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采用直流电弧等离子体法, 以Al粉和Er2O3粉为原料, 在氮气环境下, 成功制备出了具有松树状纳米结构的Er3+掺杂AlN (AlN:Er3+)材料. 通过X射线衍射、X射线光电子能谱、能量色散光谱、扫描电子显微镜、透射电子显微镜和高分辨率透射电子显微镜的分析, 详细测定了松树状纳米结构的成分、形貌特征和显微结构. 结果显示, 该材料呈现出典型的六方纤锌矿晶体结构, 其形态由主干与分支纳米线交织而成, 且证实Er3+成功掺入其晶格中. 光致发光光谱显示, AlN:Er3+能够发出强烈的绿光(～548 nm), 并伴有多个发光峰, 分别对应于Er3+内层4f电子跃迁的特征发光峰. 根据不同温度下热耦合能级(2H11/2/4S3/2→4I15/2)发光光谱强度的比值, 在温度为293 K时获得最高相对灵敏度, 为1.9×10–2 K–1. 磁学测量表明, AlN:Er3+显现出明显的室温铁磁性. 通过第一性原理计算后发现其磁矩主要由Al空位周围N原子的2p轨道电子自旋极化产生. AlN:Er3+松树状纳米结构在光电器件、温敏传感器以及稀磁半导体等多个领域展现出潜在的应用前景.Erbium-doped aluminum nitride (AlN:Er3+) pine-shaped nanostructures are synthesized, through a direct reaction between aluminum (Al) and erbium oxide (Er2O3) mixed powders in a nitrogen (N2) atmosphere, by using a direct current arc discharge plasma method. X-ray diffraction (XRD) analysis reveals that the diffraction peaks of AlN:Er3+ shift towards lower angles for the doped sample compared with those of undoped AlN, indicating lattice expansion due to Er3+ incorporation. X-ray photoelectron spectroscopy (XPS) confirms that Al, N, and Er are coexistent, while energy-dispersive X-ray spectroscopy (EDS) quantitatively shows that the atomic ratio for Al:N:Er is about 46.9∶52.8∶0.3. The nanostructures, resembling pine trees, are measured to be 5–10 μm in height and 1–3 μm in width, with branch nanowires extending 500 nm–1 μm in length and 50–100 nm in diameter. These branches, radiating at about 60° from the main trunk, are found to grow along the [100] direction of wurtzite-structured AlN, as evidenced by high-resolution transmission electron microscopy (HRTEM) showing lattice spacing of 0.27 nm corresponding to the (100) plane. Photoluminescence studies identify distinct emission peaks in the visible region (527, 548, and 679 nm) and near-infrared region (801, 871, and 977 nm), which is attributed to intra-4f electron transitions of Er3+ ions. The average lifetime of the excited state at 548 nm is measured to be 9.63 μs, slightly shorter than those of other Er3+-doped materials. The nanostructures demonstrate that the superior temperature sensing capability possesses a maximum relative sensitivity of 1.9×10–2 K–1 at 293 K, based on the fluorescence intensity ratio of thermal-coupled levels (2H11/2/4S3/2). Magnetic characterization reveals that the room-temperature ferromagnetism has a saturation magnetization of 0.055 emu/g and a coercive field of 49 Oe, with a Curie temperature exceeding 300 K, which shows the potential for room-temperature spintronic applications. First-principle calculations attribute the observed ferromagnetism to Al vacancies, whose formation energy is significantly reduced by Er doping, leading to a high concentration of Al vacancies. These findings highlight the potential of AlN:Er3+ pine-shaped nanostructures in various applications, including optoelectronics, temperature sensing, and dilute magnetic semiconductors.
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Keywords:
- aluminum nitride /
- photoluminescence /
- temperature sensitive /
- dilute magnetic semiconductor
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图 1 未掺杂AlN和AlN:Er3+松树状纳米结构的XRD图谱(插图为(100), (002), (101)峰的放大图)
Fig. 1. XRD patterns of undoped AlN and AlN:Er3+ pine-shaped nanostructure (the enlarged (100), (002) and (101) peaks in inset).
图 2 AlN:Er3+松树状纳米结构的(a) XPS全图谱, 以及(b) Al 2p, (c) N 1s, (d) Er 4d的高分辨率图谱
Fig. 2. XPS patterns of AlN:Er3+ pine-shaped nanostructure: (a) Survey spectrum; high resolution spectra for (b) Al 2p, (c) N 1s, (d) Er 4d.
图 3 (a)—(c) AlN:Er3+松树状纳米结构从低倍到高倍的SEM图像; (d) EDS图谱
Fig. 3. (a)–(c) Scanning electron microscopy images from low to high magnification of AlN:Er3+ pine-shaped nanostructure; (d) EDS spectrum.
图 4 AlN:Er3+松树状纳米结构的(a) TEM图像、(b) HRTEM图像、(c) FFT图像和(d) EDS元素映射图像
Fig. 4. (a) TEM image, (b) HRTEM image, (c) FFT pattern and (d) EDS element mapping of AlN:Er3+ pine-shaped nanostructure.
图 5 (a)未掺杂的AlN和AlN:Er3+松树状纳米结构的漫反射光谱; (b) AlN:Er3+松树状纳米结构在548 nm处的激发光谱; (c)室温下AlN:Er3+松树状纳米结构在可见光(378 nm激发)到红外光(532 nm激发)范围内的发射光谱(插图为可见光范围内的光致发光成像); (d) Er3+能级跃迁图
Fig. 5. (a) DRSs of undoped AlN and AlN:Er3+ pine-shaped nanostructure; (b) excitation spectrum of AlN:Er3+ pine-shaped nanostructure at 548 nm; (c) the room-temperature Vis-NIR emission spectrum of AlN:Er3+ pine-shaped nanostructure (the visible PL imaging in inset); (d) the schematic energy level diagram for Er3+ ions.
图 7 (a)不同温度下AlN:Er3+松树状纳米结构的PL光谱; (b) AlN:Er3+松树状纳米结构在293—553 K的FIR (I527 nm/I548 nm)及对其随温度变化线性拟合结果(三角形标记代表FIR的实验值, 虚线为拟合曲线); 相对灵敏度Sr随温度的变化(菱形标记代表Sr的值)
Fig. 7. (a) Temperature-dependence spectra of AlN:Er3+ pine-shaped nanostructure; (b) FIR values of AlN:Er3+ pine-shaped nanostructure at the temperature of 293−553 K and the linear fitted results between the FIR and the temperature (the triangular markers represent the experimental values of FIR, and the dashed line is the fitting curve); the variation of relative sensitivity (Sr) with temperature (the diamond markers represent the values of Sr).
图 8 (a)室温下AlN:Er3+松树状纳米结构的磁滞回线; (b)单位磁化强度随温度的变化
Fig. 8. (a) Magnetization hysteresis loops of AlN:Er3+ pine-shaped nanostructure measured at room temperature; (b) variation of unit magnetization intensity with temperature.
图 9 自旋极化态密度图 (a) ErAl体系; (b) ErAl + VN体系; (c) ErAl + VAl体系; 正值为自旋向上, 负值为自旋向下, 费米能级用垂直虚线来表示
Fig. 9. Total DOS and partial DOS of Er atom, Al atom and N atom for (a) ErAl system, (b) ErAl + VN system, (c) ErAl + VAl system. The Fermi level is indicated by the vertical dashed line.
图 10 自旋电荷密度的空间分布 (a) ErAl体系; (b) ErAl + VN体系; (c) ErAl + VAl体系
Fig. 10. Spatial distribution of the spin density: (a) ErAl system; (b) ErAl + VN system; (c) ErAl + VAl system.
表 1 基于FIR技术对Er3+掺杂不同材料的相对灵敏度(Sr)进行比较
Table 1. Comparison of relative sensitivity (Sr) of Er3+ doped different materials based on FIR technology.
下载: 导出CSV
表 2 VAl和ErAl + VAl体系在富Al和富N条件下的形成能
Table 2. Formation energy under the Al-rich and N-rich conditions of the VAl and ErAl + VAl systems.
体系 形成能/eV 富Al 富N VAl 9.1935 6.1735 ErAl + VAl 10.35831 4.31831
下载: 导出CSV
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