钙钛矿微纳激光器研究进展 
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1 引言
自1960年梅曼研制的第一台红宝石激光器问世以来[1],激光技术在近60年间迅猛发展,凭借其高强度和强相干性等特性,已广泛应用于光通信、光谱学和成像等领域[2-5]。近年来,随着纳米科技的飞速发展,光电子元器件的发展越来越趋向于小型化和集成化[6]。新型的微纳激光器由于其物理尺寸有望突破传统的衍射极限,并且具有小尺寸(微米或亚微米量级)、低损耗等优点,在高密度信息存储、生物成像、超灵敏传感器、光学集成应用和全息等领域有着潜在的应用前景,引起人们的广泛关注和研究[7-10]。
在过去的三十年里,大量的无机和有机半导体纳米材料作为优良的增益介质,可以引发受激辐射现象;本身还可以作为光学谐振腔,提供光反馈,被广泛应用于微纳激光器的研究[11-12]。从2001年Huang等[9]在光泵浦的单晶氧化锌纳米线中观察到激光发射以来,激光的发射先后在各种半导体纳米结构中实现,例如纳米线、纳米片、量子点和光子晶体等[13-18]。尽管半导体微纳激光已经取得了很多的研究成果,但是仍然有很多技术上难题,阻碍半导体微纳激光器的进一步应用。例如,部分无机半导体材料依赖于昂贵的高温真空处理条件[19],可以替代的有机半导体材料和胶体量子点却分别被低损伤阈值和高的表面缺陷浓度限制;其次,微型化的固态激光器增益介质光学损失大,比如俄歇复合损失和固有的热损伤,使得激光阈值高[20];最后,优良的载流子输运的特性是实现电注入的半导体微纳激光器急需解决的问题[21-22]。所以,发展高增益、低阈值、稳定性好的半导体微纳激光器具有重大意义。
在过去的十年,钙钛矿作为人们关注的焦点,取得了巨大的科学进展。从2009年Kojima等[23]第一次利用有机无机杂化钙钛矿MAPbI3实现染料敏化太阳能电池到2019年,太阳能电池的光电转换效率已经从3.8%提升到24.2%,可以与商业的硅和碲化镉太阳能电池相媲美[24]。这些都得益于钙钛矿材料的优异的光电性能,如较大的吸收系数、较低的缺陷态密度、较长的载流子扩散长度等[22]。除了在光伏领域的应用,钙钛矿作为新兴的有潜力的半导体材料,在光电探测器、LED、激光等领域也发展迅速[25]。其次,作为激光增益介质,钙钛矿具有的大吸收系数、低缺陷态密度、高荧光量子产率等优点得天独厚,同时折射率比传统的半导体材料相对较高,与环境形成较大的反射对比,是无外腔纳米激光器非常好的选择,同时也为激光器尺寸突破传统的衍射极限提供可能。
自2014年Xing等[26]首次在低温溶液法合成的有机无机杂化MAPbI3钙钛矿薄膜中实现放大的自发辐射(ASE)以来,基于不同的形貌调控,如纳米线、纳米片、单晶、量子点、亚微米球等微纳激光器相继出现,同时伴随着回音壁模式 (WGM)、法布里-珀罗(F-P)模式及随机模式激光在不同种类的钙钛矿中实现[27]。本文首先介绍钙钛矿材料的结构及其特性,然后根据不同的发射模式介绍钙钛矿微纳激光的发展状况,最后对钙钛矿激光器的发展做出总结,对其现存的问题进行阐述,并对未来钙钛矿激光的发展趋势给出自己的看法。
2 钙钛矿结构及其特性
2.1 钙钛矿晶体结构
钙钛矿是具有通式ABX3结构的一类化合物,化学结构如
图 1. 钙钛矿晶体结构[22]。(a)钙钛矿晶胞单元结构图;(b)通式ABX3钙钛矿三维晶体结构图
Fig. 1. Perovskite crystal structure[22]. (a) Perovskite cell structure; (b) general ABX3 perovskite 3D crystal structure
A、B和X的半径和能否形成稳定的钙钛矿结构有很大的关系,决定着钙钛矿晶体结构的容忍因子t=
2.2 钙钛矿的增益特性
激光是腔内能提供反馈的增益物质受到激发后形成粒子数反转产生光辐射的过程。半导体受激辐射实现光学增益的过程是:一个光子入射到半导体材料发生电子跃迁,同时产生一个和自身相同的受激辐射光子。钙钛矿作为半导体材料,能带附近的光激发态影响着电荷输运和光发射,带边缘存在着自由载流子和激子两种光激励,激子结合能反映光激发的电子空穴对的库仑相互作用的强度,决定着两种激励粒子的平衡。与传统的有机半导体(数百毫电子伏特)和无机半导体(几个毫电子伏特)的激子结合能不同,钙钛矿材料的激子结合能介于两者之间,从不同的实验方法和结果来看,通过改变钙钛矿材料的堆叠、结构和阳离子等[27],其激子结合能存在一个较宽的分布范围(几毫电子伏特到几百毫电子伏特)[30],这使得钙钛矿材料的受激辐射的机制仍然是一个争议。
当半导体的激子结合能小于热涨落能量时,会很容易离解成自由载流子;反之,自由载流子会形成激子。对于光发射的模型,钙钛矿的激子结合能一般都较大,主要是通过激子发生的辐射复合可以在相对较低的载流子密度下来获得较高的量子产率[30]。在对MAPbX3研究的实验中,发现受激辐射主要是自由载流子在带边缘的积累为电子空穴等离子体实现光辐射放大提供粒子数反转[31]。而在CsPbX3纳米粒子的受激辐射中,主要是双激子的复合机制[32]。在钙钛矿增益材料中,相对较大的激子结合能对于室温下稳定的激光发射具有重要的意义。
光学增益用来描述光入射到增益介质上,其发射光强随着距离增大而发生的指数增长的过程;光学损耗则表示光在半导体介质中传输时,发生的光子散射、非辐射复合和边缘散射等的情况。要实现激光的输出,必须满足增益大于损耗,即有正的净增益。为了进一步描述钙钛矿的激光增益特性,引入光学净增益的模型。2005年,Chan等[33]使用可变条纹长度的方法,对壳核结构的CdS / ZnS纳米晶的增益系数进行测量,随后被广泛应用到半导体增益材料中。由于泵浦光斑长度的变化,使得样品的发射强度也发生改变,则根据增益损耗的情况建立净增益模型公式
2.3 发射波长可调谐
发射波长可调谐是钙钛矿材料的一个非常有意思的特性。钙钛矿阳离子或者卤素离子的替换可以改变钙钛矿材料的带宽,进而实现发射波长从可见到红外的调谐。
由于钙钛矿晶体的Pb-X键和能带结构相关,从氯到溴到碘的替换,带隙依次减小[39],因此可以通过卤素离子的替换实现钙钛矿材料发射波长的可调谐。此外,通过混合卤素元素对钙钛矿材料进行调控,实现了发射波长的连续调谐。2013年,Noh等[40]通过改变MAPb(I1-xBrx)3纳米复合物中的溴使得吸收带从786 nm蓝移到544 nm,带隙增大[
图 2. 钙钛矿纳米材料的波长可调谐。(a)改变MAPb(I1-xBrx)3中碘和溴的比例,可以实现786 nm到544 nm的调谐。上图是吸收光谱,下图是纳米复合物的图像[40];(b) MAPbX3(X=Cl、Br、I)改变卤化物的比例,可以实现390到790 nm可见红外的发射波长调谐[26];(c)(d)改变卤素原子,对无机钙钛矿CsPbX3的波长调谐[41-42];(e)对A位原子的调谐。改变FA和MA
Fig. 2. Wavelength tunability of perovskite nanomaterials. (a) By changing the ratio of iodine to bromine in MAPb(I1-xBrx)3, tuning of 786 to 544 nm can be achieved. Above is the absorption spectrum, below is an image of the nanocomposite[40]; (b) MAPbX3(X=Cl, Br, I) can be tuned to the emission wavelength from 390 to 790 nm in visible infrared by changing the ratio of hal
2.4 非线性光学特性
随着研究的不断深入,钙钛矿材料的非线性光学特性同样引人关注。与线性吸收和发射相比,半导体材料的非线性具有穿透深度深、空间分辨率高、对目标样品损伤小等特性。由于作用在材料上光强的不同,所以产生的非线性效应不一样。非线性吸收可以分为饱和吸收和反饱和吸收,反饱和吸收进一步可以分为双光子吸收(TPA)、三光子吸收等。双光子吸收是一个三阶非线性过程,电子在从基态跃迁到激发态的过程中伴随着两个光子的吸收,在高光子通量时变得很重要。
2015年,Walters等[47]使用800 nm飞秒激光激发MAPbBr3单晶,发现了双光子吸收特性。实验测得发光中心波长为572 nm,实验中使用z扫描技术测得非线性吸收系数为8.6 cm/GW。2016年,Gu等[48]在MAPbBr3 纳米线中也观测到双光子吸收现象,当激发波长为400 nm时,激光阈值为3.14 μJ/cm2,发射峰的半峰全宽为0.8 nm;当激发波长为800 nm时,出现双光子吸收现象,激光阈值增大为674 μJ/cm2,其值约为单光子激发阈值的 200 倍,且无需传统固态激光实现频率上转换对相位匹配的要求。随后,Kalanoor等[49]在MAPbI3薄膜中发现非线性光学特性,同年,Zhang等[50]在MAPbBr3纳米片和纳米线中观察到双光子吸收效应。2017年Gao等[51]使用1240 nm、100 fs、1 kHz 强激光泵浦,在MAPbBr3微观结构中观察到明显的光学极限现象,发射波长为540 nm。随着泵浦功率密度的增加,实现了三光子吸收,并测得三光子吸收系数为2.26×10-5 cm3/GW2。2019年,Liu等[52]在FAPbBr3纳米晶中实现双光子泵浦的自发辐射放大,并且测得非线性吸收系数为0.76 cm/GW。2016年,Wang等[53]首次报道全无机钙钛矿CsPbBr3纳米晶中的双光子吸收特性,测得的双光子吸收截面高达1.2×105 GM,在CsPbBr3纳米晶体薄膜上观察到双光子泵浦的低阈值频率上转换的受激发射,并通过三光子泵浦(激发波长为1250 nm),实现绿光ASE激射。同年,Xu等[54]测得 甲苯溶液中的钙钛矿CsPbBr3纳米晶双光子吸收截面为2.7×106 GM,并将钙钛矿CsPbBr3纳米晶嵌入微管中,实现双光子泵浦的低阈值WGM激光。2017年,Wang等[55]合成截面为三角形的全无机CsPbBr3纳米棒,通过多光子泵浦实现激光发射,并进一步证明电子空穴等离子体是产生多光子抽运激光的主要原因。
在过去的几年里,随着钙钛矿材料的非线性光学特性研究不断深入,研究人员发现钙钛矿材料不仅具有双光子吸收、双光子泵浦光致发光、双光子泵浦放大自发辐射,还具有三光子吸收和光致发光作用;优良的非线性光学特性使得钙钛矿材料在双光子上转换激光、三维光信息存储、高分辨成像、光开关等领域有着广泛的应用前景。
3 钙钛矿微纳激光
3.1 WGM钙钛矿微纳激光器
回音壁模式的激光即WGM激光,是纳米介质的内壁和外环境中的折射率差引起的全反射造成的,并且光在传输过程中在介质内部形成光路闭环,光束被很好地限制在介质内部。钙钛矿自被应用到激光领域以来,其不同形貌的纳米结构WGM激光性能已被广泛报道[56-58]。
2014年,Zhang等[59]首次实现室温下的近红外高性能的WGM钙钛矿纳米片激光器。通过两步化学气相沉积的方法在云母基底上获得了六边形和三角形的MAPbI3-aXa钙钛矿纳米片,如
除了有机-无机杂化钙钛矿纳米片外,全无机钙钛矿纳米片的WGM激光也得到广泛的研究,在具备同样甚至更高的激光性能的同时,在稳定性方面有更大的优势。2016年,Zhang等[43]在使用气相沉积范德瓦尔斯外延的方法合成的单晶CsPbBr3上实现WGM激光,如
随着微纳激光器的发展,为了实现更高品质的激光输出,出现了各种方案各种样式的WGM激光器。2017年,Wang等[64]利用交叉的单晶MAPbBr3微米棒的横切面形成WGM腔,实现低阈值(2.37 μJ/cm2)、窄线宽(~0.1 nm)、高品质(Q>5500)的激光发射,如
图 3. 有机无机杂化钙钛矿WGM 激光。(a)六边形和三角形钙钛矿MAPbI3-aXa纳米片的近红外WGM模式激光[59];(b)四边形钙钛矿MAPbBr3纳米片随着泵浦强度的增大,WGM激光模式的出现以及在阈值上下的纳米片光学激发图像[60];(c)三角形钙钛矿纳米片MAPbI3形成的WGM腔[61];(d)随着泵浦能量增加,三角形钙钛矿纳米片MAPbI3中出现WGM激光[61];(e)近似环形腔的WGM激光发射[59] ; (b) quadrilateral perovskite MAPbBr3 nanoplatelet with the increase of pump strength, the appearance of WGM laser and the optical excitation image of nanoplatelet above and below the threshold[60]; (c) WGM
2018年,Hu等[71]在实验中证明,将CsPbBr3钙钛矿量子点嵌入硅球中比纯无机钙钛矿量子点的发光性能和稳定性要更好,如
图 4. 不同方案实现的WGM激光。(a)利用两个交叉的钙钛矿MAPbBr3纳米棒的横切面形成的WGM微腔[64];(b)可调谐尺寸的无机钙钛矿CsPbX3纳米球WGM微腔[65];(c)通过硅球作为谐振腔,实现WGM模式激光[35];(d)在可尺寸调谐的无机钙钛矿CsPbBr3微米线阵列中实现WGM激光[67]; (e)激光打印实现的钙钛矿MAPbBrxIy微盘,以及宽谱调谐的WGM激光的发射[Fig. 4. Different schemes of WGM mode laser. (a) WGM microcavity was formed by cross section of two crossed perovskite MAPbBr3 nanorods[64]; (b) tunable size of the perovskite CsPbX3 nano inorganic spheres WGM microcavity[65]; (c) WGM laser is realized by using silicon sphere as resonator[35]; (d) WGM mode laser is implemented
Fig. 4. Different schemes of WGM mode laser. (a) WGM microcavity was formed by cross section of two crossed perovskite MAPbBr3 nanorods[64]; (b) tunable size of the perovskite CsPbX3 nano inorganic spheres WGM microcavity[65]; (c) WGM laser is realized by using silicon sphere as resonator[35]; (d) WGM mode laser is implemented
图 5. 不同方案实现的WGM模式激光。(a)将无机钙钛矿CsPbBr3量子点嵌入二氧化硅球以及发光原理[72]; (b)将CsPbBr3-SiO2微米球放进直径40 μm的圆柱形微管中的发光图像以及WGM模式激光的原理[72];(c)CdS/CsPbBr3壳核结构[74]; (d) CsPbBr3/CdS核/壳结构放入圆柱形微管中产生WGM激光以及内嵌图为发光原理的图片[74]; (e)无机钙钛矿Cs4PbBr6微盘,随着激发光强增大,出现WGM激光
Fig. 5. Different schemes of WGM mode laser. (a) Schemes of inorganic perovskite CsPbBr3 quantum dots embedded silica sphere[72]; (b) CsPbBr3-SiO2 micro sphere into a diameter of 40 μm cylindrical tubes of luminous images, and the principle of laser WGM mode[72]; (c) CdS/CsPbBr3 shell/core structure[74]; (d) CsPb
3.2 F-P模式钙钛矿微纳激光器
由于半导体纳米线具有紧凑的物理尺寸、高局域性的相干光输出和光传导效率高等优点,在纳米尺寸的光电子器件领域非常有应用前景。钙钛矿材料的吸收系数大、载流子扩散长度长等优点应用于纳米线激光器,此外还有着低阈值、高品质等优点,为半导体纳米线激光器带来可观的发展前景。在纳米线的轴向方向,由于钙钛矿增益介质和空气折射率的差造成的全反射的作用将光波限制在纳米线波导内传播,光波在两个端面的反射形成F-P模式激光,如
2015年,Zhu等[44]首次实现钙钛矿纳米线激光。通过采用一步湿化学方法制造出高质量的MAPbX3钙钛矿纳米线F-P激光腔,在402 nm、150 fs、250 kHz的激光泵浦下,实现超低阈值(220 nJ/cm2),高品质因子(Q=3600)的F-P激光发射,如
图 6. 钙钛矿纳米线激光。 (a)纳米线结构发光原理图[76-77]; (b) MAPbX3钙钛矿纳米线随着泵浦光强的增加的光学图像[44]; (c)钙钛矿MAPbIxCl3-x纳米线随着泵浦强度的增加,F-P模式激光的强度分布[78]; (d)钙钛矿MAPbBr3、MAPbIxCl3-x和MAPbI3的F-P模式激光图以及激发阈值[Fig. 6. Perovskite nanowire laser. (a) Scheme of nanowire structure lasers[76-77]; (b) optical image of MAPbX3 perovskite nanowires with increased pump light intensity[44]; (c) with the increase of pumping intensity, intensity distribution of F-P mode perovskite MAPbIxCl3-x nanowires laser[
Fig. 6. Perovskite nanowire laser. (a) Scheme of nanowire structure lasers[76-77]; (b) optical image of MAPbX3 perovskite nanowires with increased pump light intensity[44]; (c) with the increase of pumping intensity, intensity distribution of F-P mode perovskite MAPbIxCl3-x nanowires laser[
虽然有机无机杂化钙钛矿纳米线激光器展示了很优秀的激光性能,但是稳定性仍然是一个问题。2016年,Eaton等[79]首次实现高稳定性和低阈值的全无机CsPbX3钙钛矿纳米线激光(长度为2~40 μm,宽度为0.2~2.3 μm),
2017年,Hu等[86]首次在低温溶液法制备的全无机钙钛矿CsPbBr3微立方块中实现单光子和双光子泵浦的性能稳定的ASE。并在飞秒激光的激发下,实现多模激射,半峰全宽为0.46 nm,品质因子为1150,如
图 7. 无机钙钛矿CsPbX3纳米线。 (a)不同泵浦强度下的纳米线发光图像[79]; (b)随着激发强度的升高,钙钛矿CsPbBr3纳米线出现F-P模式激光[79]; (c)在固定的脉冲能量激发下,纳米线激光可以维持超过1 h(相当于109个激发循环)[79];(d)钙钛矿MAPbX3纳米线阵列[84];(e)全无机钙钛矿CsPbX3纳米线阵列[85]
Fig. 7. All inorganic perovskite CsPbX3 nanowires. (a) Nanowire lasing image with different pump density[79]; (b) with the increase of excitation intensity, F-P mode laser appears on perovskite CsPbBr3 nanowires[79]; (c) nanowire laser can last for more than an hour (equivalent to 109 excitation cycles) with a fixed pulsed energy[
图 8. 不同方案的F-P模式激光。(a)全无机钙钛矿CsPbBr3微米立方块中实现F-P模式激光[86];(b)使用改良的低温溶液处理方法合成高品质钙钛矿CsPbBr3纳米立方块SEM图像[87];(c)F-P腔的晶体结构和驻波示意图[87];(d)无机钙钛矿CsPbBr3纳米立方块随着激发强度的增加实现单模激光[87];(e)立方金字塔形状的杂化钙钛矿MAPbBr3实现F-P模式的激光发射[88];(f) 立方金字
Fig. 8. Different schemes of F-P mode lasers. (a) F-P mode laser in all inorganic perovskite CsPbBr3 micron cube[86]; (b) SEM image of high-quality perovskite CsPbBr3 nano cubes using an improved low-temperature solution treatment method[87]; (c) schematic of the crystal structure and standing wave of the F-P cavity[87]; (d) inorganic
除了利用钙钛矿本身与周围环境的折射率差形成的谐振腔,外加辅助腔的F-P模式激光器也被广泛研究。2014年,Deschler等[90]首次实现垂直发射的F-P模式激光。将500 nm厚的杂化钙钛矿MAPbI3-xClx增益层放到介质镜和顶层蒸镀的金镜之间,在波长为532 nm,脉宽为0.4 ns的脉冲激发下,阈值只有0.2 μJ/pulse,如
图 9. 外加辅助腔实现F-P模式激光。(a)钙钛矿MAPbI3-xClx垂直腔F-P模式激光光谱[90]; (b) 全无机钙钛矿CsPbBr3垂直发射激光器的结构[93];(c)F-P模式激光光谱图[93];(d)钙钛矿激光器的DFB光栅的结构[94];(e)F-P模式激光[94];(f)全无机钙钛矿DFB激光器结构[Fig. 9. F-P mode laser with auxiliary cavity. (a) Perovskite MAPbI3-xClx vertical cavity F-P mode laser spectrum[90]; (b) structure of all-inorganic perovskite CsPbBr3 VCSEL[93]; (c) FP mode laser spectrogram[93]; (d) perovskite laser with DFB structure[94
Fig. 9. F-P mode laser with auxiliary cavity. (a) Perovskite MAPbI3-xClx vertical cavity F-P mode laser spectrum[90]; (b) structure of all-inorganic perovskite CsPbBr3 VCSEL[93]; (c) FP mode laser spectrogram[93]; (d) perovskite laser with DFB structure[94
3.3 随机模式钙钛矿激光
与传统的激光器不同,随机激光不需要反射镜构成的光学谐振腔。随机激光的产生主要是依赖高度无序的增益介质将光束限制在介质内部,受激发后,介质内部的粒子间多重散射将光路折叠,同时光束通过介质实现光学放大,形成激光[
胶体量子点有着尺寸可控、高荧光效率等优点[101],2015年,Yakunin等[35]首次在尺寸为10 nm的单分散的全无机钙钛矿CsPbX3胶体量子点薄膜中实现随机激光[
图 10. 随机激光。(a)利用无序介质的多重散射实现随机激光[96]。 (b)荧光图像显示出泵浦强度下,钙钛矿MAPbI3做成平面的微晶网络实现随机激光的空间分布[97];(c)低于泵浦阈值、泵浦阈值相近、高于泵浦阈值的发射光谱图[97];(d)单晶钙钛矿CsPbBr3薄膜的TEM图像[35];(e) 单晶CsPb(Br/Cl)3薄膜中的随机激光光谱图[35];(f) 一步法合成的CsPbBr3量子点用胺基介质钉扎在硅
Fig. 10. Random lasers. (a) Random lasers using multiple scattering from a disordered medium[96]; (b) fluorescent images showing the pumping intensity, spatial distribution of perovskite MAPbI3 random lasers[97]; (c) emission spectrum diagrams below the pump threshold, close to the pump threshold, and above the pump threshold[97]; (d) TEM image o
4 结束语
金属卤化物钙钛矿作为一种新兴的半导体光电材料,具有高的吸收系数、低的缺陷态密度、高的荧光量子产率、可调谐发光带隙等优异的光电性能,作为增益介质,为高品质、低阈值的高性能微纳激光的发展提供了可观的前景。
然而钙钛矿材料的稳定性严重限制着其在发光领域的发展。钙钛矿材料对周围环境(水分、氧和热)比较敏感,很容易离解;采用新的化学合成方法,通过调控形貌和发展新结构的钙钛矿材料有望提升钙钛矿激光的稳定性。其次,钙钛矿中铅元素的毒性使得钙钛矿材料的应用受阻,发展新型的无铅或少铅的钙钛矿材料,如 Sn、Bi、Cu基钙钛矿等,对钙钛矿微纳激光器的实际应用具有重要意义;另外,发展电泵浦的钙钛矿激光器也是一个极大的挑战。最后,卤化物钙钛矿作为增益介质,其材料的光物理特性,如载流子动力学,是依然困惑的问题。在钙钛矿大家族中,激子和载流子行为在改变有机和无机单元上表现出较大的差异。特别是混合钙钛矿系统不能简单地用无机半导体或有机半导体的理论来理解,因此深入了解杂化钙钛矿的基本光激发机制是非常必要的。
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Article Outline
黄斯豪, 刘征征, 杜鹃, 冷雨欣. 钙钛矿微纳激光器研究进展[J]. 激光与光电子学进展, 2020, 57(7): 071602. Sihao Huang, Zhengzheng Liu, Juan Du, Yuxin Leng. Review of Perovskite Micro -and Nano-Lasers[J]. Laser & Optoelectronics Progress, 2020, 57(7): 071602.
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