IMiP - Institut für Mikroverfahrenstechnik und Partikeltechnologie
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- Agglomerieren (2)
- X-ray microtomography (2)
- contact angle (2)
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The research program “Engineered Artificial Minerals (EnAM)” addresses the challenge of recycling valuable elements from battery waste streams. These elements, such as lithium (Li), often migrate in the slag phase, in some cases as crystals. EnAM crystals represent concentrated reservoirs of these elements, which can only be effectively recycled if they are extracted from the slag matrix and then separated. Selective wet agglomeration is a separation process based on a three-phase system and is often used in coal and ore processing. The produced agglomerates in this process can be easily separated from the remaining suspension. The precise quantification of the wetting properties and adhesion strength between suspended particles and binding liquid droplets is a scientific challenge. An accurate technique suitable for adhesion force measurements in three-phase systems with micrometer-scale particles is Fluidic Force Microscopy (FluidFM®). An experimental setup with optical control is being developed to measure adhesion forces between droplets and flat/rough surfaces. This will enable precise measurements of adhesion forces between solid EnAM crystals and binding liquid droplets. Based on these measurements, optimal agglomeration conditions can be selected in the future to improve selective wet agglomeration with respect to recycling processes.
The aim of this work was to develop a novel method for studying the 3D morphology of agglomerates obtained by spherical agglomeration. It has been found, that the combination of shock-freezing the samples in a mixture of ethanol and dry ice followed by an X-ray microtomography measurement leads to useful results. Hereby, the image quality for low absorbing material like the used graphite was enhanced by propagation-based X-ray microtomography, which results in phase contrast images. We also discuss our 3D image post-processing routine, which is used to determine the morphology parameters sphericity, fractal dimension and packing density. Furthermore, a two-dimensional kernel density estimation is used to calculate the joint probability density of agglomerate size and the morphology parameter. In future, this method will be used to determine the morphological behaviour of agglomerates during the different phases of spherical agglomeration.
As productive biofilms are increasingly gaining interest in research, the quantitative monitoring of biofilm formation on- or offline for the process remains a challenge. Optical coherence tomography (OCT) is a fast and often used method for scanning biofilms, but it has difficulty scanning through more dense optical materials. X-ray microtomography (μCT) can measure biofilms in most geometries but is very time-consuming. By combining both methods for the first time, the weaknesses of both methods could be compensated. The phototrophic cyanobacterium Tolypothrix distorta was cultured in a moving bed photobioreactor inside a biocarrier with a semi-enclosed geometry. An automated workflow was developed to process µCT scans of the biocarriers. This allowed quantification of biomass volume and biofilm-coverage on the biocarrier, both globally and spatially resolved. At the beginning of the cultivation, a growth limitation was detected in the outer region of the carrier, presumably due to shear stress. In the later phase, light limitations could be found inside the biocarrier. µCT data and biofilm thicknesses measured by OCT displayed good correlation. The latter could therefore be used to rapidly measure the biofilm formation in a process. The methods presented here can help gain a deeper understanding of biofilms inside a process and detect any limitations.
Automated evaluation of contact angles in a three-phase system of selective agglomeration in liquids
(2020)
This study aims to an automated evaluation of contact angles in a three-phase system of selective agglomeration in liquids. Wetting properties, quantified by contact angles, are essential in many industries and their processes. Selective agglomeration as a three-phase system consists of a suspension liquid, a heterogeneous solid phase and an immiscible binding liquid. It offers the chance of establishing more efficient separation processes because of the shape-dependent wetting properties of fine particles (size ≤ 10 µm). In the present paper, an experimental setup for contact angle measurements of fine particles based on the Sessile Drop Method is described. Moreover, a new algorithm is discussed, which can be used to automatically compute contact angles from image data captured by a high-speed camera. The algorithm uses a marker-based watershed transform to segment the image data into regions representing the droplet, the carrier plate coated by fine particles, and the background. The main idea is a parametric modelling approach forthe time-dependent droplet’s contour by an ellipse.
The results show that the development of the dynamic contact angles towards a static contact angle can be efficiently determined based on this novel technique. These findings are useful for a detailed discrimination of wetting properties of spherical and irregularly shaped particles as well as their wetting kinetics. Also, a better understanding of selective agglomeration processes will be promoted by this user-friendly method.
