Al纳米颗粒表面等离激元对ZnO光致发光增强的研究

刘姿; 张恒; 吴昊; 刘昌

doi:10.7498/aps.68.20190062

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摘要

基于聚苯乙烯球自组装法, 在P型氮化镓(P-GaN)衬底上制备了有序致密的掩模板; 采用热蒸发法在该模板上沉积金属Al薄膜, 通过甲苯溶液去除聚苯乙烯球, 得到了金属Al纳米颗粒阵列; 采用原子层沉积法, 在Al纳米颗粒阵列表面依次沉积氧化铝(Al₂O₃)和氧化锌(ZnO). 通过测试Al纳米颗粒阵列的消光谱以及ZnO薄膜的光致发光谱, 研究了Al纳米颗粒表面等离激元与ZnO薄膜激子之间的耦合效应. 实验结果表明: 引入Al纳米颗粒后, 在约380 nm位置附近的ZnO近带边发光峰积分强度增强了1.91倍. 对Al纳米颗粒表面等离激元增强ZnO光致发光的机理进行探讨.

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Abstract

During the past few decades, surface plasmons (SPs) have become a research hotspot. The SPs are the collective oscillations of free electrons at the interface between metal and dielectric surrounding. Localized surface plasmon resonance (LSPR) for metal nanoparticles (NPs) has a wide application in the light emission enhancement by the selective photon absorption and by increasing local electromagnetic field. Nowadays, many achievements of SP-enhanced-emissions are applied to light emitting diodes. With the advantages of the direct wide band gap (3.37 eV) and large exciton binding energy (60 meV), zinc oxide (ZnO), which is considered as a potential material, has a wide range of applications, especially in ultraviolet (UV) optoelectronic devices. However, the low photoluminescence efficiency of ZnO limits the commercial applications of ZnO-devices. The relevant research shows that the selection of different metal NPs, such as platinum (Pt), aluminum (Al), argentum (Ag), aurum (Au), is one of the approaches to improving the UV emission from ZnO. In this study, two-dimensional arrays of Al NPs are used to improve the LSPR photoluminescence efficiency from ZnO grown by the atomic layer deposition (ALD). The two-dimensional arrays of Al NPs are fabricated on the surfaces of p-type Gallium nitride (GaN) substrates by colloid lithography. With the air-liquid interface self-assembly, the monolayer masks for colloid lithography are obtained on the substrates of p-type GaN. Then, after a 50-nm Al layer is deposited by thermal evaporation, the Al NPs’ arrays are gained by being dipped into toluene and extra sonication to remove the masks. Finally, 15 nm Al₂O₃ and 200 nm ZnO films are deposited in sequence by ALD at a temperature of 125 ℃. The extinction spectra of Al NPs’ arrays are acquired by an ultraviolet-visible spectrophotometer. The results of the extinction spectra suggest that the radiative recombination rate is increased by the resonance coupling between the localized surface plasmons (LSP) of the Al NPs arrays and the excitons of the ZnO. A 1.91-fold enhancement of photoluminescence integral intensity in band-edge emission is measured because of the Al NP arrays coupled with ZnO. The result means that the LSP of the Al NPs’ arrays can increase the UV-emission of the ZnO. Therefore, this cost-effective and facile approach can be used in high-performance optoelectronic devices.

Keywords:

作者及机构信息

武汉大学物理科学与技术学院, 人工微结构教育部重点实验室, 核固体物理湖北省重点实验室, 武汉　430072

通信作者: 吴昊, h.wu@whu.edu.cn ; 刘昌, chang.liu@whu.edu.cn

基金项目: 国家重点研究与发展计划(批准号: 2017YFA0205802)、国家自然科学基金(批准号: 11574235, 11875212)和江苏省自然科学研究基金(批准号: BK20151250)资助的课题.

Authors and contacts

Key Laboratory of Artificial Micro- and Nano-structures of Ministry of Education, Hubei Nuclear Solid Physics Key Laboratory, School of Physics and Technology, Wuhan University, Wuhan 430072, China

Corresponding author: Wu Hao, h.wu@whu.edu.cn ; Liu Chang, chang.liu@whu.edu.cn

Funds: Project supported by the National Key Research and Development Plan (MOST), China (Grant No. 2017YFA0205802), the National Natural Science Foundation of China (Grant Nos. 11574235, 11875212), and the Funding of Jiangsu Province, China (Grant No. BK20151250).

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参考文献

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[17]	Zheng C 2012 Ph. D. Dissertation (Nanjing: Nanjing University) (in Chinese)
[18]	陈超 2015 Ph. D. Dissertation (Wuhan: Wuhan University) (in Chinese)
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[25]	Gontijo I, Boroditsky M, Yablonovitch E, Keller S, Mishra U, DenBaars S 1999 Phys. Rev. B 60 11564 Google Scholar
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施引文献

图 1 (a) PS球阵列SEM图; (b) Al纳米颗粒阵列SEM图

Fig. 1. (a) The SEM image of PS arrays; (b) the SEM image of Al nanoparticle arrays.

下载: 全尺寸图片幻灯片

图 2 引入Al纳米颗粒前后ZnO的PL光谱

Fig. 2. Comparison of ZnO photoluminescence spectra with and without Al nanoparticles

下载: 全尺寸图片幻灯片

图 3 Al纳米颗粒的吸收谱

Fig. 3. The absorption spectrum of Al nanoparticles.

下载: 全尺寸图片幻灯片

图 4 (a)无Al纳米颗粒ZnO薄膜的AFM图; (b)有Al纳米颗粒ZnO薄膜的AFM图

Fig. 4. The AFM image of ZnO without Al nanoparticls; (b) the AFM image of ZnO with Al nanoparticls.

下载: 全尺寸图片幻灯片

[1]	You D T, Xu C X, Qin F F, Zhu Z, Manohari A G, Xu W, Zhao J, Liu W 2018 Sci. Bull. 63 38 Google Scholar
[2]	Lu Y J, Shi Z F, Shan C X, Shen D Z 2017 Chin. Phys. 26 047703 Google Scholar
[3]	李江江, 高志远, 薛晓玮, 李慧敏, 邓军, 崔碧峰, 邹德恕, 2016 物理学报 65 118104 Google Scholar Li J J, Gao Z Y, Xue X W, Li H M, Deng J, Cui B F, Zou D S 2016 cta Phys. Sin. 65 118104 Google Scholar
[4]	任艳东, 郝淑娟, 邱忠阳 2013 物理学报 62 147302 Google Scholar Ren Y D, Hao S J, Qiu Z Y 2013 Acta Phys. Sin. 62 147302 Google Scholar
[5]	邱东江, 范文志, 翁圣, 吴惠桢, 王俊 2011 物理学报 60 087301 Google Scholar Qiu D J, Fan W Z, Weng S, Wu H Z, Wang J 2011 Acta Phys. Sin. 60 087301 Google Scholar
[6]	Yang L, Liu W, Xu H, Ma J, Zhang C, Liu C, Wang Z, Liu Y 2017 J. Mater. Chem. C 5 3288 Google Scholar
[7]	Feng W, Jing A, Li J, Liang G 2016 Optoe. Lett. 12 195 Google Scholar
[8]	Zhang S G, Zhang X W, Yin Z G, Wang J X, Si F T, Gao H L, Dong J J, Liu X 2012 J. Appl. Phys. 112 013112 Google Scholar
[9]	Liu W Z, Xu H Y, Zhang L X, Zhang C, Ma J G, Wang J N, Liu Y C 2012 Appl. Phys. Lett. 101 142101 Google Scholar
[10]	Zhang S G, Zhang X W, Yin Z G, Wang J X, Dong J J, Gao H L, Si F T, Sun S S, Tao Y 2011 Appl. Phys. Lett. 99 181116 Google Scholar
[11]	Chan G H, Zhao J, Schatz G C, van Duyne R P 2008 J. Phys. Chem. C 112 13958 Google Scholar
[12]	Wu K W, Lu Y F, He H P, Huang J Y, Zhao B H, Ye Z Z 2011 J. Appl. Phys. 110 601
[13]	Lin Y 2013 Ph. D. Dissertation (Wuhan: Wuhan University) (in Chinese)
[14]	Kao C C, Su Y K, Lin C L, Chen J J 2010 IEEE Photonic. Tech. L. 22 984 Google Scholar
[15]	Liu K W, Tang Y D, Cong C X, Sum T C, Huan A C H, Shen Z X, Wang L, Jiang F Y, Sun X W, Sun H D 2009 Appl. Phys. Lett. 94 151102 Google Scholar
[16]	刘斌斌, 肖湘衡, 吴伟, 任峰, 蒋昌忠 2011 武汉大学学报: 理学版 57 205 Liu B B, Xiao X H, Wu W, Ren F, Jiang C Z 2011 J. Wuhan Univ.: Science Edition 57 205
[17]	Zheng C 2012 Ph. D. Dissertation (Nanjing: Nanjing University) (in Chinese)
[18]	陈超 2015 Ph. D. Dissertation (Wuhan: Wuhan University) (in Chinese)
[19]	Zhang H, Su X, Wu H, Liu C 2019 J. Alloy. Compd. 772 460 Google Scholar
[20]	马勇, 王万录, 廖克俊, 吕建伟, 孙晓楠 2004 功能材料 35 139 Google Scholar Ma Y, Wang W L, Liao K J, Lü J W, Sun X L 2004 J. Funct. Mater. 35 139 Google Scholar
[21]	Zou S L, Janel N, Schatz G C 2004 J. Chem. Phys. 120 10871 Google Scholar
[22]	Shen Y Z, Swiatkiewicz J, Lin T C, Markowicz P, Prasad P N 2002 J. Phys. Chem. B 106 4040 Google Scholar
[23]	Zhang J Y, Ye Y H, Wang X Y, Rochon P, Xiao M 2005 Phys. Rev. B 72 201306 Google Scholar
[24]	Komarala V K, Rakovich Y P, Bradley A L, Byrne S J, Gun’ko Y K, Gaponik N, Eychmüller A 2006 Appl. Phys. Lett. 89 253118 Google Scholar
[25]	Gontijo I, Boroditsky M, Yablonovitch E, Keller S, Mishra U, DenBaars S 1999 Phys. Rev. B 60 11564 Google Scholar
[26]	Bagnall D M, Chen Y F, Zhu Z, Yao T, Shen M Y, Goto T 1998 Appl. Phys. Lett. 73 1038 Google Scholar
[27]	张丽, 蒋昌忠, 任峰, 石瑛, 付强 2004 功能材料 35 160 Google Scholar Zhang L, Jiang C Z, Ren F, Shi Y, Fu Q 2004 J. Funct. Mater. 35 160 Google Scholar

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Al纳米颗粒表面等离激元对ZnO光致发光增强的研究

武汉大学物理科学与技术学院, 人工微结构教育部重点实验室, 核固体物理湖北省重点实验室, 武汉　430072

通信作者: 吴昊, h.wu@whu.edu.cn ; 刘昌, chang.liu@whu.edu.cn

基金项目: 国家重点研究与发展计划(批准号: 2017YFA0205802)、国家自然科学基金(批准号: 11574235, 11875212)和江苏省自然科学研究基金(批准号: BK20151250)资助的课题.

收稿日期: 2019-01-13

修回日期: 2019-03-13

上网日期: 2019-05-01

刊出日期: 2019-05-20

摘要: 基于聚苯乙烯球自组装法, 在P型氮化镓(P-GaN)衬底上制备了有序致密的掩模板; 采用热蒸发法在该模板上沉积金属Al薄膜, 通过甲苯溶液去除聚苯乙烯球, 得到了金属Al纳米颗粒阵列; 采用原子层沉积法, 在Al纳米颗粒阵列表面依次沉积氧化铝(Al₂O₃)和氧化锌(ZnO). 通过测试Al纳米颗粒阵列的消光谱以及ZnO薄膜的光致发光谱, 研究了Al纳米颗粒表面等离激元与ZnO薄膜激子之间的耦合效应. 实验结果表明: 引入Al纳米颗粒后, 在约380 nm位置附近的ZnO近带边发光峰积分强度增强了1.91倍. 对Al纳米颗粒表面等离激元增强ZnO光致发光的机理进行探讨.

关键词:

Enhancement of photoluminescence from zinc oxide by aluminum nanoparticle surface plasmon

Key Laboratory of Artificial Micro- and Nano-structures of Ministry of Education, Hubei Nuclear Solid Physics Key Laboratory, School of Physics and Technology, Wuhan University, Wuhan 430072, China

Corresponding author: Wu Hao, h.wu@whu.edu.cn ; Liu Chang, chang.liu@whu.edu.cn

Fund Project: Project supported by the National Key Research and Development Plan (MOST), China (Grant No. 2017YFA0205802), the National Natural Science Foundation of China (Grant Nos. 11574235, 11875212), and the Funding of Jiangsu Province, China (Grant No. BK20151250).

Received Date: 13 January 2019

Accepted Date: 13 March 2019

Available Online: 01 May 2019

Published Online: 20 May 2019

Abstract: During the past few decades, surface plasmons (SPs) have become a research hotspot. The SPs are the collective oscillations of free electrons at the interface between metal and dielectric surrounding. Localized surface plasmon resonance (LSPR) for metal nanoparticles (NPs) has a wide application in the light emission enhancement by the selective photon absorption and by increasing local electromagnetic field. Nowadays, many achievements of SP-enhanced-emissions are applied to light emitting diodes. With the advantages of the direct wide band gap (3.37 eV) and large exciton binding energy (60 meV), zinc oxide (ZnO), which is considered as a potential material, has a wide range of applications, especially in ultraviolet (UV) optoelectronic devices. However, the low photoluminescence efficiency of ZnO limits the commercial applications of ZnO-devices. The relevant research shows that the selection of different metal NPs, such as platinum (Pt), aluminum (Al), argentum (Ag), aurum (Au), is one of the approaches to improving the UV emission from ZnO. In this study, two-dimensional arrays of Al NPs are used to improve the LSPR photoluminescence efficiency from ZnO grown by the atomic layer deposition (ALD). The two-dimensional arrays of Al NPs are fabricated on the surfaces of p-type Gallium nitride (GaN) substrates by colloid lithography. With the air-liquid interface self-assembly, the monolayer masks for colloid lithography are obtained on the substrates of p-type GaN. Then, after a 50-nm Al layer is deposited by thermal evaporation, the Al NPs’ arrays are gained by being dipped into toluene and extra sonication to remove the masks. Finally, 15 nm Al₂O₃ and 200 nm ZnO films are deposited in sequence by ALD at a temperature of 125 ℃. The extinction spectra of Al NPs’ arrays are acquired by an ultraviolet-visible spectrophotometer. The results of the extinction spectra suggest that the radiative recombination rate is increased by the resonance coupling between the localized surface plasmons (LSP) of the Al NPs arrays and the excitons of the ZnO. A 1.91-fold enhancement of photoluminescence integral intensity in band-edge emission is measured because of the Al NP arrays coupled with ZnO. The result means that the LSP of the Al NPs’ arrays can increase the UV-emission of the ZnO. Therefore, this cost-effective and facile approach can be used in high-performance optoelectronic devices.

Keywords:

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1. 引　言

ZnO是宽带隙化合物半导体, 其禁带宽度为3.37 eV, 室温下激子结合能高达60 meV, 远高于室温热离化能26 meV, 其近带边发射峰在380 nm附近, 因此成为紫外发光二极管（LED）、紫外激光器、紫外探测器的理想候选材料^[1-3]. 在制备ZnO过程中, 由于引入了晶格缺陷和杂质, ZnO的光致发光（photoluminescence, PL）除了紫外波段的近带边发光外, 还有位于可见光波段的缺陷发光. 如何提高紫外发光效率, 减小缺陷杂质发光的干扰, 成为ZnO材料用于制造紫外激光器、LED等器件迫切需要解决的问题.

随着微纳加工技术的进步, 利用金属表面等离激元提高LED发光效率的研究得到快速发展. 目前已有工作表明, 通过采用不同的贵金属Ag, Au^[4,5]等, 利用金属局域表面等离子体, 即金属表面自由电子在金属纳米颗粒与电介质之间界面处产生集体振荡, 能够增强ZnO近带边发射峰^[6-10]. 由于贵金属成本较高, 限制了其商业化应用, 同时对金属Al表面等离激元与ZnO激子之间的相互作用的研究较少^[11,12], 故本文采用成本较低且含量丰富的金属Al代替贵金属Ag, Au, 研究Al表面等离激元对ZnO薄膜PL特性的影响.

利用金属表面等离激元增强ZnO近带边发射峰, 最关键的是调控金属表面等离激元共振频率与ZnO近带边发光峰相吻合. 金属表面等离激元的共振频率与很多因素有关, 比如纳米颗粒的形状、大小以及周围电介质等, 大多数利用金属表面等离激元提高ZnO发光效率的研究中, 制备金属纳米颗粒都是先蒸镀一层金属薄膜, 再通过热退火方法自组装形成金属纳米颗粒, 该方法不能精确控制金属纳米颗粒的形状和大小, 进而不能精确调控金属表面等离激元的共振频率^[8-10]. 其他制备金属纳米颗粒的方法是采用微加工, 该方法加工复杂、成本高昂, 难以制备大面积结构^[13]. 因此, 本文基于聚苯乙烯(Polystyrene, PS)球自组装法^[14-16], 在P-GaN衬底上制备Al纳米颗粒, 再采用原子层沉积(atomic layer deposition, ALD)技术在Al纳米颗粒表面依次沉积Al₂O₃和ZnO薄膜. PL谱实验结果表明, 引入Al纳米颗粒后, ZnO近带边发射峰得到增强.

2. 实验设计

基于PS球自组装法, 在P-GaN衬底上制备有序致密的PS球掩模板, 具体方法如下^[16]: 通过载玻片, 将所配制的PS球溶液引流到去离子水表面并铺展开; 利用水表面张力分散PS球, 自组装形成大面积无序的单层膜; 再滴加浓度2%的十二烷基硫酸钠(sodium dodecyl sulfate, SDS)溶液, 形成高密度、大面积、有序排列的PS球单层膜; 待液面稳定后, 用镊子夹住P-GaN衬底, 从PS球单层膜区域将其缓慢提拉出水面, 静置晾干即可得到有序的PS球掩模板. PS球的大小不同, 得到的金属颗粒大小也不同.

室温下采用热蒸发法在该模板上沉积50 nm金属Al薄膜, 沉积腔体背景压强为4 × 10^–4 Pa, 沉积速率为0.02 Å/s. 通过甲苯溶液去除PS球, 形成有序的Al纳米颗粒阵列. 采用ALD技术在Al纳米颗粒表面依次沉积15 nm Al₂O₃和200 nm ZnO, 沉积温度为125 ℃. 由于金属的电子费米面能级比半导体的导带能级低, 同时比价带能级高, 电子将会从导带直接转移到金属费米能级, 并不能发生有效的辐射跃迁, 最后以热振动的形式被耗尽能量, 这是SPs淬灭半导体发光的作用机制. 淬灭发光不能增强其光致发光, 插入Al₂O₃缓冲层能避免发生淬灭^[17].

本实验室ALD机器型号为Beneq公司的TSF 200. Al₂O₃所用的前驱体源是三甲基铝（Trimethylaluminium, TMA）和水（H₂O）, 生长速率为0.1 nm/cycle. ZnO所用的前驱体源是二乙基锌（Diethylzinc, DEZn）和H₂O, 生长速率为0.2 nm/cycle, 具体生长工艺参见本课题组之前工作^[18].

使用原子力显微镜(atomic force microscope, AFM, Shimadzu, SPM-9500J3)来表征分析ZnO薄膜表面粗糙度, 使用扫描电子显微镜(scanning electron microscope, SEM)观察自组装形成的PS球掩模板, 使用仪器Varian Cary5000型紫外-可见-红外双光束分光光度计测量样品的吸收谱, 以325 nm He-Cd激光器作激发源测量样品的PL谱.

4. 结　论

本文提供了一种采用金属纳米颗粒表面等离激元耦合增强ZnO薄膜PL发光强度的方法. 基于PS球自组装法制备了特征尺寸的Al纳米颗粒阵列, 使用ALD技术沉积ZnO薄膜. 实验中可以明显观察到ZnO薄膜与Al纳米颗粒表面等离子体耦合效应, 在ZnO近带边发光峰380 nm附近处, 其PL谱积分强度增强了1.91倍, 并产生了轻微的峰位红移. ZnO的PL增强机理是由于Al纳米颗粒表面等离子体和ZnO自身激子之间的电磁相互作用引起的.

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Al纳米颗粒表面等离激元对ZnO光致发光增强的研究