近红外二区长波发射<inline-formula><tex-math id="Z-20240723110058">\begin{document}${\rm Na_3YSi_3O_9}{:}x {\rm Cr^{3+}}$\end{document}</tex-math><alternatives><graphic specific-use="online" xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="15-20240663_Z-20240723110058.jpg"/><graphic specific-use="print" xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="15-20240663_Z-20240723110058.png"/></alternatives></inline-formula>硅酸盐及多格位占据光谱展宽

龚长帅; 王建通; 王渤文; 薛绪岩; 王雪娇

doi:10.7498/aps.73.20240663

摘要

以Cr³⁺为激活剂的荧光粉被认为是目前最有可能实现商业化的近红外材料. 但目前这类荧光粉的发射波长一般位于小于850 nm的近红外一区, 以Cr³⁺为激活剂实现近红外二区发射仍然具有挑战. 本文采用普适的固相法制备了一系列Na₃Y_1–xSi₃O₉:x Cr³⁺硅酸盐荧光粉, 利用Na₃YSi₃O₉硅酸盐属性及结构中多种适于Cr³⁺占据的八面体位点有效红移并展宽光谱. 对样品的物相、晶体结构、微观形貌、光致发光、主发射峰衰减和热稳定性等进行了系统研究. 结果显示, 所制样品均为纯相, 形貌不均匀略有团聚, 尺寸在微米量级. Cr³⁺在Na₃YSi₃O₉晶格中位于弱晶体场环境, 八面体晶体场参数Dq和Racah参数B的比值Dq/B = 2.29. 在485 nm蓝光激发下Na₃Y_1–xSi₃O₉:x Cr³⁺荧光粉最强发射峰位于984 nm处(NIR II区), 长于大多数Cr³⁺激活的荧光粉. 且得益于Cr³⁺在晶格中的多格位占据, 发射光谱的半峰宽高达183 nm. Na₃Y_1–xSi₃O₉:x Cr³⁺中最佳掺杂浓度为3%, 猝灭机理为Cr³⁺离子间的偶极-偶极作用. Na₃Y_1–xSi₃O₉:x Cr³⁺主发射峰荧光衰减动力学分析表明室温荧光寿命约为37.95 μs, 且随着掺杂浓度增大及温度升高(至423 K)逐渐降低.

关键词:

硅酸盐 /
Cr³⁺ /
宽带近红外 /
多格位

Abstract

Phosphors-converted near-infrared LED (pc-NIR LED) possesses applications in various fields including food quality analysis, night vision, biomedical imaging, and biomedicine. The design and development of broadband near-infrared (NIR) phosphors with the required properties are of decisive significance for pc-NIR LED devices. The Cr³⁺ doped phosphors are considered to be most promising near-infrared materials for commercialization. Broadband NIR luminescent materials doped with Cr³⁺ have attracted more and more attention due to their potential applications in NIR light sources. However, the emission wavelength of Cr³⁺ doped phosphor is generally located in the NIR I region of less than 850 nm, and realizing the NIR II region emission is still a challenge. In this work, a series of Cr³⁺ doped Na₃YSi₃O₉ new silicate phosphors is prepared by solid-state method in N₂ atmosphere at 1150 ℃ for 8 h. We take advantages of the silicate nature and the multi octahedral sites suitable for Cr³⁺ in the studied Na₃YSi₃O₉ materials to redshift and broaden the spectrum. The phase, crystal structure, microstructure, photoluminescence, main emission peak decay and thermal stability of the samples are systematically studied. The results show that the prepared samples are pure phases, with uneven morphology, slight agglomeration, and the sizes in the micrometer range. The Cr³⁺ is located in the weak crystal field environment of Na₃YSi₃O₉ lattice, with a Dq/B value of 2.29. Under the excitation of blue light at a wavelength of 485 nm, the strongest emission peaks of Na₃Y_1–x Si₃O₉:x Cr³⁺ phosphors are located at 984 nm (NIR II region), which is longer than those of most Cr³⁺ activated phosphors. Due to the multi-site occupation of Cr³⁺ in the lattice, the full width at half maximum (FWHM) of the emission spectrum is as high as 183 nm. The optimal doping concentration of Na₃Y_1–x Si₃O₉:x Cr³⁺ is 3%, and the quenching mechanism is the dipole-dipole interaction between Cr³⁺ ions. Fluorescence decay curves show that the luminescence lifetime of Na₃Y_0.97Si₃O₉:0.03Cr³⁺ sample gradually decreases with the increase of doping concentration and temperature. The results of the temperature-dependent spectra show that the emission intensity decreases in a temperature range from 298 K to 423 K, and the activation energy ΔE of Cr³⁺ is 0.157 eV.

Keywords:

作者及机构信息

渤海大学化学与材料工程学院, 锦州　121013

通信作者: 王雪娇, wangxuejiao@bhu.edu.cn

基金项目: 辽宁省教育厅自然科学基金(批准号: JYTMS20231627)和辽宁省科技厅自然科学基金(批准号: 2020-MS-286)资助的课题.

Authors and contacts

School of Chemistry and Materials Engineering, Bohai University, Jinzhou 121013, China

Corresponding author: Wang Xue-Jiao, wangxuejiao@bhu.edu.cn

Funds: Project supported by the Natural Science Foundation of the Educational Department of Liaoning Province, China (Grant No. JYTMS20231627) and the Natural Science Foundation of Liaoning Provincial Department of Science and Technology, China (Grant No. 2020-MS-286).

文章全文 : translate this paragraph

补充材料

157803-20240663补充材料.pdf

参考文献

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施引文献

图 1 (a) Na₃Y_1–x Si₃O₉:x Cr³⁺ (x = 0—0.1)样品的XRD图谱; (b) Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品Rietveld精修结果; (c) Na₃YSi₃O₉的晶体结构; (d) Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品FE-SEM及元素扫描分布图

Fig. 1. (a) The XRD patterns of the Na₃Y_1–x Si₃O₉:x Cr³⁺ (x = 0–0.1) samples; (b) Rietveld refinement results of the Na₃Y_0.97Si₃O₉:0.03Cr³⁺ sample; (c) crystal structure of Na₃YSi₃O₉; (d) the FE-SEM morphology and elemental mapping of the Na₃Y_0.97Si₃O₉:0.03Cr³⁺ sample.

下载: 全尺寸图片幻灯片

图 2 Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品　(a) 漫反射光谱; (b) 带隙能量的测定

Fig. 2. Na₃Y_0.97Si₃O₉:0.03Cr³⁺ samples: (a) Diffuse reflectance spectrum; (b) determination of band gap energy.

下载: 全尺寸图片幻灯片

图 3 (a) Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品的XPS全谱; (b) Cr 2p轨道的精细谱; (c) Cr的 K边X射线吸收近边结构(XANES)光谱

Fig. 3. (a) XPS full spectrum for Na₃Y_0.97Si₃O₉:0.03Cr³⁺ sample; (b) high-resolution XPS spectra of Cr 2p orbital; (c) Cr K-edge X-ray absorption near-edge structure (XANES) spectrum.

下载: 全尺寸图片幻灯片

图 4 (a)—(c) Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品的(a)归一化的激发和发射光谱、(b) 田边-菅野图、(c) 80—300 K 范围内变温发射光谱; (d)—(f) Na₃Y_1–x Si₃O₉:x Cr³⁺ (x = 0—0.1)样品的(d)发射光谱; (e) log(x)-log(I/x)对应关系; (f) 荧光衰减曲线(λ_ex = 485 nm, λ_em = 984 nm)

Fig. 4. (a) Normalized excitation and emission spectra, (b) Tanabe-Sugano energy level diagram, (c) temperature-dependent emission spectra in the range of 80—300 K for the Na₃Y_0.97Si₃O₉:0.03Cr³⁺ samples; (d) emission spectra, (e) the log(x) versus log(I/x) plot, (f) luminescence decay curves (λ_ex = 485 nm, λ_em = 984 nm) for the Na₃Y_1–x Si₃O₉:x Cr³⁺ (x = 0–0.1) samples.

下载: 全尺寸图片幻灯片

图 5 (a) Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品变温发射光谱的等高线图; (b) 1/kT与ln[(I₀/I) －1]的对应关系; (c) Cr³⁺热猝灭过程的位形坐标示意图; (d) 不同温度下的荧光衰减曲线

Fig. 5. (a) Contour plot of the temperature-dependent PL spectra of Na₃Y_0.97Si₃O₉:0.03Cr³⁺; (b) ln[(I₀/I) －1] vs. 1/kT relationship; (c) the thermal quenching process of Cr³⁺ depicted with the configurational coordinate diagram; (d) fluorescence decay curves at different temperatures.

下载: 全尺寸图片幻灯片

表 1 由Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品XRD图谱精修所得的结构参数和可靠因子及纯相Na₃YSi₃O₉晶胞参数信息 (PDF #72-2455)

Table 1. Structure parameters and reliability factors obtained via refinement of the XRD pattern for Na₃Y_0.97Si₃O₉:0.03Cr³⁺ sample and the cell parameters from pure Na₃YSi₃O₉ (PDF #72-2455).

Chemical formula	Na₃YSi₃O₉	Na₃Y_0.97Si₃O₉:0.03Cr³⁺
Space group	P2₁2₁2₁	P2₁2₁2₁
a/Å	15.408(4)	15.0362(4)
b/Å	15.312(5)	15.2116(5)
c/Å	15.222(4)	15.1460(4)
α/(°)	90	90
β/(°)	90	90
γ /(°)	90	90
V/Å³	3591.016(18)	3464.26(18)
R_p/%	—	4.75
R_wp/%	—	7.41
χ²	—	2.140

下载: 导出CSV

表 2 Na₃Y_0.97Si₃O₉:0.03Cr³⁺样品中4种[YO₆]多面体键长及多面体畸变指数汇总

Table 2. Bond length and distortion index of four kinds [YO₆] polyhedrons in Na₃Y_0.97Si₃O₉:0.03Cr³⁺ sample.

Bond	d₁	d₂	d₃	d₄	d₅	d₆	d_av	d_dis
Y1—O	2.4937	2.1867	2.0643	2.2623	3.1427	3.0236	2.2589	0.1461
Y2—O	2.1108	2.2302	2.2744	2.8329	2.1218	2.1108	2.2801	0.0808
Y3—O	2.2707	1.9528	2.7648	1.8012	3.8077	2.8960	2.5822	0.2223
Y4—O	2.2642	2.052	1.6169	1.8874	3.1401	3.2249	2.3643	0.2307

下载: 导出CSV

表 3 Na₃Y_1–xSi₃O₉:x Cr³⁺ (x = 0—0.1)样品荧光衰减曲线拟合结果 (λ_ex = 485 nm, λ_em = 984 nm)

Table 3. Fluorescence decay curve fitting results of Na₃Y_1–xSi₃O₉:x Cr³⁺ (x = 0–0.1) samples (λ_ex = 485 nm, λ_em = 984 nm)

浓度	λ_em/nm	A₁	A₂	τ₁	τ₂	χ²	τ/μs
0.005	984	2020.38	802.09	16.50	54.35	0.987	37.95
0.01	984	1993.95	836.83	15.08	50.03	1.054	35.42
0.02	984	1808.84	729.58	12.14	44.47	1.059	31.42
0.03	984	1963.30	726.19	12.61	45.56	0.961	31.45
0.05	984	1837.09	818.42	13.02	43.06	0.986	30.91
0.10	984	1985.01	692.64	13.29	45.20	0.984	30.61

下载: 导出CSV

[1]	Chen Y, Wang S F, Zhang F 2023 Nat. Rev. Bioeng. 1 60 Google Scholar
[2]	Wu H Y, Jiang L H, Li K, Li C Y, Zhang H J 2021 J. Mater. Chem. C 9 11761 Google Scholar
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[13]	Rajendran V, Huang W T, Chen K C, Chang H, Liu R S 2022 J. Mater. Chem. C 10 14367 Google Scholar
[14]	Huang W T, Chen K C, Huang M H, Liu R S 2023 Adv. Opt. Mater. 11 2301166 Google Scholar
[15]	Liu Y, Stasio F D, Bi C H, Zhang J B, Xia Z G, Shi Z F, Manna L 2024 Adv. Mater. 36 2312482 Google Scholar
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[22]	Li C J, Zhong J Y 2023 Adv. Opt. Mater. 11 2202323 Google Scholar
[23]	Dumesso M U, Xiao W, Zheng G, Basore E T, Tang M, Liu X, Qiu J 2022 Adv. Opt. Mater. 10 2200676 Google Scholar
[24]	Huang D, Liang S, Chen D, Hu J, Xu K, Zhu H 2021 Chem. Eng. J. 426 131332 Google Scholar
[25]	Pan L, Lu R, Zhu Q, McGrath J M, Tu K 2015 Postharvest Biol. Tec. 102 42 Google Scholar
[26]	Cai H, Liu S Q, Song Z, Liu Q L 2021 J. Mater. Chem. C 9 5469 Google Scholar
[27]	Kenry, Duan Y, Liu B 2018 Adv. Mater. 30 1802394 Google Scholar
[28]	Xia Z G, Zhou J, Mao Z Y 2013 J. Mater. Chem. C 1 5917 Google Scholar
[29]	Wang F, Jin Y, Liu Y F, Zhang L L, Dong R, Zhang J H 2019 J. Lumin 206 227 Google Scholar
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[34]	刘云鹏, 盛伟繁, 吴忠华 2021 无机材料学报 36 901 Google Scholar Liu Y P, Sheng W F, Wu Z H 2021 J. Inorg. Mater. 36 901 Google Scholar
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近红外二区长波发射${\rm Na_3YSi_3O_9}{:}x {\rm Cr^{3+}}$硅酸盐及多格位占据光谱展宽

Long wavelength near-infrared II emitting Na₃YSi₃O₉:x Cr³⁺silicate and spectral broadening by multi-site occupancy

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渤海大学化学与材料工程学院, 锦州　121013

通信作者: 王雪娇, wangxuejiao@bhu.edu.cn

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School of Chemistry and Materials Engineering, Bohai University, Jinzhou 121013, China

Corresponding author: Wang Xue-Jiao, wangxuejiao@bhu.edu.cn

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近红外二区长波发射${\rm Na_3YSi_3O_9}{:}x {\rm Cr^{3+}}$硅酸盐及多格位占据光谱展宽

Long wavelength near-infrared II emitting Na3YSi3O9:x Cr3+ silicate and spectral broadening by multi-site occupancy

渤海大学化学与材料工程学院, 锦州 121013

通信作者: 王雪娇, wangxuejiao@bhu.edu.cn

School of Chemistry and Materials Engineering, Bohai University, Jinzhou 121013, China

Corresponding author: Wang Xue-Jiao, wangxuejiao@bhu.edu.cn

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Long wavelength near-infrared II emitting Na₃YSi₃O₉:x Cr³⁺silicate and spectral broadening by multi-site occupancy

渤海大学化学与材料工程学院, 锦州　121013