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

doi:10.6023/A25100334

摘要/Abstract

采用直流电弧等离子体法, 以Zn粉, Er₂O₃和Yb₂O₃粉末为反应原料, 在氧气环境中成功制备了ZnO:Er³⁺/Yb³⁺分级纳米棒. 通过多种表征手段(X射线衍射、Raman、X射线光电子能谱、扫描电子显微镜、透射电子显微镜和光致发光光谱), 系统分析了样品的晶体结构, 形貌和上转换发光性能. 在980 nm激光激发下, 样品在525 nm、546 nm以及662 nm呈现了发光峰. 变温发光(298~573 K)测试表明, 基于热耦合能级(²H_11/2和⁴S_3/2)和非热耦合能级(⁴S_3/2和⁴F_9/2)荧光强度比, 其最大相对灵敏度分别可达到1.03 %•K⁻¹和2.20 %•K⁻¹, 而基于⁴S_3/2能级荧光寿命的最大相对灵敏度更是高达2.43 %•K⁻¹. 本研究利用单一发光中心实现了三模态光学测温, 证明该分级纳米棒在宽温度范围内具有优异的信号区分度和高灵敏度, 在光学测温领域展现出重要应用潜力.

关键词: 氧化锌, 稀土掺杂, 光学测温, 上转换发光, 荧光寿命

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

引用此文

刘庆, 陈双龙, 王秋实, 王雪娇, 刘才龙. 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[J]. 化学学报, 2026, 84(2): 196-207.

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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图/表 15

图1. (a)未掺杂的ZnO和ZnO:Er3+/Yb3+分级纳米棒的XRD图谱, 插图为(100), (002)和(101)峰的放大图; (b) Raman光谱

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

图2. (a) ZnO:Er3+/Yb3+分级纳米棒的XPS全扫描谱图, (b) Zn 2p, (c) O 1s, (d) Er 4d和(e) Yb 4d峰的XPS高分辨率图谱

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

图3. ZnO:Er3+/Yb3+分级纳米棒的(a)低倍率、(b)高倍率SEM图像, (c) EDS能谱, (d)低倍率、(e)高倍率TEM图像, (f) HRTEM图像, (g) HAADF图像和(h) Zn、(i) O、(j) Er、(k) Yb元素分布

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

图4. 未掺杂的ZnO和ZnO:Er3+/Yb3+分级纳米棒的(a) 980 nm激光激发下的上转换发光光谱和(b)漫反射光谱

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

图5. (a)未掺杂的ZnO和(b) ZnO:Er3+/Yb3+分级纳米棒的带隙分析曲线图

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

图6. (a)不同激发功率下ZnO:Er3+/Yb3+分级纳米棒的上转换发光光谱(激光功率: 0.5~1.2 W, 对应功率密度: 5~12 W/cm2); (b) 525 nm、546 nm及662 nm处发射峰积分强度与激发功率的关系

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

图7. ZnO:Er3+/Yb3+分级纳米棒中Er3+和Yb3+的激发和发射机理(λex=980 nm)

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

图8. 不同温度下ZnO:Er3+/Yb3+分级纳米棒的(a)上转换发光光谱; (b) 525 nm、546 nm及662 nm处发射峰积分强度随温度的变化关系

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

图9. ZnO:Er3+/Yb3+分级纳米棒的(a) FIR(I525 nm/I546 nm)随温度的变化, 插图为FIR(I525 nm/I546 nm)的循环测试; (b)相对灵敏度Sr及温度分辨率δT随温度的变化

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

表1. Er3+/Yb3+掺杂不同基质材料的基于荧光强度比的光学参数

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

图10. FIR(I525 nm/I546 nm)的对数与绝对温度倒数的关系图

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

图11. ZnO:Er3+/Yb3+分级纳米棒的(a) FIR(I662 nm/I546 nm)随温度的变化, 插图为FIR(I662 nm/I546 nm)的循环测试; (b)相对灵敏度Sr及温度分辨率δT随温度的变化

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

图12. ZnO:Er3+/Yb3+分级纳米棒的546 nm处的平均寿命随温度的变化

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

图13. ZnO:Er3+/Yb3+分级纳米棒的(a) 546 nm处的荧光寿命随温度的变化; (b)相对灵敏度Sr及温度分辨率δT随温度的变化

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

表2. Er3+/Yb3+掺杂不同基质材料的基于荧光寿命的光学参数

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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