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柔性储能器件是可穿戴电子设备与智能纺织品走向实用的核心关键。在众多柔性储能体系中，纤维型锌离子混合超级电容器兼具锌金属的高容量优势和超级电容器的高功率特性，且具有宽电压窗口、高能量密度、本质安全等突出优点，近年来备受关注。然而，如何同时实现高面积电容、高能量密度和超长循环寿命，并有效抑制锌枝晶生长，仍是ZIHSCs迈向实用化面临的关键挑战。
MXene（Ti?C?T?）因其超高体积电容、优异金属导电性和丰富表面化学，是柔性电极的理想材料。但传统MXene纤维制备方法难以同时实现片层高度取向与多孔结构的协同调控——致密堆积有利于导电但限制离子传输，多孔结构有利于离子扩散但牺牲导电性。此外，MnO?作为高容量电池型正极材料，其本征低导电性和纳米颗粒易团聚问题严重制约了电化学性能的发挥。
本文，北京服装学院Mei Zhang等在《Journal of Materials Chemistry A》期刊发表名为"Flexible zinc-ion hybrid supercapacitors with high energy density and long cycling life enabled by the microfluidic assembly of MXene composite fibers"的论文。该研究提出了微流控辅助湿法纺丝技术，精确制备了高度取向且多孔的MXene纤维，并通过原位生长法在MXene纤维表面均匀沉积MnO?纳米颗粒，构建了MXene/MnO?复合纤维正极，同时制备了rGO/MXene复合纤维负极，组装了高性能柔性锌离子混合超级电容器。
该策略的核心创新在于：(1) 微流控湿法纺丝——通过微通道内的剪切力精确调控MXene片层的高度取向排列，同时利用凝固浴的相分离过程在纤维内部构建多孔结构，实现高导电性与快速离子传输的兼顾；(2) 原位生长MnO?——纳米级MnO?均匀沉积在MXene纤维多孔骨架上，MXene的导电网络有效缓解了MnO?的团聚问题并提供快速电子传输通道；(3) 正负极匹配设计——MXene/MnO?电池型正极 + rGO/MXene电容型负极 + ZnSO?水系电解液，有效抑制锌枝晶，将电压窗口扩展至?0.1~1.5 V。优化后的柔性ZIHSCs实现了1356 mF cm?2的高面积电容和120.5 μWh cm?2的能量密度，在PVA/ZnCl?–MnSO?凝胶电解液中经10000次循环后容量保持率接近100%。
图文导读
图1、Fabrication of the MXene composite fibers via microfluidics for flexible supercapacitors. (a) Preparation processes of MXene/MnO2 composite fibers. (b) Preparation processes of rGO/MXene composite fibers. (c) Assembly and application of flexible ZIHSCs.
图2、(a)–(c) Surface SEM images of the MXene/MnO2-2 fibers under different magnifications. (d) and (e) Cross-sectional SEM images and (f) EDX elemental mapping images of the MXene/MnO2-2 fibers. (g) XRD patterns of MAX, MXene, MnO2 and MXene/MnO2. (h) XPS survey spectrum of the MXene/MnO2-2 fibers. (i) C 1s, (j) Ti 2p, (k) O 1s and (l) Mn 2p XPS spectra of the MXene/MnO2-2 fibers.
图3、Electrochemical performance of the flexible symmetric supercapacitors assembled from the MXene fibers prepared using different spinning channels in a 0–1 V voltage window of the PVA/H2SO4 electrolyte: (a) GCD curves at a current density of 0.6 mA cm?2, (b) specific areal capacitance comparisons, and (c) CV curves at a scan rate of 100 mV s?1. Electrochemical performance of FSCs assembled using the MXene composite fibers with various amounts of MnO2 in the PVA/H2SO4 gel electrolyte: (d) GCD curves at a current density of 0.8 mA cm?2, (e) specific areal capacitance comparison at current densities of 0.4–2.0 mA cm?2, (f) CV curves at 100 mV s?1, and (g) EIS curves, with the equivalent circuit diagram as an inset. Electrochemical performance of FSCs assembled using the MXene/MnO2-2 fibers: (h) GCD curves at 0.4–2.0 mA cm?2 and (i) CV curves at 5–100 mV s?1.
图4.(a) and (b) SEM images of the surface and cross-section of the 30% rGO/MXene fibers. (c) XPS survey spectrum of the 30% rGO/MXene fibers. (d) C 1s, (e) Ti 2p and (f) O 1s XPS spectra of the 30% rGO/MXene fibers.
图5、Electrochemical performance of a three-electrode system with a 1 M H2SO4 electrolyte: (a) comparison of the CV curves for the rGO/MXene composite fibers with different rGO contents under a voltage window of ?0.2–0.5 V and (b) CV curves of the MXene/MnO2-2 fibers and 30% rGO/MXene fibers. Electrochemical performance of the flexible ASCs assembled using the MXene/MnO2-2//30% rGO/MXene composite fibers under a voltage window of ?0.4–1.1 V in a PVA/H2SO4 gel electrolyte: (c) GCD curves at various current densities of 0.4–2.0 mA cm?2, (d) relationship between the logarithmic peak current and logarithmic scan rate, (e) contribution of the capacitive effects at scan rates of 1–10 mV s?1, and (f) capacitive response and diffusion-controlled contributions at a scan rate of 10 mV s?1.
图6、(a) CV curves of the MXene/MnO2-2 fibers and 30% rGO/MXene fibers in a three-electrode system using a 2 M ZnSO4 electrolyte. Electrochemical performance of the flexible ZIHSCs assembled using the MXene/MnO2-2//30% rGO/MXene composite fibers in an aqueous ZnSO4 electrolyte under a potential window of ?0.1–1.5 V: (b) comparison of the GCD curves at current densities of 0.6–2.0 mA cm?2, (c) CV curves at scan rates of 5–100 mV s?1, (d) EIS curves, with the equivalent circuit diagram as an inset, (e) relationship between the peak current and scan rate, (f) contribution ratio of the capacitive and diffusion-controlled processes at scan rates of 1–10 mV s?1, (g) contribution ratio of the capacitive effects at a scan rate of 10 mV s?1, and (h) comparison of the specific areal capacitance and energy density of energy storage devices at different current densities. (i) Ragone plot of the comparison of energy density and power density with those of other asymmetric supercapacitors.
图7.Electrochemical performance of the quasi-solid-state flexible ZIHSCs assembled using the MXene/MnO2-2 and 30% rGO/MXene composite fibers in a PVA/ZnCl2–MnSO4 gel electrolyte: (a) capacitance retention after 10?000 cycles at a current density of 2.0 mA cm?2 and GCD curves of the last 10 cycles; (b) GCD curves of a single and two flexible ZIHSCs connected in series; (c) GCD curves of a single and two flexible ZIHSCs connected in parallel; (d) bending stability at angles of 0°, 45°, 90°, 135° and 180° at 200 mV s?1; and (e) energy supply application of flexible ZIHSCs for an electronic watch.
小结
总而言之，该工作通过微流控辅助湿法纺丝技术精确制备了高度取向且多孔的MXene纤维，结合原位生长MnO?构建了MXene/MnO?复合纤维电池型正极，同时制备了rGO/MXene复合纤维电容型负极，组装了高性能柔性锌离子混合超级电容器。微流控纺丝实现了MXene片层取向与多孔结构的协同调控，原位生长的MnO?在MXene导电骨架中均匀分布避免了团聚，正负极匹配设计有效抑制了锌枝晶并将电压窗口扩展至1.6 V。优化后的柔性ZIHSCs实现了1392.0 mF cm?2的对称器件面积比电容、1356 mF cm?2的ZIHSCs面积比电容、120.5 μWh cm?2的能量密度，以及准固态器件10000次循环近100%容量保持的卓越稳定性。该工作为高性能柔性锌离子混合超级电容器的设计与组装提供了新思路，在可穿戴设备和智能纺织品领域具有重要的应用前景。
文献：
https://doi.org/10.1039/D6TA02290A
信息来源：材料分析与应用
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