一种介孔结构海胆状NiCo2O4/立体构筑石墨烯微球复合材料的制备方法及应用，包括如下步骤：(1)先将立体构筑石墨烯用氧化性酸在高压反应釜中处理，经水洗、干燥后得到亲水性的立体构筑石墨烯；(2)将亲水性的立体构筑石墨烯通过超声法分散在水中，然后加入钴盐、镍盐、表面活性剂和沉淀剂，充分搅拌形成均匀溶液；(3)将混合溶液进行水热反应得到钴酸镍前驱体；(4)将钴酸镍前驱体在空气气氛中煅烧得到介孔结构NiCo2O4/立体构筑石墨烯微球复合物。本发明制备工艺简单、环保、原料来源广，产品电化学性能。利用该材料制备的锂离子电池负极材料在首次放电中的比容量高达1403mA h g‑1。用作钠离子电池负极材料时，首次放电比容量高达818.4mA h g‑1。
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