Two-dimensional (2D) zinc oxide (ZnO) has attracted much attention for its potential applications in electronics, optoelectronics, ultraviolet photodetectors, and resistive sensors. However, little attention has been focused on the growth mechanism, which is highly desired for practical applications. In this paper, the growth mechanism of 2D ZnO by surfactant-assisted ion-layer epitaxy (SA-ILE) is explored by controlling the amounts of surfactant, temperature, precursor concentration, and growth time. It is found that the location and the number of nucleation sites at the initial stages are restricted by the surfactant, which absorbs ions via electrostatic attraction at the water-air interface. Then, the growth of 2D ZnO is administered by the temperature, precursors, and growth time. In other words, the temperature is connected with the diffusion of solute ions and the number of nucleation sites. The concentration of precursors determines the solute ions in solution, which plays a dominant role in the growth rate of 2D ZnO, while growth time affects the nucleation, growth, and dissolution processes of ZnO. However, if the above criteria are exceeded, the nucleation sites significantly increase, resulting in multiple 2D ZnO with tiny size and multilayers. By optimizing the above parameters, 2D ZnO nanosheets with a size as large as 20 μm are achieved with 10 × 10−5 of the ratio of sodium oleyl sulfate to , 70 °C, 50 mM of precursor concentration, and 50 min of growth time. 2D ZnO sheets, are confirmed by scanning electron microscope (SEM), energy-dispersive X-ray spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), and Raman spectrum. Our work might guide the development of SA-ILE and pave the platform for practical applications of 2D ZnO on photodetectors, sensors, and resistive switching devices.

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Excitation polarized upconversion luminescence (EPUL) from lanthanide ions has attracted considerable attention due to its wide applications in microfluidics, single particle tracking, security inks, and cell internal viscosity testing. However, controlling the degree of excitation polarization (DOEP) of the EPUL remains a significant challenge. Here, the modulation of the DOEP (from 0 to 0.5) of the EPUL from Er3+ doped single nanorods by changing the concentration of doped Er3+, Yb3+, or Mn2+ is systematically studied. By analyzing the lifetimes and disproportionate changes in luminescence intensities, it is found that optimizing Er3+, Yb3+, or Mn2+ concentration can reduce non‐radiative transition and population density in excited states, leading to the enhancement of the DOEP under a good alignment of transition dipoles. Furthermore, the possibility of anti‐counterfeiting based on such tunable EPUL is illustrated. Three kinds of fine patterns with a small size of 10 µm are realized by assembling the single nanorods accurately via optical tweezers. The patterns and their EPUL guarantee double protection for the feasibility of anti‐counterfeiting. The findings of this study offer insights into the EPUL from lanthanide ions and provide a microscale platform via the EPUL for the application of multidimensional information encoding and reconfigurable double anti‐counterfeiting.