Diamond-Coated Silicon ATR Elements for Process Analytics

Infrared attenuated total reflection (ATR) spectroscopy is a common laboratory technique for the analysis of highly absorbing liquids or solid samples. However, ATR spectroscopy is rarely found in industrial processes, where inline measurement, continuous operation, and minimal maintenance are important issues. Most materials for mid-infrared (MIR) spectroscopy and specifically for ATR elements do not have either high enough infrared transmission or sufficient mechanical and chemical stability to be exposed to process fluids, abrasive components, and aggressive cleaning agents. Sapphire is the usual choice for infrared wavelengths below 5 µm, and beyond that, only diamond is an established material. The use of diamond coatings on other ATR materials such as silicon will increase the stability of the sensor and will enable the use of larger ATR elements with increased sensitivity at lower cost for wavelengths above 5 µm. Theoretical and experimental investigations of the dependence of ATR absorbances on the incidence angle and thickness of nanocrystalline diamond (NCD) coatings on silicon were performed. By optimizing the coating thickness, a substantial amplification of the ATR absorbance can be achieved compared to an uncoated silicon element. Using a compact FTIR instrument, ATR spectra of water, acetonitrile, and propylene carbonate were measured with planar ATR elements made of coated and uncoated silicon. Compared to sapphire, the long wavelength extreme of the spectral range is extended to approximately 8 μm. With effectively nine ATR reflections, the sensitivity is expected to exceed the performance of typical diamond tip probes.

A System Identification and Implementation of a Soft Sensor for Freeform Bending

The primary goal of this study is the formulation of a soft sensor that predicts industrially relevant mechanical properties for freeform bending. This serves as the foundation of a closed-loop property control. It is hypothesized that by inline measurement of hardness, predictions regarding residual hoop stresses, local strength and strain level can be achieved. A novel hardness-based correlation scheme is introduced, which is implemented into an extended Kalman filter (EKF) and allows an inline prediction of local strength, residual hoop stresses and plasticity. Furthermore, the ultrasonic contact impedance (UCI) method is validated as a suitable inline measuring solution.

A Novel Shadowgraphic Inline Measurement Technique for Image-Based Crystal Size Distribution Analysis

A novel shadowgraphic inline probe to measure crystal size distributions (CSD), based on acquired greyscale images, is evaluated in terms of elevated temperatures and fragile crystals, and compared to well-established, alternative online and offline measurement techniques, i.e., sieving analysis and online microscopy. Additionally, the operation limits, with respect to temperature, supersaturation, suspension, and optical density, are investigated. Two different substance systems, potassium dihydrogen phosphate (prisms) and thiamine hydrochloride (needles), are crystallized for this purpose at 25 L scale. Crystal phases of the well-known KH2PO4/H2O system are measured continuously by the inline probe and in a bypass by the online microscope during cooling crystallizations. Both measurement techniques show similar results with respect to the crystal size distribution, except for higher temperatures, where the bypass variant tends to fail due to blockage. Thiamine hydrochloride, a substance forming long and fragile needles in aqueous solutions, is solidified with an anti-solvent crystallization with ethanol. The novel inline probe could identify a new field of application for image-based crystal size distribution measurements, with respect to difficult particle shapes (needles) and elevated temperatures, which cannot be evaluated with common techniques.

Analysis of elastic rolling stand deformation and interstand tension effects on section faults of hot rolled wire rod and bars

The present work aims at the modelling and simulation of the hot rolling process for wire rod and bars. After the fundamentals of plasticity, which are essential for the understanding of the process characteristics have been described, typical section deviations that can be expected in wire rod and bar mills are calculated with help of a numerical simulation model. The model allows the calculation of section shapes under the influence of elastic rolling stand deformations and interstand tensions. From this computational assessment of section faults, the necessity of inline measurement and process control for wire rod and bar mills is shown. This work is part of the PIREF project which incorporates the development of sensors, control systems and process models in order to control the dimensional accuracy of hot rolled wire rod and bars. The metal forming process model, as described here is used internally as a model for the static and kinematic interactions in the rolling process inside of the control model.