Developing an efficient and reliable method for achieving high-yield and high-quality synthesis of transition metal sulfides combined with carbonaceous materials is highly desirable but still challenging. Herein, a very simple and cost-effective solid state reaction method for the fabrication of ultrafine CoS nanoparticles encapsulated within heteroatom-doped carbon scaffold is presented. By directly grinding cobalt acetate tetrahydrate, o-vanillin and o-phenylenediamine together with a molar ratio of 1:2:1 at ambient temperature in the presence of sulfur powder, a self-assembly solid state reaction took place to give rise to a bis-Schiff base complex with cobalt (II), which was evenly distributed in the sulfur powder surroundings. After subsequent annealing at elevated temperature, simultaneous carbonization and sulfidization occurred, resulting to the in-situ formation of ultrafine CoS nanoparticles (∼3.8 nm) encapsulated within an irregular N, S-codoped carbon scaffold (denoted as CoS⊂NSC). When evaluated as an anode material for sodium-ion batteries (SIBs), the CoS⊂NSC hybrid exhibits good cycling stability (305.6 mA h g⁻¹ after 400 cycles at 100 mA g⁻¹) and excellent rate capability (412.3 and 263.3 mA h g⁻¹ at current densities of 200 and 5000 mA g⁻¹, respectively), demonstrating exceptional electrochemical sodium storage performances. The findings in this work pave a novel way to synthesize the promising anode materials for high performance SIBs.

迫切需要开发一种高效可靠的方法，以实现与碳质材料结合的过渡金属硫化物的高产率和高质量合成，但仍具有挑战性。在此，提出了一种非常简单且具有成本效益的固态反应方法，用于制造包裹在掺杂杂原子的碳支架中的超细CoS纳米颗粒。通过直接研磨四水合醋酸钴，邻香草醛和邻钴-苯二胺与硫粉存在下于环境温度下以1：2：1的摩尔比进行的自组装固态反应生成了具有钴（II）的双席夫碱配合物，该配合物为均匀分布在硫磺粉周围。随后在高温下退火后，同时发生碳化和硫化，导致原位形成超细CoS纳米颗粒（约3.8 nm），包裹在不规则的N，S掺杂的碳支架（表示为CoS⊂NSC）中。当用作钠离子电池（SIBS），所述CoS⊂NSC混合表现出良好的循环稳定性的阳极材料进行评价（305.6毫安汞柱^-1在100mA克400次循环后^-1和优异的倍率性能（412.3和263.3毫安汞柱）^-1电流密度分别为200和5000 mA g ^-1时），证明了出色的电化学钠存储性能。这项工作中的发现为合成用于高性能SIB的有前途的阳极材料铺平了一条新途径。