Peng Jin, Wenlong Tan, Jia Huo*, Tingting Liu, Yu Liang, Shuangyin Wang,*and Darren Bradshaw* S1. Experimental Section S2. Preparation and characterization of interfacial nanoassembly/ emulsion polymerization S3. Generality of interfacial nanoassembly/ emulsion polymerization

在本次研究中，实验团队设计了一个简单而强大的硫化策略，首次合理设计空心TiO2@Co9S8芯分支阵列，作为碱性介质中OER和 HER的坚固双功能电催化器。无绑定 TiO2@Co9S8 芯分支阵列，被证明具有较大的孔隙度/表面积，从而使其具有更快的离子/电子传输速率和更好的结构稳定性。

硫和氮双掺杂石墨烯纤维（SNGF）是由优化的化学气相沉积制成的。SNGF具有稳定的三维纤维结构、高表面积、丰富的中孢、S原子和N原子的均匀分布等缺陷。作为超级电容器的电极，SNGF 的特定电容达到 311 F g-1。SNGF//SNGF 对称超级电容器可提供 42.7 W h kg-1 和 14.8 kW kg-1 的最大能量和功率密度，具有出色的循环稳定性（5000 次循环后保持 92.2% 的电容）。结果表明，SNGF是超级电容器的高质量电极材料的候选产品。

能量密度和循环稳定性是锂硫电池实用化过程中的巨大挑战。通常采用轻质的非极性碳材料作为硫载体，但锂硫电池的循环稳定性和体积能量密度依然不够理想。本工作以质地较重的钴酸镍纳米纤维作为非碳硫载体，构筑了复合硫正极材料。

MgO nanofiber with good morphology was difficult to obtain through high temperature heat-treatment due to the widely existed pulverization phenomenon, which restricted its applications in the high-temperature field. In this work, MgO nanofibers were prepared by electrospinning through mixed precursors: magnesium acetate (MA) and magnesium citrate (MC). The fiber with MC mass content in the range of 30–50% exhibited good hightemperature stability and the original feature was preserved after heat-treated at 1000 °С. A plausible formation mechanism of the polycrystalline MgO nanofibers was provided in the present paper. Suitable confection of MA and MC brought a milder decomposition process and led to a more compact structure of MgO nanofiber, which contributed to the excellent high-temperature stability. The considerable effects of microstructure on thermal