Leibniz Institute of Surface Engineering (IOM), Department of Functional Coatings, Permoserstr. 15, D-04318, Leipzig, Germany.
Leibniz Institute of Surface Engineering (IOM), Department of Functional Coatings, Permoserstr. 15, D-04318, Leipzig, Germany.
Talanta. 2021 Feb 1;223(Pt 1):121696. doi: 10.1016/j.talanta.2020.121696. Epub 2020 Sep 25.
The thickness of thin layers of the conductive polymer PEDOT:PSS in the range between about 60 and 300 nm was determined by a near-infrared spectroscopic method using a hyperspectral camera. The reflection spectra of the layers do not contain bands, but consist of a moderate slope of the overall reflectance in the range between 1320 and 1850 nm. Despite the low thickness, the spectra show an extremely strong dependence on the thickness of the layers, which allows their use for quantitative measurements. The prediction of quantitative thickness data from the reflection spectra was based on a chemometric approach using the partial least squares (PLS) algorithm. Calibration was carried out by means of spin-coated layers of PEDOT:PSS, whose thickness was determined by white-light interferometry and stylus profilometry. Finally, this resulted in a calibration model with a root mean square error of prediction (RMSEP) of about 9 nm. After external validation of this model, it was used for quantitative imaging of the thickness distribution in PEDOT:PSS layers. The precision of the predicted values was confirmed by comparison with data from the reference methods. Moreover, it was shown that this approach can be also used for hyperspectral imaging of the thickness of thin printed layers and structures of this conductive polymer on polymer film or paper with excellent thickness resolution. This analytical approach opens new possibilities for in-line process control by large-scale monitoring of thickness and homogeneity of thin layers of conductive polymers.
使用高光谱相机,通过近红外光谱法确定了范围在约 60nm 至 300nm 之间的导电聚合物 PEDOT:PSS 的薄层的厚度。这些层的反射光谱不包含谱带,而是由在 1320nm 至 1850nm 范围内整体反射率的适度斜率组成。尽管厚度较低,但光谱显示出对层厚度的极强依赖性,这使其可用于定量测量。从反射光谱预测定量厚度数据的方法基于使用偏最小二乘(PLS)算法的化学计量学方法。校准是通过旋涂 PEDOT:PSS 层进行的,其厚度通过白光干涉测量法和触针轮廓测量法确定。最终,这导致预测误差(RMSEP)约为 9nm 的校准模型。对该模型进行外部验证后,将其用于 PEDOT:PSS 层的厚度分布的定量成像。通过与参考方法的数据进行比较,确认了预测值的精度。此外,还表明该方法还可以用于在聚合物膜或纸上的这种导电聚合物的薄印刷层和结构的高光谱成像,具有出色的厚度分辨率。这种分析方法通过对导电聚合物的薄层的厚度和均一性进行大规模监测,为在线过程控制开辟了新的可能性。