ID16B Beamline at the ESRF: a Nanoprobe for the Characterization of Nanomaterials and Nanodevices

J. Segura-Ruíz, R. Tucoulou, J. Villanova, Damien SalomonJoel Eymery, G. Martínez-Criado
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Abstract

Extended Abstract Nanomaterials and nano-devices are continuously evolving. This continuous evolution requires powerful characterization techniques to better understand and further improve the properties of the materials and the performances of the devices. The advanced characterization tools provided by synchrotron installations can play an important role in these R&D processes. Here, the compositional and optical properties of NW-based InGaN coaxial nano-Light Emitting Diodes will be studied using the ID16B hard X-ray nanoprobe beamline. The ID16B beamline at the European Synchrotron Radiation Facility (ESRF) [1] is a nano-probe that provides a focused (down to 50x50 nm), intense (up to 10 ph/s), hard X-rays (up to 33 keV) beam. ID16B offers several characterization techniques and diverse sample environments. In this study we will use X-ray fluorescence (XRF) and X-ray excited optical luminescence (XEOL) simultaneously to characterize at Liquid-He temperature InGaN/GaN coaxial nano-LEDs. The coaxial LED heterostructure was fabricated by metalorganic vapour phase epitaxy and consists of an inner n-doped GaN core (∼2 μm diameter) with five periods of InxGa1-xN/GaN MQWs shell (1.25-nm-thick InGaN well with ∼15% In concentration and 10-nm-thick GaN barrier) [2]. The nano-LEDs were dispersed on a Si substrate and pre-localized with the help of a Scanning Electron Microscope. The Si-substrate was then mounted on a liquid-He mini-cryostat compatible with the experimental setup available on the beamline ID16B and cooled down to 6 K. The sample was scanned with the 50x50 nm beam and the XRF and and XEOL signals were collected simultaneously. Both, XRF and XEOL signals were analysed using the PyMCA software [3] in order to obtain elemental and emission correlated maps. The combined use of XRF and XEOL techniques with the He-cryostat available on ID16B provided unique space-resolved information to clarify the interplay between the compositional and optical properties of these nano-devices at the nanometre scale. The sharpness of the emission features observed in the XEOL spectra thanks to the very low temperatures provided by the He-cryostat allowed the visualization nanometre sized regions of the device having very localized emission with different peak energies. This emission-energyallowed filtering was used to localize quantum-dot like regions within In-rich regions at the bottom of the coaxial LEDs, in the area where the deposition of the InGaN/GaN MQWs shell was not completed. The direct comparison between the XRF and the XEOL maps allowed to attribute this emission to InGaN nuclei with different In-concentrations in the range between x=0.01 to x=0.4. These results demonstrate the power of ID16B as a characterization tool for the study of complex nanomaterials and single nano-devices.
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ESRF上的ID16B光束线:表征纳米材料和纳米器件的纳米探针
纳米材料和纳米器件在不断发展。这种持续的发展需要强大的表征技术来更好地理解和进一步改善材料的特性和器件的性能。同步加速器装置提供的先进表征工具可以在这些研发过程中发挥重要作用。本文将利用ID16B硬x射线纳米探针光束线研究nw基InGaN同轴纳米发光二极管的组成和光学特性。欧洲同步辐射设施(ESRF)的ID16B光束线[1]是一种纳米探针,可提供聚焦(低至50x50 nm),强(高达10 ph/s),硬x射线(高达33 keV)光束。ID16B提供了几种表征技术和不同的样品环境。在这项研究中,我们将同时使用x射线荧光(XRF)和x射线激发光学发光(XEOL)来表征液- he温度下InGaN/GaN同轴纳米led。同轴LED异质结构是由金属有机气相外延制成的,由一个内n掺杂的GaN芯(直径约2 μm)和五个周期的InxGa1-xN/GaN MQWs壳(1.25 nm厚的InGaN井,浓度约15%,10 nm厚的GaN势垒)组成[2]。纳米led分散在硅衬底上,并在扫描电子显微镜的帮助下进行预定位。然后将si衬底安装在与光束线ID16B上可用的实验装置兼容的液体- he微型低温恒温器上,并冷却至6 K。用50x50 nm光束扫描样品,同时采集XRF和XEOL信号。使用PyMCA软件[3]分析XRF和XEOL信号,以获得元素和发射相关图。将XRF和XEOL技术与ID16B上的he低温恒温器结合使用,提供了独特的空间分辨信息,以阐明这些纳米器件在纳米尺度上的成分和光学性质之间的相互作用。由于氦低温恒温器提供的非常低的温度,在XEOL光谱中观察到的发射特征的清晰度使得器件的纳米尺寸区域具有非常局部的发射,具有不同的峰值能量。这种允许发射能量的滤波用于定位同轴led底部富in区域内的类量子点区域,在InGaN/GaN MQWs壳层沉积未完成的区域。XRF和XEOL图之间的直接比较允许将这种发射归因于在x=0.01至x=0.4范围内具有不同in浓度的InGaN原子核。这些结果证明了ID16B作为复杂纳米材料和单纳米器件研究的表征工具的能力。
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