Multimodal X-ray and Hyperspectral Thin-Film Nano-material Evaluation and Quality Imaging

Project Information

NanoQI

Grant agreement ID: 862055

DOI

10.3030/862055

Project closed

EC signature date 12 March 2020

Start date 1 March 2020

End date 31 August 2023

Funded under

• INDUSTRIAL LEADERSHIP - Leadership in enabling and industrial technologies - Advanced materials

Total cost

€ 4 994 792,50

EU contribution

€ 4 994 792,50

Coordinated by

FRAUNHOFER GESELLSCHAFT ZUR FORDERUNG DER ANGEWANDTEN FORSCHUNG EV
Germany

Periodic Reporting for period 2 - NanoQI (Multimodal X-ray and Hyperspectral Thin-Film Nano-material Evaluation and Quality Imaging)

Reporting period: 2021-09-01 to 2023-08-31

Summary of the context and overall objectives of the project

Functional performances of nano-materials and thin films with nano-scale thickness are determined not only by material selection but also by their nano-physical dimensions, nano-scale structure and their nano-scale chemical composition. Precise characterisation of these properties is critical to develop new functional nano-materials and optimise processes toward higher performance, improved reproducibility and yield and up-scaling to larger quantities. X-ray characterisation techniques such as X-ray diffraction analysis (XRD) or X-ray reflectometry (XRR) are widely used in research laboratories for this task but are rarely used in industrial material development and assessment of production processes due to technical limitations and required high level expertise. The project NanoQI targets the development of an industry-suited, real-time and in-line capable technique to characterise nano-structure and nano-dimensions of (thin-film) nano-materials by optimisation of area-detector based XRR and XRD concepts and their multi-modal combination with a novel wide-angle hyper-spectral imaging (HSI) technique. Therewith, NanoQI will provide industry access to real time evaluation of nano-material geometry, structure and morphology and correlative imaging of deviations of these properties. NanoQI technology will be demonstrated in three relevant industrial application scenarios: in-situ process assessment in manufacturing of perovskite solar cells; large-area vacuum roll-to-roll coating of polymer webs and industrial atomic layer deposition of dielectric and gas barrier layers.

Work performed from the beginning of the project to the end of the period covered by the report and main results achieved so far

In the first 18 months, the NanoQI partners were able to commission the first prototypes of the measuring instruments, which are being configured at Bruker AXS and Norsk Elektro Optikk AS (Norway) specifically for the requirements of the project: A combined X-ray diffractometer (XRD) and X-ray reflectometer (XRR) is located at Fraunhofer FEP in Dresden (Germany). Another XRD was integrated for the first time inline into a curing oven at TNO (Netherlands) in a facility for the production of thin-film perovskite solar cells. A third unit at BAXS was set up to evaluate the multi-modal superposition of XRD and HSI in the same unit. With these devices, layer thicknesses and roughnesses in the nanometer range, as well as crystal structures of thin layers or layer stacks can be measured very precisely and at high speed. A real-time capable measurement and data analysis speed below 1 minute was demonstrated for XRR based thickness measurement on a four layer transparent electrode on plastic web.
The material data obtained in this way will serve as the basis for the generation of optical models for high-resolution HSI analysis of large coated substrate areas (10x10 cm² to 30 x 30 cm²).
At the NanoQI partner Fraunhofer IWS, machine learning algorithms were implemented to further accelerate the data analysis and to enable the determination of derived functional properties of the layers from the HSI image data based on reference data received from XRR and XRD results. NanoQI could successfully demonstrate imaging of layer thickness deviations < +- 4 % in the first step on a 220 mm wide film. In the next step the HSI camera prototypes will be installed and commissioned at the demonstration partners' facilities starting in November 2021. Subsequently, both the XRR / XRD units and the HSI systems will be evaluated in relevant scenarios (technology readiness level 6) for inline monitoring of pilot scale perovskite solar cell manufacturing, roll-to-roll vacuum deposition of transparent electrodes, optical coatings and gas barrier films and atomic layer deposition for encapsulation of flexible electronic devices as well as printing of organic semiconductors on 15 x 15 cm² in pilot scale.
At the end of the project, all the demonstration facilities were equipped with the multimodal system and TRL6 evaluation and testing for the three scenarios (FhG-FEP, FhG-IAP and TNO) were performed. Moreover, the R2R coater at FhG-FEP was ready for work with external customers.

Progress beyond the state of the art and expected potential impact (including the socio-economic impact and the wider societal implications of the project so far)

In the future, the combination of XRD, XRR and HSI integrated into the machines will significantly simplify quality control and process monitoring in the industrial production of thin functional coatings. Coating plants will use NanoQI know-how to collect spatially resolved data on the properties of the coatings with a high resolution. The data will give immediate feedback to the machine operators on whether the thin film properties still meet the product specification. In case the properties run out of the specifications, the machine operator will be able to immediately adjust process parameters and avoid producing scrap or receiving warranty complains from the customer. Therewith, manufacturing yield in thin film processing is increased significantly and scrap is reduced by more than 50%. This reduces material consumption, manufacturing cost and also the environmental footprint caused by unusable production output.
Exploitable Results (ERs) were assessed throughout the NanoQI project, as the partners were discovering the limitations and benefits of this multimodal characterization for the three selected applications. Overall, the results of the project have proven that the application potential of hyperspectral imaging, in combination with a technique to gather ground-truth data, is immense. Several partners have since participated in follow-up activities, such as the establishment of the spin-off company DIVE imaging systems GmbH., or a follow-up project granted from the Horizon Europe spring 2023 calls among the consortium partners NEO, FhG-IWS & AMI on further industrial applications of hyperspectral imaging
Moreover, in the last two months of the project, partners are evaluating potential forms of agreements to continue using the equipment in follow-up activities at the TNO, FhG-FEP and FhG-IAP sites. The coordinating institution FhG-FEP is also evaluating possibilities of follow-up research activities and projects based on the results of the NanoQI project.
Overall, the project has generated results that can serve as a solid base for further research and industrial uptake of technologies of nanomaterial characterization in Europe.

Multimodal XRD unit with HSI camera and adapted substrate transport for inline machine integration