持久发光纳米颗粒(PLNPs)在生物成像、癌症治疗、应力感知和光生物催化等领域展示了特殊优势。然而，缺乏对PLNPs进行可控合成以得到均匀形态和强持久发光的方法严重制约了PLNPs的应用。在此，我们报告了通过非化学计量反应改变氧化锌镓锗酸盐（ZGGO）PLNPs的电子结构，可制备出具有可控大小和持久发光的高度均一纳米立方体。通过非化学计量增加ZGGO中锗/镓比例，ZGGO PLNPs从纳米立方体和小纳米球的混合体转化为高度均匀且对称的大纳米立方体，并使持久发光强度增强了约3.7倍。此外，我们发现ZGGO PLNPs对活性氧自由基（ROS）具有响应性，即ZGGO的持久发光可以被ROS猝灭。通过开发的PLNPs实现了自荧光血清ROS检测。此外，基于ZGGO PLNPs对H2O2的响应性设计了一种葡萄糖氧化酶(GOx)的生物传感测定方法。这项研究为更好地控制PLNPs的大小、形貌和持久发光提供了一种新途径，并进一步促进了PLNPs在从诊断治疗到太阳能利用等领域的应用。

Persistent luminescence nanoparticles (PLNPs) have shown special advantages in areas such as bioimaging, cancer therapy, stress sensing, and photo-biocatalysis. However, the lack of methods for controllable synthesis of PLNPs with uniform morphologies and strong persistent luminescence has seriously hindered the applications of PLNPs. Herein, we reported that modifying the electronic structures of zinc gallogermanate (ZGGO) PLNPs by nonstoichiometric reactions can produce highly uniform nanocubes with controllable size and persistent luminescence. By nonstoichiometric increase of the Ge/Ga ratio in ZGGO, the ZGGO PLNPs were transformed from a mixture of nanocubes and small nanospheres into highly symmetrical and uniform large nanocubes, accompanied by the enhancement of persistent luminescence intensity by about 3.7 times. Moreover, we found that ZGGO PLNPs were responsive to reactive oxygen species (ROS), that is, the persistent luminescence of ZGGO can be quenched by ROS. Autofluorescence-free serum ROS detection was achieved with the developed PLNPs. Further, a biosensing assay for glucose oxidase (GOx) was designed based on the responsiveness of ZGGO PLNPs to H2O2. This study may pave a new way for better control of PLNPs' size, morphology, and persistent luminescence, and it can further promote the applications of PLNPs in areas ranging from theranostics to solar energy utilization.