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However, previous studies have mainly focused on the complete transformation from MAX phases to MXene, whereas the controllable synthesis and structural elucidation of intermediate products remain largely unexplored. Here, by tuning the etching time in a CuCl\n                    <jats:sub>2<\/jats:sub>\n                    \u2010based molten\u2010salt system, controllable structural evolution from Nb\n                    <jats:sub>2<\/jats:sub>\n                    GaC to Nb\n                    <jats:sub>2<\/jats:sub>\n                    CT\n                    <jats:italic>\n                      <jats:sub>x<\/jats:sub>\n                    <\/jats:italic>\n                    is achieved. A series of intermediate products, denoted as Nb\n                    <jats:sub>2<\/jats:sub>\n                    GaC\u2010\n                    <jats:italic>n<\/jats:italic>\n                    , are successfully isolated. With increasing etching time, the interlayer Cu and Ga contents gradually decrease, enabling precise tuning of the interlayer atomic configuration. Synchrotron x\u2010ray absorption fine structure spectroscopy reveals that the controlled etching process induces electronic\u2010structure modulation and short\u2010range structural disorder. Benefiting from the optimized local atomic environment, the intermediate heterostructure delivers enhanced lithium\u2010storage performance, including a high reversible capacity of 281 mAh g\n                    <jats:sup>\u22121<\/jats:sup>\n                    at 0.1 A g\n                    <jats:sup>\u22121<\/jats:sup>\n                    and remarkable cycling stability, with 177 mAh g\n                    <jats:sup>\u22121<\/jats:sup>\n                    retained after 2000 cycles at 1.0 A g\n                    <jats:sup>\u22121<\/jats:sup>\n                    . This work establishes a viable strategy for engineering MXene\u2010based heterostructures with tailored local atomic configurations.\n                  <\/jats:p>","DOI":"10.1002\/smtd.71093","type":"journal-article","created":{"date-parts":[[2026,10,7]],"date-time":"2026-10-07T06:10:06Z","timestamp":1791353406000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Stage\u2010Controlled Synthesis of MXene\/MAX Heterostructures With Local Atomic Disorder for Enhanced Lithium\u2010Ion Storage"],"prefix":"10.1002","author":[{"given":"Xiaoyu","family":"Han","sequence":"first","affiliation":[{"name":"National Synchrotron Radiation Laboratory State Key Laboratory of Precision and Intelligent Chemistry School of Nuclear Science and Technology University of Science and Technology of China  Hefei Anhui China"},{"name":"Spallation Neutron Source Science Center  Dongguan Guangdong 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