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X-ray microtomography is a non-destructive method that allows for detailed three-dimensional visualisation of the internal microstructure of materials. In the context of using phosphorus-rich residual streams in combustion for further ash recycling, physical properties of ash particles can play a crucial role in ensuring effective nutrient return and sustainable practices. In previous work, parameters such as surface area, porosity, and pore size distribution, were determined for ash particles. However, the image analysis involved binary segmentation followed by time-consuming manual corrections. The current work presents a method to implement deep learning segmentation and an approach for quantitative analysis of morphology, porosity, and internal microstructure. Deep learning segmentation was applied to microtomography data. The model, with U-Net architecture, was trained using manual input and algorithm prediction. 

• The trained and validated deep learning model could accurately segment material (ash) and air (pores and background) for these heterogeneous particles.
• Quantitative analysis was performed for the segmented data on porosity, open pore volume, pore size distribution, sphericity, particle wall thickness and specific surface area.
• Material features with similar intensities but different patterns, intensity variations in the background and artefacts could not be separated by manual segmentation – this challenge was resolved using the deep learning approach.

The purpose of this study was to provide detailed knowledge of the morphological properties of ash particles, including the volumetric fractions and 3D distributions of phosphates that lay within them. The ash particles came from digested sewage sludge co-combusted with K- and Si-rich wheat straw or K-rich sunflower husks. X-ray micro-tomography were combined with elemental composition and crystalline phase information to analyse the ash particles in 3D.

Analyses of differences in the X-ray attenuation enabled calculation of 3D phosphate distributions that showed high heterogeneity in the slag particles. This is underscored by a distinct absence of phosphates in iron-rich and silicon-rich parts. The slag from silicate-based wheat straw mixtures had lower average attenuation than that from sunflower husks mixtures, which contained more calcium. Calculated shares of phosphates between 7 and 17 vol% were obtained, where the highest value for a single assigned phosphate was observed in hard slag from wheat straw with 10 % sewage sludge. The porosity was notably higher for particles from pure wheat straw combustion (62 vol%), compared to the other samples (15–35 vol%). A high open pore volume fraction (60–97 vol%) indicates that a large part of the pores can be accessed by the surroundings. For all samples, more than 60 % of the discrete (closed) pores had an equivalent diameter < 30 μm, while the largest volume fraction consisted of pores with an equivalent diameter > 75 μm. Slag from sunflower husk mixtures had larger pore volumes and a greater relative number of discrete pores >75 µm compared to wheat straw mixtures.

Recycling phosphorus from waste streams for fertilization purposes could contribute to a sustainable society. The production in the pulp and paper industry results in several waste streams, among others nutrient-rich sludges in different forms. This study presents a detailed chemical and 3D characterization of ash from co-combustion of bark and two types of sludges from a paper mill; mixed sludge and biosludge. The combustion performance was investigated for these experiments and advanced analysis methods were used to characterise the ashes to correlate chemical and physical properties relevant for nutrient recycling. The elemental composition was determined by energy-dispersive X-ray spectroscopy; dominating crystalline phases by X-ray diffraction; and morphology, porosity, pore size distribution and active surface area of the slag were analysed with synchrotron-based X-ray micro-tomography and image analysis. Slag was formed in all combustion experiments to a large extent with increasing amounts with a higher proportion of sludge. Nutrient amounts indicate that slag particles from co-combustion of both biosludge and mixed sludge can be useful either as a soil improvement directly or for recovery processes. Slag from combustion of 30 wt% biosludge and 70 wt% bark contained the highest amount of phosphorus, 9 at% on a C and O free basis. Evaluation of tomography data showed that discrete and open pores could be distinguished on a micrometre scale. The porosity of the slag varied between the replicates and fuel mixtures, on average between 17 and 23 vol% for the bark and sludge mixtures. Open pore volume displayed large variations, on average 39–56 vol% of the pores were open pores connected to the surrounding volume. For all samples, 90 % of the pores were small, with an equivalent diameter under 30 μm, but the largest pore volume (80–90 %) consists of pores with an equivalent diameter over 75 μm. In soils, pores with a minimum equivalent diameter over 30 μm generally transmit water and the smaller pores store water. The slag particles have relatively thick walls, with few pore openings to the surroundings, indicating that the slag needs to be pre-treated by milling or crushing before application in the soil.

Combustion of phosphorus-rich residual streams can produce nutrient-rich ashes and these can be used either in further processing or as materials for direct nutrient recycling. The latter requires knowledge on morphological parameters of such ash particles that may impact plant growth, nutrient availability, and soil physical properties. The present work aims to determine the porosity, pore size, and specific surface area of ash particles, and discuss these properties in light of literature concerning interaction with soil water and plant roots. Bottom ash particles from combustion of sewage sludge and wheat straw and their co-combustion were analysed with X-ray microtomography. Image analysis provided information on morphology, specific surface area, porosity, and pore structure on a micrometre scale resolution. Co-combusting sewage sludge with wheat straw resulted in differences in ash particles' porosity and pore structure compared to combustion of pure fuels. Pure wheat straw ash displayed 62 vol% porosity while there was no apparent difference between 10 wt% or 30 wt% mixtures of sewage sludge, with a porosity of 29–31 vol%. Open pore volume comprise the largest part of the porosity (72–99 vol%) enabling interaction between surrounding pore water and nutrients.

Overall, the ash particles display large open volume fractions and thin particle walls which may lead to rapid weathering and extensive interaction with soil water. The particles generally contained pore openings over 200 µm towards the surroundings, which provide opportunities for interaction with microbes and roots from a variety of plant species in addition to nutrient transport by soil water.

Phosphorus has been identified as a critical element by the European Union and recycling efforts are increasingly common. An important phosphorus-containing waste stream for recycling is municipal sewage sludge (MSS), which is used directly as fertilizer to farmland. However, it contains pollutants such as heavy metals, pharmaceutical residues, polychlorinated bi-phenyls (PCBs) and nano-plastics. The interest in combustion of MSS is continuously growing, as it both reduces the volume as well as destroys the organic materials and could separate certain heavy metals from the produced ashes. This results in ashes with a potential for either direct use as fertilizer or as a suitable feedstock for upgrading processes. The aim of this study was to investigate co-combustion of MSS and biomass to create a phosphorus-rich bottom ash with a low heavy metal content. A laboratory-scale fixed-bed reactor in addition to an 8 MWth grate-boiler was used for the experimental work. The concentration of phosphorus and selected heavy metals in the bottom ashes were compared to European Union regulation on fertilizers, ash application to Swedish forests and Swedish regulations on sewage sludge application to farmland. Element concentrations were determined by ICP-AES complemented by analysis of spatial distribution with SEM-EDS and XRD analysis to determine crystalline compounds. The results show that most of the phosphorus was retained in the bottom ash, corresponding to 9-16 wt.% P2O5, while the concentration of cadmium, mercury, lead and zinc was below the limits of the regulations. However, copper, chromium and nickel concentrations exceeded these standards.

The effect of mechanical screening of severely contaminated forest fuel chips was investigated, focusing on main ash-forming elements and slagging tendency and other properties with relevance for thermal conversion. In this study, screening operations were performed according to practice on an industrial scale by combining a star screen and a supplementary windshifter in six different settings and combinations. Mechanical screening reduced the amount of ash and fine particles in the accept fraction. However, the mass losses for the different screening operations were substantial (20-50 wt %). Fuel analyses of the non-screened and the screened fuels showed that the most significant screening effect was a reduction of Si and Al, indicating an effective removal of sand and soil contaminations. However, the tested fuel's main ash-forming element's relative concentration did not indicate any improved combustion characteristics and ash-melting behavior. Samples of the accept fractions and non-screened material were combusted in a single-pellet thermogravimetric reactor, and the resulting ashes' morphology and elemental composition were analyzed by scanning electron microscopy-energy dispersive X-ray spectrometry and the crystalline phases by powder X-ray diffraction. Results from both these analyses confirmed that screening operations had no, or minor, effects on the fuels' ash chemistry and slagging tendencies, i.e., the fuels' proneness to ash melting was not improved. However, the reduction of ash and fine particles can reduce slagging and other operational problems in smaller and more sensitive combustion units.