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Topochemical transformation has emerged as a promising method for fabricating two-dimensional (2D) materials with precise control over their composition and morphology. However, the large-scale synthesis of ultrathin 2D materials with controllable thickness remains a tremendous challenge. Herein, we adopt an efficient topochemical synthesis strategy, employing a confined reaction space to fabricate ultrathin 2D Sn4P3 nanosheets in large-scale. By carefully adjusting the rolling number during the processing of Sn/Al foils, we have successfully fabricated Sn4P3 nanosheets with varied layer thicknesses, achieving a remarkable minimum thickness of two layers (~ 2.2 nm). Remarkably, the bilayer Sn4P3 nanosheets display an exceptional initial capacity of 1088 mAh·g−1, nearing the theoretical value of 1230 mAh·g−1. Furthermore, we reveal their high-rate property as well as outstanding cyclic stability, maintaining capacity without fading more than 3000 cycles. By precisely controlling the layer thickness and ensuring nanoscale uniformity, we enhance the lithium cycling performance of Sn4P3, marking a significant advancement in developing high-performance energy storage systems.
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