Plasma-assisted Synthesis of ZnO:Er3+/Yb3+ Hierarchical Nanorods and Their Upconversion Luminescence-based Trimodal Optical Thermometry Properties

doi:10.6023/A25100334

Abstract

Through the direct current arc discharge plasma method, ZnO:Er³⁺/Yb³⁺ hierarchical nanorod optical temperature-sensing materials were successfully prepared using Zn powder, Er₂O₃ powder, and Yb₂O₃ powder as raw materials in an oxygen (O₂) atmosphere. The crystal structure, morphological characteristics, and upconversion luminescence properties of the samples were systematically characterized through X-ray diffraction (XRD), Raman, X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), transmission electron microscopy (TEM), and photoluminescence analyses. Both XRD and Raman analyses indicated the absence of secondary phases in the samples, and the XRD and Raman spectra of ZnO:Er³⁺/Yb³⁺ exhibited a low-angle shift compared to undoped ZnO, confirming the substitution of Er or Yb ions at the main Zn lattice sites. XPS confirmed the coexistence of Zn, O, Er, and Yb elements, while energy dispersive spectroscopy (EDS) quantitative analysis revealed an atomic ratio of Zn∶O∶Er∶Yb as 47.22∶46.47∶0.81∶1.33. SEM results showed that the hierarchical nanorod structure consists of a robust main trunk and numerous radial branches grown from the main surface. Each nanorod maintained a uniform diameter along its entire length, with an average diameter ranging from 20 nm to 45 nm and a length of approximately 500 nm. High-resolution transmission electron microscopy revealed that the adjacent lattice fringe spacing of the branched nanorods was about 0.271 nm, corresponding to the (002) plane spacing of wurtzite-type ZnO, confirming their well-crystallized single-crystal structure. This result also indicated that the [001] crystal orientation is the primary growth direction of the ZnO nanorods. Photoluminescence studies identified characteristic emission peaks at 525 nm, 546 nm, and 662 nm in the visible region, attributed to the intra-4f electronic transitions of Er³⁺ ions. Through temperature-dependent luminescence tests from 298 K to 573 K, the maximum relative sensitivities of the fluorescence intensity ratios for the thermally coupled levels (²H_11/2 and ⁴S_3/2) and non-thermally coupled levels (⁴S_3/2and ⁴F_9/2) were determined to be 1.03 %•K⁻¹ and 2.20 %•K⁻¹, respectively, while the maximum relative sensitivity of the ⁴S_3/2 level fluores- cence lifetime was 2.43 %•K⁻¹. In this study, a single luminescent center is used to achieve three-mode optical temperature measurement. The ZnO:Er³⁺/Yb³⁺ hierarchical nanorod optical temperature-sensing material demonstrated excellent signal discrimination and high sensitivity across a broad temperature range, highlighting its significant potential for applications in optical temperature sensing.

Key words: zinc oxide, rare earth doping, optical temperature measurement, upconversion luminescence, fluorescence lifetime

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Qing Liu, Shuanglong Chen, Qiushi Wang, Xuejiao Wang, Cailong Liu. Plasma-assisted Synthesis of ZnO:Er³⁺/Yb³⁺ Hierarchical Nanorods and Their Upconversion Luminescence-based Trimodal Optical Thermometry Properties[J]. Acta Chimica Sinica, 2026, 84(2): 196-207.

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Fig. & Tab. 15

Figure 1. (a) XRD patterns of undoped ZnO and ZnO:Er3+/Yb3+ hierarchical nanorods, with the inset showing enlarged views of the (100), (002), and (101) peaks; (b) Raman spectra

Figure 2. (a) XPS full scan spectrum of ZnO:Er3+/Yb3+ hierarchical nanorods, high-resolution XPS spectra of (b) Zn 2p, (c) O 1s, (d) Er 4d, and (e) Yb 4d peak

Figure 3. (a) Low-magnification and (b) high-magnification SEM images, (c) EDS spectrum, (d) low-magnification and (e) high-magnification TEM images, (f) HRTEM image, (g) HAADF image and the corresponding distribution of (h) Zn, (i) O, (j) Er, (k) Yb of ZnO:Er3+/Yb3+ hierarchical nanorods

Figure 4. (a) UC luminescence spectra under 980 nm laser excitation and (b) diffuse reflectance spectra of undoped ZnO and ZnO:Er3+/Yb3+ hierarchical nanorods

Figure 5. (a) Bandgap analysis curves of undoped ZnO and (b) ZnO:Er3+/Yb3+ hierarchical nanorods

Figure 6. (a) Upconversion luminescence spectra of ZnO:Er3⁺/Yb3⁺ hierarchical nanorods under varied excitation power (Laser power: 0.5~1.2 W, corresponding power density: 5~12 W/cm2); (b) Integrated emission intensity at 525 nm, 546 nm, and 662 nm as a function of excitation power

Figure 7. Excitation and emission mechanisms of Er3+ and Yb3+ (λex=980 nm) of ZnO:Er3+/Yb3+ hierarchical nanorods

Figure 8. (a) Upconversion luminescence spectrum of ZnO:Er3+/Yb3+ hierarchical nanorods at different temperatures; (b) Temperature dependent variation of emission peak integral intensity at 525 nm, 546 nm, and 662 nm

Figure 9. (a) Temperature dependence of the FIR(I525 nm/I546 nm) for the ZnO:Er3+/Yb3+ hierarchical nanorods. The inset shows the cycling test of the FIR(I525 nm/I546 nm). (b) Temperature dependence of the relative sensitivity Sᵣ and temperature resolution δT

Er³⁺/Yb³⁺掺杂不同基质材料	跃迁能级	温度范围/K	最大相对灵敏度/(%•K⁻¹)	参考文献
NaYF₄	²H_11/2, ⁴S_3/2	198~498	0.46	[64]
β-NaGdF₄	²H_11/2, ⁴S_3/2	303~563	0.37	[65]
NaLnTiO₄	²H_11/2, ⁴S_3/2	300~510	0.45	[66]
LiGa₅O₈	²H_11/2, ⁴S_3/2	300~480	0.35	[67]
Ba₂SrLu₄O₉	²H_11/2, ⁴S_3/2 ²H_11/2, ⁴F_9/2	303~573	0.99 0.88	[13]
Ca₃Y₂Ge₃O₁₂	²H_11/2, ⁴S_3/2 ²H_11/2, ⁴F_9/2	293~473	1.29 1.09	[56]
ZnO	²H_11/2, ⁴S_3/2 ²H_11/2, ⁴F_9/2	298~573	1.03 2.20	本文

Table 1. Optical parameters based on fluorescence intensity ratio for Er3+/Yb3+ doped in different matrix materials

Figure 10. The graph of the logarithm of FIR (I525 nm/I546 nm) versus the reciprocal of absolute temperature

Figure 11. (a) Temperature dependence of the FIR(I662 nm/I546 nm) for the ZnO:Er3+/Yb3+ hierarchical nanorods. The inset shows the cycling test of the FIR(I662 nm/I546 nm). (b) Temperature dependence of the relative sensitivity Sr and temperature resolution δT

Figure 12. Variation of the average lifetime at 546 nm for ZnO:Er3+/Yb3+ hierarchical nanorods with temperature

Figure 13. (a) Fluorescence lifetime variation at 546 nm of ZnO:Er3+/Yb3+ hierarchical nanorods with temperature; (b) Temperature dependence of the relative sensitivity Sr and temperature resolution δT

Er³⁺/Yb³⁺掺杂不同基质材料	跃迁能级	温度范围/K	最大相对灵敏度/(%•K⁻¹)	参考文献
Ca₂MgWO₆	⁴S_3/2	303~573	0.11	[16]
Ba₉Y₂Si₆O₂₄	⁴S_3/2	303~483	0.14	[68]
Na₂YMg₂(VO₄)₃	⁴S_3/2	323~573	0.09	[22]
Ba₂SrLu₄O₉	⁴S_3/2	303~573	0.36	[13]
Y_{1. 88}WO₆	⁴S_3/2	303~543	0.10	[69]
Ca₃Y₂Ge₃O₁₂	⁴S_3/2	293~473	1.03	[56]
ZnO	⁴S_3/2	298~573	2.43	本文

Table 2. Optical parameters based on fluorescence lifetime for Er3+/Yb3+ doped in different host materials

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等离子体辅助合成ZnO:Er³⁺/Yb³⁺分级纳米棒及其上转换发光的三模态光学测温性能

Plasma-assisted Synthesis of ZnO:Er³⁺/Yb³⁺ Hierarchical Nanorods and Their Upconversion Luminescence-based Trimodal Optical Thermometry Properties

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等离子体辅助合成ZnO:Er3+/Yb3+分级纳米棒及其上转换发光的三模态光学测温性能