本发明公开了一种纤维状MXene负载NiCoS复合材料，以四水合乙酸镍、乙酸钴、均苯三甲酸、1,4‑二氮杂双环[2,2,2]辛烷和十二烷基硫酸钠为原料，经水热反应制得NiCo‑MOFs；以Ti3AlC2、氟化锂和浓盐酸为原料，经刻蚀处理和震荡处理得到纤维状MXene；最后，以NiCo‑MOFs为前驱体，纤维状MXene为基体，加入硫代乙酰胺，经第二次水热反应，在纤维状MXene表面均匀负载颗粒状NiCoS复合材料即可制得；少层片状MXene具有微米的片状结构；纤维状MXene为直径为10‑40 nm的纤维状结构；颗粒状NiCoS的直径为5‑30nm。其制备方法包括以下步骤：1，NiCo‑MOFs的制备；2，纤维状MXene的制备；3，NiCoS@MXene的制备。作为超级电容器电极材料的应用，比电容为1300‑1500 F g‑1；能量密度高达63.3 W h kg‑1；10000圈循环后的循环稳定性保持为原始的73%。
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