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However, its performance hinges on the design of advanced electrode materials. Herein, we proposed a novel strategy to prepare the yolk\u2010shell structured transition metal phosphides\/hollow mesoporous carbon spheres (HMCSs) composites (HZNP). The unique hollow interior effectively accommodates volume variation during ion intercalation\/deintercalation. Meanwhile, the mesoporous carbon shell offers a high specific surface area and continuous pathways for ion diffusion, thereby synergistically improving charge transfer kinetics and structural stability. The HZNP\u201020\u201030 composite demonstrates an optimal desalination capacity of 49.6 mg g\n                    <jats:sup>\u22121<\/jats:sup>\n                    . This performance is attributable to its preserved ZIF framework from ion\u2010exchange etching, which maintains chemical and structural integrity. Furthermore, the synergistic effect between the CoNi bimetallic phosphides and the N\u2010doped mesoporous carbon shell significantly enhances the electrochemical performance. This study not only provides strong theoretical support for the confined growth of metal phosphide nanoparticles in HMCSs but also verifies the superiority of the yolk\u2010shell structure in the application of CDI.\n                  <\/jats:p>","DOI":"10.1002\/smll.73129","type":"journal-article","created":{"date-parts":[[2026,3,16]],"date-time":"2026-03-16T04:51:27Z","timestamp":1773636687000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Metal\u2013Organic Framework\u2010Derived Yolk\u2010Shell Phosphides@Hollow Mesoporous Nanosphere Architecture for Capacitive Deionization"],"prefix":"10.1002","volume":"22","author":[{"given":"Songtao","family":"Zhang","sequence":"first","affiliation":[{"name":"School of Chemistry and Materials Testing Center Yangzhou University  Yangzhou P. R. 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