Physico-chemical characterization of sterilized Ce0.75Zr0.25O2 nanoparticles by XPS / HAXPES / SEM
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Here a dataset of XPS, HAXPES and SEM measurements for the physico-chemical characterization of sterilized nanoparticles is presented. The measurements are part of the H2020 project “NanoSolveIT”. Ce<sub>0.75</sub>Zr<sub>0.25</sub>O<sub>2</sub> nanoparticles were provided by Promethean Particles and treated differently by project partners from the University of Birmingham (EMR identifiers in the project: ERM00000400, ERM00000442, ERM00000421). The particles were treated by different sterilization methods (autoclave or microwave) and BSA was or was not added as stabilizer. This finally leads to five different samples: pristine, autoclave, microwave, autoclave with BSA, microwave with BSA. Prior to the measurements, the samples were prepared from the solution as drop cast on Si wafers. First SEM and EDS measurements were performed, followed by XPS and HAXPES measurements on the same samples. Here at first survey spectra were recorded followed by high resolution spectra. For XPS / HAXPES several Si-wafers were mounted together on one platen. The platen was left in the intro chamber of the instrument for several hours before the measurement started. Equipment: SEM images were acquired with a <em>Supra 40 </em>(Zeiss) SEM equipped with a <em>Quantax 400 </em>(Bruker) SDD EDS spectrometer. For X-ray spectroscopy experiments, a combined XPS / HAXPES spectrometer (<em>Quantes </em>from ULVAC-PHI) was used, where XPS is measured at 1486.6 eV (monochromatic Al Kα source) and HAXPES at 5414.9 eV (monochromatic Cr Kα source). Here it is possible to perform the measurements at the exact same position. Data: For SEM, the data are given in .tif format. For XPS / HAXPES the raw data are given as .spe (PHI format) and .npl (VAMAS format) files. The measurement conditions are given in the data files. Naming of data: SEM: <em>sample_treatment (n)</em>, with n a consecutive number. XPS / HAXPES: For the .spe and for the corresponding .npl files <em>Pn.m.o.sample_treatment, </em>with Pn: platen-number, m: spectrum number (order of the measurements); o: point-number, of the position on the sample, sample_treatment with "m" for microwave and "a" for autoclave. The authors thank Sigrid Benemann, who performed the SEM measurements.
本数据集收录了用于灭菌纳米粒子理化表征的X射线光电子能谱(X-ray Photoelectron Spectroscopy, XPS)、硬X射线光电子能谱(Hard X-ray Photoelectron Spectroscopy, HAXPES)与扫描电子显微镜(Scanning Electron Microscopy, SEM)测量数据。该测量工作隶属于欧盟地平线2020(Horizon 2020)框架计划项目"NanoSolveIT"。 由Promethean Particles提供的Ce₀.₇₅Zr₀.₂₅O₂纳米颗粒,经伯明翰大学项目合作伙伴开展差异化处理(项目内物料识别码:ERM00000400、ERM00000442、ERM00000421)。研究人员采用两种灭菌方式(高压灭菌或微波灭菌)对颗粒进行处理,并添加或不添加牛血清白蛋白(Bovine Serum Albumin, BSA)作为稳定剂,最终得到五组不同样品:原始样、高压灭菌样、微波灭菌样、添加BSA的高压灭菌样以及添加BSA的微波灭菌样。 测量前,将样品溶液滴涂在硅片上制备待测样。首先对同一样品开展SEM与能量色散X射线谱(Energy Dispersive X-ray Spectroscopy, EDS)测量,随后进行XPS与HAXPES测量:先采集全谱,再采集高分辨谱。本次测量中,多张硅片被一同安装在样品台上,样品台在测量启动前置于仪器引入腔中静置数小时。 实验设备:SEM成像采用蔡司(Zeiss)Supra 40型扫描电子显微镜,搭配布鲁克(Bruker)Quantax 400型硅漂移探测器(Silicon Drift Detector, SDD)能谱仪。X射线光谱实验使用ULVAC-PHI公司的Quantes组合式XPS/HAXPES光谱仪:其中XPS测量采用1486.6 eV单色Al Kα激发源,HAXPES测量采用5414.9 eV单色Cr Kα激发源,该设备支持在样品同一位置开展两类测量。 数据格式:SEM数据以.tif格式存储;XPS与HAXPES的原始数据分别以.spe(PHI格式)与.npl(VAMAS格式)文件存储,测量条件均已包含在数据文件内。 数据命名规则:SEM数据命名格式为<sample_treatment (n)>,其中n为连续编号。XPS/HAXPES数据:.spe文件及其对应的.npl文件命名格式为<Pn.m.o.sample_treatment>,其中Pn为样品台编号,m为谱图编号(测量顺序),o为样品上的测量点位编号,sample_treatment字段中“m”代表微波灭菌,“a”代表高压灭菌。 作者感谢Sigrid Benemann完成本次SEM测量工作。



