the ROS molecules, hydrogen peroxide (H 2 O 2 ) is prime reactive species, whose overproduction is closely related to various diseases, including inflammation, cancer, or neurological diseases. [5][6][7][8][9] Thus it is of great importance in monitoring the concentration of H 2 O 2 in living specimens. To this end, a number of mapping tools including "dark" biological processes and radiative recombination mechanism have been developed. Chemiluminescence (CL), a kind of light emission induced by energy transfer from chemical reactions, has evoked considerable interest as one ultrasensitive chemical analysis method with quantification and localization. [10][11][12] Without auto-fluorescent interference and phototoxicity from high-energy excitation light, CL shows high signal-to-noise ratio and low perturbation in sensing H 2 O 2 in vivo compared to photoluminescence (PL) method. [13][14][15] Moreover, unlike the bioluminescence probe requiring the activation of bioactive enzyme, CL imaging of H 2 O 2 is a process of nonenzymatic reaction employing a H 2 O 2 -responsive peroxalate that can transfer chemical energy to the CL emitter. Nevertheless, current CL reporters on H 2 O 2 concentrate mainly on small-molecular dyes, semiconducting polymer, and aggregation induced emission nanoparticles, which suffer from low efficiency, short emission wavelength, and low chemical stability in highly oxidative ROS. [16,17] Thereby, it is meaningful to develop new class of CL nanosensors for the imaging and detecting ROS in vitro and in vivo.Carbon nanodots (CDs), which are considered as discrete quasi-spherical nanoparticles with sizes less than 10 nm, are one kind of promising nanomaterials in bioimaging, photocatalysis, optoelectronics, and sensing owing to its unique properties such as high emission efficiency, good biocompatibility, high photo-stability, and tunable luminescence. [18][19][20][21][22][23][24][25][26][27][28] Recently, the CL properties of CDs in peroxlate-H 2 O 2 system have been investigated, and it has been found that multicolor bright and persistent CL can be obtained from CDs. [29] Therefore, it is practicable to develop versatile CL probes based on CDs to detect ROS via in vivo or in vitro imaging. In general, there are several advantages for CDs as the CL imaging probes: (i) CDs exhibit excellent light emission ability and the luminescence property can be tuned by different methods; [30,31] (ii) CDs with emission Reactive oxygen species (ROS) are generated in the body and related to many pathophysiological processes. Hence, detection of ROS is indispensable in understanding, diagnosis, and treatment of many diseases. Here, near-infrared (NIR) chemiluminescent (CL) carbon nanodots (CDs) are fabricated for the first time and their CL quantum yield can reach 9.98 × 10 −3 einstein mol −1 , which is the highest value ever reported for CDs until now. Nanointegration of NIR CDs and peroxalate (P-CDs) through the bridging effect of amphiphilic triblock copolymer can serve as turn-on probes for the detection an...