properties, high atom utilization efficiency and excellent performance for different electrocatalytic applications. [11][12][13][14][15][16] Typically, the discrete Ni-N x moieties supported on NC materials have demonstrated considerable activity for electrochemical CO 2 reduction but still require further improvement. [17][18][19][20][21] Apart from the local electronic structure of the metal centers, [22][23][24][25] the number of accessible active centers and mass transfer characteristics play critical roles in the final activity of M-NC catalysts. [26,27] But only a small fraction of isolated metal sites can be regarded as active sites for most M-NC catalysts fabricated using the pyrolysis method. [27,28] One of the main reasons for this drawback is that many single-metal sites are buried in the dense carbon framework or hosted in the inaccessible micropores. These unavailable sites will not be involved in the catalytic reaction. For example, ZIF-8, a typical zeolitic imidazolate framework (ZIF), has been widely used for preparing M-NC catalysts. [29] Unfortunately, the resulting dense carbon framework impedes the mass transfer and blocks many metal sites. [27,30] Therefore, it is highly desirable to unleash the active sites for more efficient catalysis by rational structural design.A favorable architecture of catalysts, featuring 3D open structures, mesopores, or hollow space, holds the potential to enhance the mass transfer and increase the number of available single-atom moieties. These advantages will eventually enhance the apparent activity of single-atom catalysts. Some advanced carbon-based architectures modified with single-atom sites have been constructed for efficient catalytic reactions. [26,27,[30][31][32][33] For instance, mesoporous NC materials loaded with single-Co or single-Fe centers have been prepared using a SiO 2 coating strategy and exhibit enhanced oxygen reduction performance. [26,27] These studies highlight the critical role of spatial structure in the activity of single-atom catalysts. Exploring novel approaches towards unique architectures is highly promising for maximizing the performance of single-atom catalysts but remains as a challenge.In this work, a zeolitic tetrazolate framework (ZTF) possessing dual linkers is developed as the precursor for fabricating assembled hollow plates (AHP) of N-rich carbon (NC), thereafter designated as NC(AHP). A schematic of this facile synthetic strategy is presented in Figure 1. First, novel assembled plates (AP) of ZTF (designated as ZTF(AP)) are prepared by employing both 2-methylimidazole (2-Mim) andThe rational design of catalysts' spatial structure is vitally important to boost catalytic performance through exposing the active sites, enhancing the mass transfer, and confining the reactants. Herein, a dual-linker zeolitic tetrazolate framework-engaged strategy is developed to construct assembled hollow plates (AHP) of N-rich carbon (NC), which is loaded with single-Ni atoms to form a highly efficient electrocatalyst (designated as Ni-NC(AHP...