Fayyaz Amir, Asghar Haroon, Waqas Muhammad, Kamal Asif, Al-Onazi Wedad A, Al-Mohaimeed Amal M
National Centre for Physics, Quaid-i-Azam University Campus, Islamabad 45320, Pakistan.
Department of Aerospace and Mechanical Engineering, The University of Arizona, Tucson, AZ 85721, USA.
Polymers (Basel). 2023 Jul 25;15(15):3156. doi: 10.3390/polym15153156.
The potential of using laser-induced breakdown spectroscopy (LIBS) in combination with various other spectroscopic and statistical methods was assessed for characterizing pure and MgO-doped nylon (6/6) organic polymer samples. The pure samples, obtained through a polycondensation chemical technique, were artificially doped with MgO prior to analysis for comparative purposes. These artificially doped samples served as crucial reference materials for comparative analysis and reference purposes. The LIBS studies were performed under local thermodynamic equilibrium (LTE) and optically thin plasma conditions. To assess the structural crystallinity of the nylon (6/6) polymer samples, X-ray diffraction (XRD) analysis, and Fourier transform infrared (FTIR) spectroscopy were employed to detect functional groups such as N-H, C-H, and C-N in the adsorbent polyamide nylon sample. Additionally, diffuse reflectance spectroscopy (DRS) analysis was conducted to investigate the effects of doping and temperature on the band gap and material reflectance across different sample temperatures. Chemical compositional analysis was performed using X-ray photoelectron spectroscopy (XPS) with the carbon C1s peak at 248.8 eV serving as a reference for spectrum calibration, along with energy-dispersive X-ray (EDX) analysis, which demonstrated good agreement between the techniques. To validate the different methodologies, the results obtained from CF-LIBS and EDX were compared with those from the standard inductively coupled plasma mass spectrometry (ICP-MS) technique. Finally, for classification analysis, principal component analysis (PCA) was applied to the LIBS spectral data at different sample temperatures (25 °C, 125 °C, 225 °C, and 325 °C). The analyses demonstrated that the combination of LIBS with PCA, along with other methods, presents a robust technique for polymer characterization.
评估了将激光诱导击穿光谱法(LIBS)与各种其他光谱和统计方法结合使用来表征纯尼龙(6/6)和氧化镁掺杂的尼龙(6/6)有机聚合物样品的潜力。通过缩聚化学技术获得的纯样品,在分析前人工掺杂氧化镁以作比较。这些人工掺杂的样品作为关键参考材料用于比较分析和参考目的。LIBS研究是在局部热力学平衡(LTE)和光学薄等离子体条件下进行的。为了评估尼龙(6/6)聚合物样品的结构结晶度,采用X射线衍射(XRD)分析和傅里叶变换红外(FTIR)光谱法来检测吸附性聚酰胺尼龙样品中的N-H、C-H和C-N等官能团。此外,进行了漫反射光谱(DRS)分析,以研究掺杂和温度对不同样品温度下带隙和材料反射率的影响。使用X射线光电子能谱(XPS)进行化学成分分析,以248.8 eV处的碳C1s峰作为光谱校准的参考,同时进行能量色散X射线(EDX)分析,结果表明这两种技术之间具有良好的一致性。为了验证不同的方法,将从CF-LIBS和EDX获得的结果与标准电感耦合等离子体质谱(ICP-MS)技术的结果进行了比较。最后,为了进行分类分析,将主成分分析(PCA)应用于不同样品温度(25℃、125℃、225℃和325℃)下的LIBS光谱数据。分析表明,LIBS与PCA以及其他方法的结合,为聚合物表征提供了一种强大的技术。