中放置12h后、不添加CHN进行水热反应后以及添加CHN进行水热反应后的扫描电镜对比图。
图3是实施例1中MAX和多层MXene的X射线衍射图。
图4是实施例1中多层MXene、MXene/TiO2复合材料及H-MXene纳米片的X 射线衍射图。
图5是实施例1中多层MXene及H-MXene纳米片的拉曼光谱图。
图6是实施例1中多层MXene(a)、MXene/TiO2复合材料(b)及H-MXene 纳米片(c)的扫描电镜照片。
图7是实施例1中多层MXene(a)、MXene/TiO2复合材料(b)及H-MXene 纳米片(c)的透射电镜照片。
图8是实施例1中多层MXene和H-MXene纳米片的BET图。
图9是实施例1中多层MXene(a)和H-MXene纳米片(b)的X射线光电子能谱图。
具体实施方式
下面结合附图和实施例对本发明技术方案进一步系统阐述说明，但是本发明保护范围不限于这些实例。
实施例1
1、将10g Ti3AlC2(MAX)缓慢加入到187.5mL质量浓度为30％的氟化氢水溶液中，室温下缓慢搅拌72h使其中Al元素被完全刻蚀掉，将刻蚀后物质用去离子水洗涤至滤液为中性，冷冻干燥后得到多层MXene。
2、取100mg多层Mxene分散到40mL蒸馏水和乙醇体积比为1:1的混合液中，超声1h后搅拌24h，再加60mg六亚甲基四胺，在反应釜中150℃水热反应5h，所得产物用水和乙醇洗涤至中性后，60℃真空干燥，得到MXene/TiO2复合材料。该步骤中，若直接将多层Mxene放置在空气中，不添加六亚甲基四胺(CHN)，且不进行水热反应，即使放置12h，多层MXene也不容易被氧化成TiO2，XRD第一个衍射峰不向小角度发生偏移(见图1中Eaching Al和图2a)；若将多层Mxene加入反应釜中但不添加CHN进行水热反应，多层MXene也极少被氧化(见图1中No CHN和图2b)，而添加CHN后进行水热反应，多层MXene发生明显氧化，第一个衍射峰明显向小角度偏移，是由于生成较多TiO2颗粒后，使片层间距增加，进一步证明在CHN作用下MXene被催化氧化成TiO2物质(见图1中CHN和图2c)，说明在水热过程中CHN对氧化具有促进作用。
3、将100mg MXene/TiO2复合材料加入50mL质量浓度为30％的氟化氢水溶液中去除TiO2，反应迅速产生大量气泡，气泡消失后用去离子水洗涤至中性，得到二维孔洞化MXene纳米片(H-MXene)。
如图3所示，Ti3AlC2(MAX)在氢氟酸刻蚀后，位于39°处衍射峰消失，证明刻蚀完全，形成多层MXene结构，同时图4曲线表明形成孔洞结构XRD保持不变，因此说明孔洞化后不影响MXene主体结构。图5拉曼光谱结果表明，普通MXene 在197、287、391、601、714cm-1处出现拉曼信号，其中197、714cm-1处对应于 Ti-C的A1g的对称面外振动，而287、391、601cm-1为Ti、C和表面平面官能团原子的面内剪切振动，形成孔洞化结构后，MXene的拉曼信号不发生改变，但强度略有减弱，同时在150cm-1附近代表TiO2的拉曼信号不存在，这表明将TiO2在氢氟酸作用下完全去除且MXene孔洞化过程中没有发生二次氧化。从图6中可以看出，通过水热反应在MXene片层表面出现明显颗粒状物质，对应于生成的TiO2，粒径大小约为20nm，后续经过氢氟酸处理，TiO2颗粒消失，MXene片层上形成孔洞化结构。为进一步表征孔洞结构，采用透射电镜对材料进行表征，如图7所示。从图 7a中可以看到，普通MXene纳米片上不存在孔隙结构，经过孔洞化处理后，其片层表面明显出现孔洞结构(图7b)，从暗场相中可以更直观的观察到(图7c)，比表面积测试结果显示孔洞化后MXene比表面积从10cm2/g增加至35cm2/g，这是由于孔洞结构存在使其比表面积增大(见图8)。使用X射线光电子能谱进行分析 (图9)，对MXene进行孔洞化处理后，其元素组成和价态不发生改变。结果证明使用该方法对MXene进行孔洞化处理不改变其晶体结构和化学性质。
实施例2
本实施例的步骤2中，在反应釜中120℃水热反应12h，其他步骤与实施例1 相同，得到二维孔洞化MXene纳米片。
实施例3
本实施例的步骤2中，在反应釜中160℃水热反应8h，其他步骤与实施例1 相同，得到二维孔洞化MXene纳米片。
Claims (5)
1.一种大片层可控孔洞化MXene纳米片的制备方法，其特征在于：
(1)将Ti3AlC2粉末加入到氢氟酸中，搅拌充分反应使其中Al元素被完全刻蚀掉，将刻蚀后物质洗至中性后冷冻干燥，得到多层MXene；
(2)将多层MXene加入到蒸馏水和乙醇的混合液中，超声分散30～60分钟后搅拌10～24小时，再加入六亚甲基四胺，在反应釜中120～160℃水热反应5～12小时，所得产物用水和乙醇洗涤至中性后真空干燥，得到MXene/TiO2复合材料；
(3)利用过量氢氟酸处理MXene/TiO2复合材料以去除TiO2，得到二维孔洞化MXene纳米片。
2.根据权利要求1所述的大片层可控孔洞化MXene纳米片的制备方法，其特征在于：所述氢氟酸是质量浓度为25％～35％的氟化氢水溶液。
3.根据权利要求1所述的大片层可控孔洞化MXene纳米片的制备方法，其特征在于：步骤(2)中，所述多层MXene与六亚甲基四胺的质量为1：0.5～0.8。
4.根据权利要求1或3所述的大片层可控孔洞化MXene纳米片的制备方法，其特征在于：步骤(2)中，在反应釜中150℃水热反应5小时。
5.根据权利要求1或3所述的大片层可控孔洞化MXene纳米片的制备方法，其特征在于：步骤(2)中，所述混合液中蒸馏水和乙醇的体积比为1：1。
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