Laboratory SWAXS combined with a low-pressure impactor for quasi-online analysis of nanoparticles generated by spark discharge
Laboratory SWAXS combined with a low-pressure impactor for quasi-online analysis of nanoparticles generated by spark discharge
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DOI：
10.1016/j.jaerosci.2015.03.004
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发表时间：
2015-07-01
影响因子：
4.5
通讯作者：
Nirschl, Hermann
中科院分区：
文献类型：
--
作者：
Guo, Xiaoai;Wagner, Moritz;Nirschl, Hermann
金属纳米颗粒广泛应用于许多不同的科学技术领域。为了满足日益增长的市场需求，一种绿色和可持续的合成工艺，即在大气压下在气体中放电，最近已经朝着扩大纳米颗粒和纳米结构生产的方向发展。快速表征合成的颗粒，例如用这种方法可以更好地了解产品质量和进一步优化合成过程。本文研制了一种新的分析系统，该系统由实验室小角和广角x射线散射（SWAXS）相机和单级多孔低压冲击器（SS-MOLPI）组成，可作为惰性气体放电产生的纳米颗粒的准在线分析过程分析工具（PAT）。SS-MOLPI允许将气溶胶颗粒直接快速采样到基板上，例如，将胶带转移到SWAXS设备进行快速分析。整个采样和分析过程只需几分钟，即可在一次运行中提供有关主要粒度、聚集状态、形态和晶体性质的信息。它比SEM/TEM和XRD技术更经济、更快速。利用该测量系统对单个发生器在惰性气体中火花放电产生的不同金属和合金纳米颗粒进行了分析。除了使用SS-MOLPI进行采样外，SWAXS相机还可以应用于用乙醇等液体洗涤带有颗粒的表面过滤器并随后进行超声波处理所制备的分散体的表征。给出了有关该方法的一些实验结果，并进行了比较讨论。并与TEM和XRD参考数据库的结果进行了比较，结果吻合较好。研究发现，独特的SWAXS和SS-MOLPI组件适用于气相产生的纳米颗粒的准在线分析和质量控制，特别是适用于由大型设施提供的气溶胶产品的过程监测和控制，这些设施包含多个并联发生器，用于合成金属纳米颗粒。(C) 2015 Elsevier Ltd.版权所有。
Metal nanoparticles are widely used in many different fields of science and technology. A green and sustainable synthesis process, namely electrical discharge in gases at atmospheric pressure, has recently been advanced towards a scale-up of nanoparticle and nanostructure production in order to meet the increasing market demand. Quick characterization of particles synthesized, e.g. with this method allows better knowledge of the product quality and further optimization of the synthesis process. In this work, a new analysis system, consisting of a laboratory small- and wide-angle X-ray scattering (SWAXS) camera and a single-stage multi-orifice low-pressure impactor (SS-MOLPI), has been developed as a process analysis tool (PAT) for quasi-online analysis of nanoparticles generated by electrical discharge in inert gas. The SS-MOLPI allows quick sampling of the aerosol particles directly onto a substrate, e.g. an adhesive tape which is transferred to the SWAXS equipment for quick analysis. The entire sampling and analysis process takes a few minutes, providing information on primary particle size, aggregation state, morphology and crystalline properties in a single run. It is much more affordable and quicker than SEM/TEM and XRD techniques, respectively. Different metallic and alloyed nanostructured particles generated by spark discharge in inert gas using a single generator were analyzed with this measuring system. In addition to sampling with the SS-MOLPI, the SWAXS camera may also be applied to the characterization of dispersions prepared by washing particle-loaded surface filters with a liquid like ethanol and subsequent ultrasonication. Some selected experimental results concerning this procedure are presented and discussed in comparison. The results obtained by SWAXS were also compared with those by TEM and the XRD reference database, and good agreement has been found. The unique SWAXS and SS-MOLPI assembly was found to be suitable for quasi-online analysis and quality control of nanoparticles produced in the gas phase, and in particular for process monitoring and control of the aerosol product delivered by large-scale facilities containing multiple parallel generators for the synthesis of metal nanoparticles. (C) 2015 Elsevier Ltd. All rights reserved.