Effect of Si Doping on Photoluminescence Properties of GaAs Nanowires

Si掺杂对GaAs纳米线发光特性的影响 Effect of Si Doping on Photoluminescence Properties of GaAs Nanowires 1 李想(1994-)，男，吉林榆树人，硕士研究生,2016年于大连民族大学获得学士学位，主要从事半导体材料表征方面的研究。E-mail: 416944265@qq.com http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350105&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350109&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350113&type= 李想 (1994-)，男，吉林榆树人，硕士研究生,2016年于大连民族大学获得学士学位，主要从事半导体材料表征方面的研究。E-mail: 416944265@qq.com 416944265@qq.com 1 1 corresp E-mail: jl_tangcust@163.com E-mail: jl_tangcust@163.com 唐吉龙(1977-)，男，吉林长春人，博士，副研究员，博士研究生导师,2011年于长春理工大学获得博士学位，主要从事半导体材料外延生长与器件方面的研究。E-mail: jl_tangcust@163.com http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350117&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350122&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350127&type= 唐吉龙 (1977-)，男，吉林长春人，博士，副研究员，博士研究生导师,2011年于长春理工大学获得博士学位，主要从事半导体材料外延生长与器件方面的研究。E-mail: jl_tangcust@163.com jl_tangcust@163.com 1 1 1 1 1 2 1 长春理工大学　高功率半导体激光国家重点实验室，吉林 　 长春 　 130022 长春理工大学　高功率半导体激光国家重点实验室，吉林 　 长春 　 130022 State Key Laboratory of High-power Semiconductor Laser, Changchun University of Science and Technology, Changchun 130022, China State Key Laboratory of High-power Semiconductor Laser, Changchun University of Science and Technology, Changchun 130022, China 长春理工大学　理学院，吉林 　 长春 　 130022 长春理工大学　理学院，吉林 　 长春 　 130022 School of Science, Changchun University of Science and Technology, Changchun 130022, China School of Science, Changchun University of Science and Technology, Changchun 130022, China 采用分子束外延技术(MBE)在Si(111)衬底上生长了非掺杂和Si掺杂砷化镓(GaAs)纳米线(NWs)。通过扫描电子显微镜(SEM)证实了生长样品的一维性;通过X射线衍射(XRD)测试和拉曼光谱(Raman)证实了掺杂GaAs纳米线中Si的存在;通过光致发光(PL)研究了非掺杂和Si掺杂GaAs纳米线的发光来源，掺杂改变了GaAs纳米线的辐射复合机制。掺杂导致非掺杂纳米线中自由激子发光峰和纤锌矿/闪锌矿(WZ/ZB)混相结构引起的缺陷发光峰消失。 Undoped and Si-doped gallium arsenide(GaAs) nanowires(NWs) were carried out on Si(111) substrates by molecular beam epitaxy(MBE). The one-dimensional properties of the nanowires were confirmed by scanning electron microscopy(SEM).The presence of Si in doped GaAs NWs was confirmed by X-ray diffraction(XRD) and Raman spectroscopy. The luminescence source of undoped and Si doped GaAs NWs was studied by photoluminescence(PL). The PL results showed that doping changed the radiation recombination mechanism of GaAs NWs. Compared with undoped NWs, the doping results that in the free exciton emission peak and the defect-related emission peak of wurtzite and zinc blende mixed structure disappear simultaneously. 光谱学 GaAs纳米线 Si掺杂 光致发光 分子束外延 spectroscopy GaAs nanowires Si doping photoluminescence MBE 1　引言 1 由于Ⅲ-V族材料比Si具有更高的载流子迁移率和吸收系数，因此Ⅲ-Ⅴ族化合物半导体被广泛认为是下一代电子器件取代Si的更有前途的候选材料 ［ 1 1 - 2 2 1-2 ］ 。GaAs纳米线作为一种重要的Ⅲ-Ⅴ族化合物半导体材料，具有较高的光电转换效率和适中的直接带隙，因此在光电探测器 ［ 3 3 - 4 4 3-4 ］ 、场效应晶体管 ［ 5 5 - 6 6 5-6 ］ 、纳米激光器 ［ 7 7 ］ 等各种光电子器件中得到了广泛的应用。尽管目前的GaAs纳米线器件已经表现出了良好的性能，但是随着对下一代器件性能要求的不断增长，还需要提高其应用精度。 众所周知，杂质引入对于提高一维纳米光电器件的性能起着至关重要的作用。GaAs纳米线具有大的表体比和高表面态密度，使得纳米线中载流子更趋向于填充表面态，表面态作为载流子非辐射复合中心，显著降低了器件的性能 ［ 8 8 - 9 9 8-9 ］ 。最近,Sager制备了锌掺杂GaAs纳米线(N型)来抑制这一现象 ［ 10 10 ］ ,N型掺杂导致能带向上弯曲并形成电子的势垒。Ali等报道了Be掺杂GaAs纳米线(P型)导致能带向下弯曲 ［ 11 11 ］ ，形成了限制空穴的势垒。势垒可以抑制载流子向纳米线表面传输，因此掺杂可以降低表面态对器件的不利影响，从而提高器件的性能。另外,Si是具有多型掺杂行为的Ⅳ族元素,Si掺杂GaAs纳米线可能表现出N型或P型掺杂行为 ［ 12 12 ］ 。N型或P型掺杂都可以形成势垒以此来提高器件性能。因此，研究Si掺杂GaAs纳米线的性质具有重要意义。目前，对Si掺杂GaAs纳米线的电学性质已有较多的研究 ［ 13 13 - 14 14 13-14 ］ ，而对其发光机理的研究较少，因此本文主要研究Si掺杂GaAs纳米线的光学性质。 本文采用分子束外延(MBE)生长技术并利用气-液-固(VLS)生长机制在Si(111)衬底上生长非掺杂和Si掺杂GaAs纳米线。通过光致发光对其光学性质进行表征，分析了非掺杂和Si掺杂GaAs纳米线的发光机理，对进一步的材料生长和器件设计具有指导意义。 2　实验 1 实验采用DCA P600型号MBE系统在Si(111)衬底上外延生长非掺杂GaAs纳米线和Si掺杂GaAs纳米线。生长之前要先对衬底进行预处理以去除其表面杂质或有机物。首先，将衬底在乙醇溶液和去离子水中均超声清洗5 min。然后，用氮气枪将衬底表面的水吹干。为了去除衬底表面残留的水和有机物,Si(111)衬底需要经历以下几个脱气步骤。首先，将衬底送入MBE的进样室(1.33×(10 -6 10 -7 ) Pa(10 -8 10 -9 Torr))，使用卤素灯照射衬底，使其温度达到200 ℃并持续2 h;然后，将衬底转移到MBE的预处理室(1.33×10 -8 Pa(10 -10 Torr))，在400 ℃下加热2 h;最后，将即将进行纳米线生长的衬底送至生长室，在750 ℃下进行30 min的脱气处理。处理完成后，采用VLS生长机制、自催化的生长方式在Si(111)衬底上进行非掺杂GaAs纳米线的生长，生长温度为600 ℃,Ga束流压为8.25×10 -6 Pa(6.2×10 -8 Torr),Ⅴ/Ⅲ束流比为25.8，生长时间为1 h。同样的条件下，控制Si源炉温度在1 280 ℃生长Si掺杂GaAs纳米线。 采用扫描电子显微镜(SEM)对样品的形貌进行表征;采用D8 Focus型X射线衍射仪测试获得样品的XRD图;采用LabRAM HR Evolution,HORIBA光谱仪在室温下对样品进行拉曼光谱测试。利用iHR550光谱仪对样品进行了光致发光测试，采用InGaAs探测器探测光信号，探测器工作温度保持在-30 ℃。在10100 K的温度范围和20300 mW/cm 2 的激发功率密度范围内进行了光致发光测试。 3　结果与讨论 1 图1(a) 图1(a) 显示的是非掺杂GaAs纳米线SEM图像, 图1(b) 图1(b) 显示的为Si掺杂GaAs纳米线SEM图像，利用粒径分布统计得到非掺杂和Si掺杂GaAs纳米线的长度分别为4.41 μm和4.36 μm，直径均为90 nm。通过SEM图像证实了生长样品的一维性。 图2(a) 图2(a) 显示的是非掺杂和Si掺杂GaAs纳米线的XRD图，其中Si衬底的衍射峰Si(111)和Si(222)对应的角度分别为28.5°和58.9°,GaAs纳米线的衍射峰GaAs(111)和GaAs(220)对应的角度分别为27.3°和45.4°。Si掺杂后的GaAs(111)和GaAs(220)衍射峰强度明显较低，这是Si掺杂导致晶格质量下降引起的，证明了Si在纳米线中的掺杂 ［ 15 15 ］ 。通过对掺杂前后的样品进行拉曼光谱测试，进一步分析样品的成分。拉曼光谱结果如 图2(b) 图2(b) 所示,GaAs纳米线存在横向光学(TO)声子、纵向光学(LO)声子以及纤锌矿结构特有的E2声子，对应峰位分别为268.5,291.7,258.6 cm -1 ，这与文献报道的数值吻合较好 ［ 16 16 - 17 17 16-17 ］ 。Si掺杂GaAs纳米线主要存在TO、LO两个模式，对掺杂前后GaAs纳米线的拉曼光谱图进行了归一化处理，结果显示Si掺杂GaAs纳米线的LO峰强度减弱，这与文献报道的Si掺杂对LO峰的影响趋势一致 ［ 18 18 ］ 。Si掺杂GaAs纳米线中E2声子消失，证明了掺杂后纳米线中纤锌矿(WZ)结构消失，同样Raman光谱也证明了GaAs纳米线实现了Si的有效掺杂。 为了研究掺杂对GaAs纳米线发光特性的影响，进行了光致发光光谱测试。 图3 图3 显示的是非掺杂GaAs纳米线和Si掺杂GaAs纳米线在10 K下的归一化光谱对比图。从图中观察到，非掺杂GaAs纳米线的发光峰位于1.519 eV和1.494 eV处，分别标记为P1和P2;Si掺杂GaAs纳米线的发光峰位于1.457 eV和1.496 eV处，分别标记为P3和P4。掺杂导致P1、P2峰消失，发光由P3、P4峰主导，掺杂后PL光谱的半峰宽明显展宽。通过PL光谱半峰宽可计算Si掺杂GaAs纳米线的载流子浓度，关系式为 ［ 19 19 ］ : http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350164&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350166&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350168&type= 其中 FWHM 为PL的半峰宽, n 为载流子浓度。由 图3 图3 可知,Si掺杂GaAs纳米线的半峰宽为0.115 eV，由公式(1)计算得到Si掺杂GaAs纳米线中载流子浓度为5.18×10 18 cm -3 。掺杂前后纳米线的PL发光峰峰位发生改变，且掺杂后GaAs纳米线半峰宽展宽，这些现象表明Si掺杂改变了GaAs纳米线的发光机制。为了对掺杂前后GaAs纳米线的发光来源进行确认，接下来对非掺杂GaAs纳米线和Si掺杂GaAs纳米线进行了变温变功率PL光谱测试。 首先对非掺杂GaAs纳米线进行变功率PL的测试，如 图4(a) 图4(a) 所示。从图中可以看出，随着激发功率密度的升高,P1峰位并未发生移动,PL峰强度与激发功率的关系可以用来确定发光峰位的来源，发光峰的积分强度与激发功率之间存在如下关系 ［ 20 20 - 21 21 20-21 ］ : http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350176&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350177&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350179&type= 其中, I 为光谱的积分强度, I 0 为激光辐射功率, η 为辐射效率, γ 为判断辐射复合机制的常数。根据 γ 的大小可对发光的辐射机制进行判断:当1 < γ < 2时，发光来自于激子复合;当 γ ≈2时，发光源于带边发光;当 γ < 1时，为杂质或者缺陷的发光。采用公式(2)对非掺杂GaAs纳米线变功率光谱进行拟合，如 图4(b) 图4(b) 所示，拟合得到的P1峰的 γ 值为1.416，且峰位位于1.519 eV，因此推断P1为自由激子的发光 ［ 22 22 ］ ，得到P2峰的 γ 值为0.9，因此证明P2是与缺陷相关的发光。 图2(b) 图2(b) 中Raman光谱测试结果证明非掺杂GaAs纳米线中存在WZ结构特有的E2声子，证明P2是纤锌矿/闪锌矿(WZ/ZB)混相结构引起的缺陷发光峰，这与文献报道的1.494 eV附近处为WZ/ZB混相相关的峰的结论符合 ［ 23 23 ］ 。 图4(c) 图4(c) 显示的是激发功率密度为300 mW/cm 2 的变温光谱，随着温度的升高,P1峰峰位发生红移，这与Ⅲ-Ⅴ半导体材料带隙随温度升高红移的规律一致，是晶格振动导致的 ［ 24 24 ］ 。 图4(d) 图4(d) 为P1发光峰位随温度变化的拟合图，采用Varshni公式进行拟合 ［ 22 22 ］ : http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350180&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350181&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350182&type= 其中, E g 是温度为 T 时材料的带隙, E 0 是温度为0 K时的带隙, α 是Varshni系数, β 是与德拜温度相关的参数。拟合后的参数分别为 E 0 =1.519 8 eV, α =4.56×10 -4 eV/K, β =305.7 K。与文献报道的 E 0 ((1.517±0.004) eV)、 α (4.8×10 -4 6.2×10 -4 eV/K)和 β ((225±89) K)范围一致 ［ 25 25 ］ ，进一步证明P1峰是自由激子的发光。 接下来对掺杂GaAs纳米线进行变功率PL光谱测试，以对其发光来源进行判断,Si掺杂GaAs薄膜材料可能会形成与Si受主杂质相关的施主受主对(DAP)和带-受主的发光 ［ 26 26 ］ 。 图5(a) 图5(a) 为Si掺杂GaAs纳米线变功率PL光谱，插图为P3、P4的变功率拟合图，拟合得到的 γ 值分别为0.54和0.65，证明P3、P4均是与掺入的Si杂质相关的复合发光。从 图5(b) 图5(b) 可以看出,P3峰位随着激发功率密度的升高发生蓝移，这与DAP的发光规律一致,DAP的发光存在如下关系 ［ 27 27 ］ : http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350187&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350189&type= http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21350191&type= 其中, hν 表示DAP的发光能量, E g 为禁带宽度, E D 和 E A 分别表示施主和受主的电离能, ε 0 为真空介电常数, ε 为相对介电常数, r 为施主-受主分离的距离。等式的最后一项代表施主和受主之间相互的库伦作用，随着激发功率的提高，施主和受主的密度增加，从而减小了施主-受主分离的距离，导致库伦作用增强，进而增大发光能量，使DAP发光峰位发生蓝移，因此证明P3是与Si受主杂质相关的DAP发光。P4峰位随着激发功率密度的提高不发生移动，且带-受主的发光应在DAP的高能侧，因此P4是与Si受主杂质相关的带-受主复合发光。 4　结论 1 本文采用分子束外延技术，利用VLS生长机制在Si(111)衬底上生长了非掺杂和Si掺杂GaAs纳米线。通过形貌表征证实了非掺杂和Si掺杂GaAs纳米线的一维性;XRD结果显示Si掺杂使得GaAs(111)和GaAs(220)强度减弱;Raman光谱测试结果显示Si掺杂使得LO峰强度减弱，证明了Si的有效掺杂;通过PL测试分析了掺杂前后纳米线的发光来源，非掺杂GaAs纳米线存在两个发光峰，其中P1为自由激子发光,P2为WZ/ZB混相引起的缺陷发光,Si掺杂GaAs纳米线的发光峰P3为与Si受主杂质相关的DAP发光,P4为与Si受主杂质相关的带-受主发光。 参考文献: DEL ALAMO J A . 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Optical properties of high quality Cu2ZnSnSe4 thin films 10.37188/CJL.20210059 O472 + .3 A 1000-7032(2021)05-0629-06 国家自然科学基金（61674021，11674038，61704011，61904017，11804335，12074045）； 吉林省教育厅项目（JJKH20200763KJ）资助 Supported by National Natural Science Foundation of China (61674021, 11674038, 61704011, 61904017, 11804335, 12074045); Project of Education Department of Jilin Province (JJKH20200763KJ) 2021-02-09 2021-02-20 2021-05-01 2021-10-22 2021 发光学报 05 42