4D microvelocimetry reveals multiphase flow field perturbations in porous media.

Many environmental and industrial processes depend on how fluids displace each other in porous materials. However, the flow dynamics that govern this process are still poorly understood, hampered by the lack of methods to measure flows in optically opaque, microscopic geometries. We introduce a 4D microvelocimetry method based on high-resolution X-ray computed tomography with fast imaging rates (up to 4 Hz). We use this to measure flow fields during unsteady-state drainage, injecting a viscous fluid into rock and filter samples. This provides experimental insight into the nonequilibrium energy dynamics of this process. We show that fluid displacements convert surface energy into kinetic energy. The latter corresponds to velocity perturbations in the pore-scale flow field behind the invading fluid front, reaching local velocities more than 40 times faster than the constant pump rate. The characteristic length scale of these perturbations exceeds the characteristic pore size by more than an order of magnitude. These flow field observations suggest that nonlocal dynamic effects may be long-ranged even at low capillary numbers, impacting the local viscous-capillary force balance and the representative elementary volume. Furthermore, the velocity perturbations can enhance unsaturated dispersive mixing and colloid transport and yet, are not accounted for in current models. Overall, this work shows that 4D X-ray velocimetry opens the way to solve long-standing fundamental questions regarding flow and transport in porous materials, underlying models of, e.g., groundwater pollution remediation and subsurface storage of CO2 and hydrogen.

Ventilatory capacity in CLAD is driven by dysfunctional airway structure.

BACKGROUND: Chronic lung allograft dysfunction (CLAD) encompasses three main phenotypes: bronchiolitis obliterans syndrome (BOS), restrictive allograft syndrome (RAS) and a Mixed phenotype combining both pathologies. How the airway structure in its entirety is affected in these phenotypes is still poorly understood. METHODS: A detailed analysis of airway morphometry was applied to gain insights on the effects of airway remodelling on the distribution of alveolar ventilation in end-stage CLAD. Ex vivo whole lung µCT and tissue-core µCT scanning of six control, six BOS, three RAS and three Mixed explant lung grafts (9 male, 9 female, 2014-2021, Leuven, Belgium) were used for digital airway reconstruction and calculation of airway dimensions in relation to luminal obstructions. FINDINGS: BOS and Mixed explants demonstrated airway obstructions of proximal bronchioles (starting at generation five), while RAS explants particularly had airway obstructions in the most distal bronchioles (generation >12). In BOS and Mixed explants 76% and 84% of bronchioles were obstructed, respectively, while this was 22% in RAS. Bronchiolar obstructions were mainly caused by lymphocytic inflammation of the airway wall or fibrotic remodelling, i.e. constrictive bronchiolitis. Proximal bronchiolectasis and imbalance in distal lung ventilation were present in all CLAD phenotypes and explain poor lung function and deterioration of specific lung function parameters. INTERPRETATION: Alterations in the structure of conducting bronchioles revealed CLAD to affect alveolar ventilatory distribution in a regional fashion. The significance of various obstructions, particularly those associated with mucus, is highlighted. FUNDING: This research was funded with the National research fund Flanders (G060322N), received by R.V.

From Corrosion Casting to Virtual Dissection: Contrast-Enhanced Vascular Imaging using Hafnium Oxide Nanocrystals.

Vascular corrosion casting is a method used to visualize the three dimensional (3D) anatomy and branching pattern of blood vessels. A polymer resin is injected in the vascular system and, after curing, the surrounding tissue is removed. The latter often deforms or even fractures the fragile cast. Here, a method is proposed that does not require corrosion, and is based on in situ micro computed tomography (micro-CT) scans. To overcome the lack of CT contrast between the polymer cast and the animals' surrounding soft tissue, hafnium oxide nanocrystals (HfO2 NCs) are introduced as CT contrast agents into the resin. The NCs dramatically improve the overall CT contrast of the cast and allow for straightforward segmentation in the CT scans. Careful design of the NC surface chemistry ensures the colloidal stability of the NCs in the casting resin. Using only 5 m% of HfO2 NCs, high-quality cardiovascular casts of both zebrafish and mice can be automatically segmented using CT imaging software. This allows to differentiate even µ $\umu$ m-scale details without having to alter the current resin injection methods. This new method of virtual dissection by visualizing casts in situ using contrast-enhanced CT imaging greatly expands the application potential of the technique.

Implementation of a dual-phase grating interferometer for multi-scale characterization of building materials by tunable dark-field imaging.

The multi-scale characterization of building materials is necessary to understand complex mechanical processes, with the goal of developing new more sustainable materials. To that end, imaging methods are often used in materials science to characterize the microscale. However, these methods compromise the volume of interest to achieve a higher resolution. Dark-field (DF) contrast imaging is being investigated to characterize building materials in length scales smaller than the resolution of the imaging system, allowing a direct comparison of features in the nano-scale range and overcoming the scale limitations of the established characterization methods. This work extends the implementation of a dual-phase X-ray grating interferometer (DP-XGI) for DF imaging in a lab-based setup. The interferometer was developed to operate at two different design energies of 22.0 keV and 40.8 keV and was designed to characterize nanoscale-size features in millimeter-sized material samples. The good performance of the interferometer in the low energy range (LER) is demonstrated by the DF retrieval of natural wood samples. In addition, a high energy range (HER) configuration is proposed, resulting in higher mean visibility and good sensitivity over a wider range of correlation lengths in the nanoscale range. Its potential for the characterization of mineral building materials is illustrated by the DF imaging of a Ketton limestone. Additionally, the capability of the DP-XGI to differentiate features in the nanoscale range is proven with the dark-field of Silica nanoparticles at different correlation lengths of calibrated sizes of 106 nm, 261 nm, and 507 nm.

Pixel-wise beam-hardening correction for dark-field signal in X-ray dual-phase grating interferometry.

The dark-field signal provided by X-ray grating interferometry is an invaluable tool for providing structural information beyond the direct spatial resolution and their variations on a macroscopic scale. However, when using a polychromatic source, the beam-hardening effect in the dark-field signal makes the quantitative sub-resolution structural information inaccessible. Especially, the beam-hardening effect in dual-phase grating interferometry varies with spatial location, inter-grating distance, and diffraction order. In this work, we propose a beam-hardening correction algorithm, taking into account all these factors. The accuracy and robustness of the algorithm are then validated by experimental results. This work contributes a necessary step toward accessing small-angle scattering structural information in dual-phase grating interferometry.

COVID-19 progression in hospitalized patients using follow-up in vivo CT and ex vivo microCT.

Background: Severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) causes coronavirus disease-19 (COVID-19) which can lead to acute respiratory distress syndrome (ARDS) and evolve to pulmonary fibrosis. Computed tomography (CT) is used to study disease progression and describe radiological patterns in COVID-19 patients. This study aimed to assess disease progression regarding lung volume and density over time on follow-up in vivo chest CT and give a unique look at parenchymal and morphological airway changes in "end-stage" COVID-19 lungs using ex vivo microCT. Methods: Volumes and densities of the lung/lobes of three COVID-19 patients were assessed using follow-up in vivo CT and ex vivo whole lung microCT scans. Airways were quantified by airway segmentations on whole lung microCT and small-partition microCT. As controls, three discarded healthy donor lungs were used. Histology was performed in differently affected regions in the COVID-19 lungs. Results: In vivo, COVID-19 lung volumes decreased while density increased over time, mainly in lower lobes as previously shown. Ex vivo COVID-19 lung volumes decreased by 60% and all lobes were smaller compared to controls. Airways were more visible on ex vivo microCT in COVID-19, probably due to fibrosis and increased airway diameter. In addition, small-partition microCT showed more deformation of (small) airway morphology and fibrotic organization in severely affected regions with heterogeneous distributions within the same lung which was confirmed by histology. Conclusions: COVID-19-ARDS and subsequent pulmonary fibrosis alters lung architecture and airway morphology which is described using in vivo CT, ex vivo microCT, and histology.

The effect of particle size on the sublimation behavior of butylhydroxytoluene as antioxidant in tablets during storage and coating.

The effect of particle size on the sublimation behavior of butylhydroxytoluene (BHT) was investigated when BHT was included as antioxidant in tablets. Sublimation of pure BHT was found to be independent of its particle size, with pore formation on the surface of all tablets after storage at room temperature and above. Moreover, a higher residual BHT content after storage was detected in tablets containing a larger size fraction. X-ray µCT scans revealed the formation of peripherally larger pores at higher BHT particle sizes, implying a slower sublimation rate in the tablet core. A stability study indicated an increase in the extent of BHT sublimation at higher temperature and longer exposure time for all size fractions. The influence of BHT particle size was more pronounced when the tablets were stored at higher temperature, but the effect receded with longer exposure time. Similar trends were seen in film-coated tablets. Due to the short exposure time to elevated temperatures, a gradient in pore size was also observed at smaller particle sizes, with peripheral pores being larger in uncoated tablets. Superficial pores disappeared when a film coating was deposited onto the tablets. After storage of the film-coated tablets, less BHT had sublimated compared to the uncoated tablet. The coating layer did not prevent sublimation, but the process was slowed down.

Characterization of Pharmaceutical Tablets by X-ray Tomography.

Solid dosage forms such as tablets are extensively used in drug administration for their simplicity and large-scale manufacturing capabilities. High-resolution X-ray tomography is one of the most valuable non-destructive techniques to investigate the internal structure of the tablets for drug product development as well as for a cost effective production process. In this work, we review the recent developments in high-resolution X-ray microtomography and its application towards different tablet characterizations. The increased availability of powerful laboratory instrumentation, as well as the advent of high brilliance and coherent 3rd generation synchrotron light sources, combined with advanced data processing techniques, are driving the application of X-ray microtomography forward as an indispensable tool in the pharmaceutical industry.

Detailed analysis of the interference patterns measured in lab-based X-ray dual-phase grating interferometry through wave propagation simulation.

In this work, we analyze the interference patterns measured in lab-based dual-phase grating interferometry and for the first time explain the spatial dependencies of the measured interference patterns and the large visibility deviations between the theoretical prediction and the experimental results. To achieve this, a simulator based on wave propagation is developed. This work proves that the experimental results can be simulated with high accuracy by including the effective grating thickness profile induced by the cone-beam geometry, the measured detector response function and a non-ideal grating shape. With the comprehensive understanding of dual-phase grating interferometry, this provides the foundations for a more efficient and accurate algorithm to retrieve sample's structure information, and the realistic simulator is a useful tool for optimizing the set-up.

Radiologic and Histologic Correlates of Early Interstitial Lung Changes in Explanted Lungs.

Background Interstitial lung abnormalities (ILAs) reflect imaging features on lung CT scans that are compatible with (early) interstitial lung disease. Despite accumulating evidence regarding the incidence, risk factors, and prognosis of ILAs, the histopathologic correlates of ILAs remain elusive. Purpose To determine the correlation between radiologic and histopathologic findings in CT-defined ILAs in human lung explants. Materials and Methods Explanted lungs or lobes from participants with radiologically documented ILAs were prospectively collected from 2010 to 2021. These specimens were air-inflated, frozen, and scanned with CT and micro-CT (spatial resolution of 0.7 mm and 90 µm, respectively). Subsequently, the lungs were cut and sampled with core biopsies. At least five samples per lung underwent micro-CT and subsequent histopathologic assessment with semiquantitative remodeling scorings. Based on area-specific radiologic scoring, the association between radiologic and histopathologic findings was assessed. Results Eight lung explants from six donors (median age at explantation, 71 years [range, 60-83 years]; four men) were included (unused donor lungs, n = 4; pre-emptive lobectomy for oncologic indications, n = 2). Ex vivo CT demonstrated ground-glass opacification, reticulation, and bronchiectasis. Micro-CT and histopathologic examination demonstrated that lung abnormalities were frequently paraseptal and associated with fibrosis and lymphocytic inflammation. The histopathologic results showed varying degrees of fibrosis in areas that appeared normal on CT scans. Regions of reticulation on CT scans generally had greater fibrosis at histopathologic analysis. Vasculopathy and bronchiectasis were also often present at histopathologic examination of lungs with ILAs. Fully developed fibroblastic foci were rarely observed. Conclusion This study demonstrated direct histologic correlates of CT-defined interstitial lung abnormalities. © RSNA, 2022 Supplemental material is available for this article. See also the editorial by Jeudy in this issue.

Development of Flow-Through Cell Dissolution Method for In Situ Visualization of Dissolution Processes in Solid Dosage Forms Using X-ray µCT.

Visualization of the dynamic behavior of pharmaceutical dosage forms during the dissolution process offers a better understanding of the drug release mechanism, enabling the design of customized dosage forms. In this study, an X-ray tomography-based approach is proposed to monitor and analyze the dynamics of the structure at the pore scale level during the dissolution process. A flow-through cell dissolution apparatus was developed, capable of mimicking the standard in vitro dissolution process, which can be easily positioned in an X-ray tomography setup. The method was utilized to study the dissolution of a Capa® (polycaprolactone)-based sustained-release 3D printed tablet. The impact of the flow rate on the active pharmaceutical ingredient (API) release rate was studied and 16 mL/min was selected as a suitable flow rate. Furthermore, cesium chloride (CsCl) was used as a contrast agent to increase the contrast between the sample and the dissolution medium. Data obtained with this novel technique were in a good agreement with the released drug rate acquired by the standard in vitro dissolution test (the similarity factor (f2) = 77%). Finally, the proposed approach allowed visualizing the internal structure of the sample, as well as real-time tracking of solution ingress into the product.

A histological description of alpaca (Vicugna pacos) cheek teeth: Findings and anatomical variations in macroscopically normal molars.

Scientific literature on veterinary dentistry in alpacas has historically focused on the description of tooth root abscesses. However, recent studies have shown a variety of other, sometimes preceding dental conditions to be widespread in this species. To allow the development and finetuning of treatment strategies in this species, a more thorough understanding of the underlying etiopathogenesis of dental disease is required. Histological studies focusing on normal dental and surrounding tissues might serve as a basis for this purpose. Nine teeth, extracted from seven alpacas were collected. All samples were retrieved from animals that died or were euthanized for non-dental reasons. Histological sections were prepared at three different levels in each tooth and examined using light microscopy focusing on the assessment of pulp tissue, dentin, cementum, periodontal tissues and the apical region. The histological appearance of the investigated dental tissues in alpacas showed great similarities with other hypsodont species. However, a rather rare type of dentin called "vasodentin" could be identified in all examined cheek teeth. Another species-specific finding was the extremely close proximity of varying neighboring tooth roots that seemed to be responsible for inducing massive resorptive lesions. The results of this study might contribute to a better understanding of the etiopathogenesis of some dental diseases in the alpaca.

Correction: Sinchuk et al. Variational and Deep Learning Segmentation of Very-Low-Contrast X-ray Computed Tomography Images of Carbon/Epoxy Woven Composites. Materials 2020, 13, 936.

We would like to change the authors' affiliation on the recent published paper [...].

Exploration of the X-ray Dark-Field Signal in Mineral Building Materials.

Mineral building materials suffer from weathering processes such as salt efflorescence, freeze-thaw cycling, and microbial colonization. All of these processes are linked to water (liquid and vapor) in the pore space. The degree of damage following these processes is heavily influenced by pore space properties such as porosity, pore size distribution, and pore connectivity. X-ray computed micro-tomography (µCT) has proven to be a valuable tool to non-destructively investigate the pore space of stone samples in 3D. However, a trade-off between the resolution and field-of-view often impedes reliable conclusions on the material's properties. X-ray dark-field imaging (DFI) is based on the scattering of X-rays by sub-voxel-sized features, and as such, provides information on the sample complementary to that obtained using conventional µCT. In this manuscript, we apply X-ray dark-field tomography for the first time on four mineral building materials (quartzite, fired clay brick, fired clay roof tile, and carbonated mineral building material), and investigate which information the dark-field signal entails on the sub-resolution space of the sample. Dark-field tomography at multiple length scale sensitivities was performed at the TOMCAT beamline of the Swiss Light Source (Villigen, Switzerland) using a Talbot grating interferometer. The complementary information of the dark-field modality is most clear in the fired clay brick and roof tile; quartz grains that are almost indistinguishable in the conventional µCT scan are clearly visible in the dark-field owing to their low dark-field signal (homogenous sub-voxel structure), whereas the microporous bulk mass has a high dark-field signal. Large (resolved) pores on the other hand, which are clearly visible in the absorption dataset, are almost invisible in the dark-field modality because they are overprinted with dark-field signal originating from the bulk mass. The experiments also showed how the dark-field signal from a feature depends on the length scale sensitivity, which is set by moving the sample with respect to the grating interferometer.

Detecting thin adhesive coatings in wood fiber materials with laboratory-based dual-energy computed tomography (DECT).

The distribution and good spreading of adhesive resins is critical for the wood-based panels industry. Full 3D non-destructive characterization is necessary, but methods are limited due to the chemical similarities between the resins and the wood fibers. For X-ray microtomography ([Formula: see text]CT), the doping of the resin with a highly attenuating contrast agent is necessary to visualize the resin distribution. However, the attenuation signal remains hard to segment clearly due to partial volume effects in the image, and phase mixing in the material. To help in the identification of the doped resin, dual-energy X-ray CT (DECT) is used to exploit the contrast agent's K-edge, based on simulations which take into account the polychromatic properties of the X-ray tube and detector response. The contrast agent's identification with DECT is validated with elemental mapping using scanning electron microscopy combined with energy-dispersive spectroscopy (SEM-EDX) on the surface of a wood-based panel sample, using data fusion between DECT and SEM-EDX. Overall, DECT results here in the first 3D identification of doped resin inside wood fiberboards, guiding the industry's efforts in further improving the durability of wood-based panels.

Poly(2-alkyl-2-oxazoline)s: A polymer platform to sustain the release from tablets with a high drug loading.

Sustaining the release of highly dosed APIs from a matrix tablet is challenging. To address this challenge, this study evaluated the performance of thermoplastic poly (2-alkyl-2-oxazoline)s (PAOx) as matrix excipient to produce sustained-release tablets via three processing routes: (a) hot-melt extrusion (HME) combined with injection molding (IM), (b) HME combined with milling and compression and (c) direct compression (DC). Different PAOx (co-)polymers and polymer mixtures were processed with several active pharmaceutical ingredients having different aqueous solubilities and melting temperatures (metoprolol tartrate (MPT), metformin hydrochloride (MTF) and theophylline anhydrous (THA)). Different PAOx grades were synthesized and purified by the Supramolecular Chemistry Group, and the effect of PAOx grade and processing technique on the in vitro release kinetics was evaluated. Using the hydrophobic poly (2-n-propyl-2-oxazoline) (P n PrOx) as a matrix excipient allowed to sustain the release of different APIs, even at a 70% (w/w) drug load. Whereas complete THA release was not achieved from the P n PrOx matrix over 24 â€‹h regardless of the processing technique, adding 7.5% w/w of the hydrophilic poly (2-ethyl-2-oxazoline) to the hydrophobic P n PrOx matrix significantly increased THA release, highlighting the relevance of mixing different PAOx grades. In addition, it was demonstrated that the release of THA was similar from co-polymer and polymer mixtures with the same polymer ratios. On the other hand, as the release of MTF from a P n PrOx matrix was fast, the more hydrophobic poly (2-sec-butyl-2-oxazoline) (P sec BuOx) was used to retard MTF release. In addition, a mixture between the hydrophilic PEtOx and the hydrophobic P sec BuOx allowed accurate tuning of the release of MTF formulations. Finally, it was demonstrated that PAOx also showed a high ability to tune the in vivo release. IM tablets containing 70% MTF and 30% P sec BuOx showed a lower in vivo bioavailability compared to IM tablets containing a low PEtOx concentration (7.5%, w/w) in combination with P sec BuOx (22.5%, w/w). Importantly, the in vivo MTF blood level from the sustained release tablets correlated well with the in vitro release profiles. In general, this work demonstrates that PAOx polymers offer a versatile formulation platform to adjust the release rate of different APIs, enabling sustained release from tablets with up to 70% w/w drug loading.

3D Correlative Imaging of Lithium Ion Concentration in a Vertically Oriented Electrode Microstructure with a Density Gradient.

The performance of Li+ ion batteries (LIBs) is hindered by steep Li+ ion concentration gradients in the electrodes. Although thick electrodes (≥300 µm) have the potential for reducing the proportion of inactive components inside LIBs and increasing battery energy density, the Li+ ion concentration gradient problem is exacerbated. Most understanding of Li+ ion diffusion in the electrodes is based on computational modeling because of the low atomic number (Z) of Li. There are few experimental methods to visualize Li+ ion concentration distribution of the electrode within a battery of typical configurations, for example, coin cells with stainless steel casing. Here, for the first time, an interrupted in situ correlative imaging technique is developed, combining novel, full-field X-ray Compton scattering imaging with X-ray computed tomography that allows 3D pixel-by-pixel mapping of both Li+ stoichiometry and electrode microstructure of a LiNi0.8 Mn0.1 Co0.1 O2 cathode to correlate the chemical and physical properties of the electrode inside a working coin cell battery. An electrode microstructure containing vertically oriented pore arrays and a density gradient is fabricated. It is shown how the designed electrode microstructure improves Li+ ion diffusivity, homogenizes Li+ ion concentration through the ultra-thick electrode (1 mm), and improves utilization of electrode active materials.

Foliar water uptake does not contribute to embolism repair in beech (Fagus sylvatica L.).

BACKGROUND AND AIMS: Foliar water uptake has recently been suggested as a possible mechanism for the restoration of hydraulically dysfunctional xylem vessels. In this paper we used a combination of ecophysiological measurements, X-ray microcomputed tomography and cryo-scanning electron microscopy during a drought treatment to fully evaluate this hypothesis. KEY RESULTS: Based on an assessment of these methods in beech (Fagus sylvatica L.) seedlings we were able to (1) confirm an increase in the amount of hydraulically redistributed water absorbed by leaves when the soil water potential decreased, and (2) locate this redistributed water in hydraulically active vessels in the stem. However, (3) no embolism repair was observed irrespective of the organ under investigation (i.e. stem, petiole or leaf) or the intensity of drought. CONCLUSIONS: Our data provide evidence for a hydraulic pathway from the leaf surface to the stem xylem following a water potential gradient, but this pathway exists only in functional vessels and does not play a role in embolism repair for beech.

Clinical insights into the three-dimensional anatomy of cheek teeth in alpacas based on micro-computed tomography - Part 2: Maxillary cheek teeth.

BACKGROUND: Scientific knowledge regarding alpaca dentistry is relatively limited despite its clinical implications. The present gap in available supportive data leads to limited treatment options for dental pathology in alpacas in comparison to other species. The main goal of this study was to gain novel insights into the general and pulp morphology of maxillary cheek teeth to allow development of more advanced treatment strategies in the future. Also, the risk of causing pulp exposure when floating maxillary cheek teeth was of particular interest. Concurent research focusing on the anatomy of mandibular cheek teeth has been performed accordingly. The results obtained in mandibular teeth are expected to be non-extrapolatable because of the structural differences between mandibular and maxillary teeth. RESULTS: Pulp morphology of maxillary cheek teeth showed great variation. A common pulp chamber was identified in 46/83 (55.4%) teeth with a mean dental age of 2 years and 7 months (± 2 years and 5 months). Pulpal segmentation was more commonly observed in teeth of increasing age. Full columnar segmentation was seen in 33/69 teeth (47.8%), whereas within-column segmentation was observed in 36/83 teeth (43.4%). Age and degree of segmentation of the pulpal tissue varied greatly according to Triadan position. Physical contact between roots of adjacent teeth was found in the majority of examined molars (range 82-94%) which resulted in morphological adaptations at the level of the root tips. The measured sub-occlusal dentinal thickness was as low as 0.46 mm above pulp horn 2 in a 14 years and 11 months old Triadan 09, emphasizing the risk of pulp exposure attributed to dental floating. CONCLUSION: This study offers an objective description of age-dependent maxillary cheek teeth pulp morphology in alpacas. Current findings are of great value to provide a basis for the development of tooth-saving techniques as a treatment for dental disease in this species. Observed physical contact between the roots of different examined molars may be a facilitating factor in the spread of apical infection in chronically diseased cases. Finally, a conservative approach regarding dental floating is recommended in order to avoid iatrogenic damage to pulp tissue.

Spin Freezing and Its Impact on Pore Size, Tortuosity and Solid State.

Spin freeze-drying, as a part of a continuous freeze-drying technology, is associated with a much higher drying rate and a higher level of process control in comparison with batch freeze-drying. However, the impact of the spin freezing rate on the dried product layer characteristics is not well understood at present. This research focuses on the relation between spin-freezing and pore size, pore shape, dried product mass transfer resistance and solid state of the dried product layer. This was thoroughly investigated via high-resolution X-ray micro-computed tomography (µCT), scanning electron microscopy (SEM), thermal imaging and solid state X-ray diffraction (XRD). It was concluded that slow spin-freezing rates resulted in the formation of highly tortuous structures with a high dried-product mass-transfer resistance, while fast spin-freezing rates resulted in lamellar structures with a low tortuosity and low dried-product mass-transfer resistance.