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At least 217 records · Page 12

Zeolite with trimodal porosity by desilication of zeolite nanocrystals aggregate

Zeolite with trimodal porosity can be synthesized by desilication of zeolite nanocrystal aggregate. In the desilication process, the originally existed intercrystalline mesopores of zeolite nanocrystal aggregate were enlarged into large mesopore, and the new small intracrystalline mesopore channel was created, thus the Zeolite with trimodal porosity was formed. The structure of resulted zeolite, both on aggregate and mesopore level can be fine tuned by the desilication degree. - Graphical abstract: The Si from the edges and boundary of nanocrystals was first removed resulted the surface roughness and enlarges of the originally existed intercrystalline mesopores. As the degree of alkali-treatment increasing, the Si species inside zeolite nanocrystals was also removed, leading to further enlarges the intercrystalline mesopores and the formation of small intracrystalline mesopores. In case the alkali-treatment is serve enough to completely dissolve the bridges between zeolite nanocrystals, zeolite nanocrystals were exfoliated from the aggregate. Highlights: Black-Right-Pointing-Pointer Zeolite with trimodal porosity by desilication of zeolite nanocrystals aggregate. Black-Right-Pointing-Pointer The original intercrystalline mesopores were enlarged into large mesopore. Black-Right-Pointing-Pointer The new intracrystalline mesopores were created as the inside Si extracted out. Black-Right-Pointing-Pointer The aggregate structure, crystallinity and acidity of parent zeolite remained. Black-Right-Pointing-Pointer Desilication is start on the edges then in the inner part of zeolite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Inducing porosity and growing carbon nanofibers in ferroin perchlorate: An example of morphological transitions in coordination complexes

Inducing porosity in solid coordination complex crystals, which are an important class of catalysts, is critical for many applications where a high surface area is required. However, unlike metal organic frameworks (MOFs), fabrication of porous coordination crystals remains a significant challenge. Here we demonstrate a simple method to produce and modulate porosity in coordination complex crystals using ferroin perchlorate, a model system that combines a common ionic complex with a very reactive counter-ion. Using thermal chemical vapor deposition (CVD), we show that by annealing ferroin perchlorate crystals at 350 °C under a flow of ethylene, hydrogen, argon, and oxygen, we induced pores in the crystal. We demonstrate that small amounts of oxygen, which may combine with hydrogen to form water, are essential for pore formation. We also demonstrate that pore size and density can be easily controlled by varying the ethylene flow. Upon raising the annealing temperature to 500 °C, we observed a second transition in which carbon nanofibers (CNFs) grew from the porous crystal. This approach represents a simple and effective method for the synthesis of porous materials with good control over pore size and density. It also enables the synthesis of complex networks of nanostructures (in our case CNFs) by simply varying process parameters such as temperature and gas flows. This represents an important advance for the fabrication of porous coordination complex crystals. - Graphical abstract: Annealing ferroin perchlorate at 350 °C induces porosity in the complex while annealing at 500 °C leads to the additional growth of carbon nanofibers Display Omitted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Combined multi-analytical approach for study of pore system in bricks: How much porosity is there?

During the firing of bricks, mineralogical and textural transformations produce an artificial aggregate characterised by significant porosity. Particularly as regards pore-size distribution and the interconnection model, porosity is an important parameter to evaluate and predict the durability of bricks. The pore system is in fact the main element, which correlates building materials and their environment (especially in cases of aggressive weathering, e.g., salt crystallisation and freeze-thaw cycles) and determines their durability. Four industrial bricks with differing compositions and firing temperatures were analysed with “direct” and “indirect” techniques, traditional methods (mercury intrusion porosimetry, hydric tests, nitrogen adsorption) and new analytical approaches based on digital image reconstruction of 2D and 3D models (back-scattered electrons and computerised X-ray micro-Tomography, respectively). The comparison of results from different analytical methods in the “overlapping ranges” of porosity and the careful reconstruction of a cumulative curve, allowed overcoming their specific limitations and achieving better knowledge on the pore system of bricks. - Highlights: •Pore-size distribution and structure of the pore system in four commercial bricks •A multi-analytical approach combining “direct” and “indirect” techniques •Traditional methods vs. new approaches based on 2D/3D digital image reconstruction •The use of “overlapping ranges” to overcome the limitations of various techniques.

36 MATERIALS SCIENCE↗

Site specific porosity-thermal performance correlations in neutron irradiated U-10Zr fuel

In this work, we present a site-specific three-dimensional analysis of porosity evolution in neutron-irradiated U–10Zr metallic fuel using high-resolution synchrotron X-ray tomography. Focused ion beam cubic lift-outs from four radial positions—fuel center, middle, edge, and fuel-cladding interaction (FCCI) zones—were imaged, reconstructed, and segmented to quantify pore volume, density, morphology, and pore connectivity. Porosity increased modestly from 5.5% at the center to 10.5% at the edge, yet pore number density increased by over two orders of magnitude in the fuel portion near the FCCI interface (from 4.8 x 10 4 to 6.0 x 10 6 pores/mm 3 ). Morphological classification revealed a progression from small spherical pores at the center to equiaxed and tortuous networks at the periphery, with enhanced orientation along the radial direction. Connectivity and permeability analysis reveal that the FCCI region maintains dense, highly interconnected pores despite a moderate volume fraction, enabling rapid fission gas transport and lanthanide migration. Effective thermal conductivity models incorporating sodium logging confirm that these site-specific pore features critically influenced heat transport during reactor irradiation. These findings demonstrate that pore topology—not just porosity fraction—controls thermal performance and thermal pathways in U–10Zr fuels, impacting fuel thermal performance in a reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Influence of scan strategy on porosity and microstructure of Ti-6Al-4V fabricated by electron beam powder bed fusion

Ti-6Al-4V is of high value in biomedical, aerospace, and industrial sectors and is ideal for additive manufacturing (AM) because of its poor machinability. In electron beam powder bed fusion of Ti-6Al-4V, a raster scan is commonly used and often results in porosity that is detrimental to the fatigue strength. In this paper, we demonstrate that spot melting can significantly minimize porosity but produces a coarser microstructure compared to raster melting. Process parameters can be optimized to achieve minimal porosity with tailored microstructures. A finite element method was used to rationalize these observations.

36 MATERIALS SCIENCE↗

A fine pore-preserved deep neural network for porosity analytics of a high burnup U-10Zr metallic fuel

Abstract U-10 wt.% Zr (U-10Zr) metallic fuel is the leading candidate for next-generation sodium-cooled fast reactors. Porosity is one of the most important factors that impacts the performance of U-10Zr metallic fuel. The pores generated by the fission gas accumulation can lead to changes in thermal conductivity, fuel swelling, Fuel-Cladding Chemical Interaction (FCCI) and Fuel-Cladding Mechanical Interaction (FCMI). Therefore, it is crucial to accurately segment and analyze porosity to understand the U-10Zr fuel system to design future fast reactors. To address the above issues, we introduce a workflow to process and analyze multi-source Scanning Electron Microscope (SEM) image data. Moreover, an encoder-decoder-based, deep fully convolutional network is proposed to segment pores accurately by integrating the residual unit and the densely-connected units. Two SEM 250 × field of view image datasets with different formats are utilized to evaluate the new proposed model’s performance. Sufficient comparison results demonstrate that our method quantitatively outperforms two popular deep fully convolutional networks. Furthermore, we conducted experiments on the third SEM 2500 × field of view image dataset, and the transfer learning results show the potential capability to transfer the knowledge from low-magnification images to high-magnification images. Finally, we use a pre-trained network to predict the pores of SEM images in the whole cross-sectional image and obtain quantitative porosity analysis. Our findings will guide the SEM microscopy data collection efficiently, provide a mechanistic understanding of the U-10Zr fuel system and bridge the gap between advanced characterization to fuel system design.

36 MATERIALS SCIENCE↗

Atomistic study of porosity impact on phonon driven thermal conductivity: Application to uranium dioxide

We present here an analytical method, based on the kinetic theory, to determine the impact of defects such as cavities on the thermal conductivity of a solid. This approach, which explicitly takes into account the effects of internal pore surfaces, will be referred to as the Phonon Interface THermal cONductivity (PITHON) model. Once exposed in the general case, this method is then illustrated in the case of uranium dioxide. It appears that taking properly into account these interface effects significantly modifies the temperature and porosity dependence of thermal conductivity with respect to that issued from either micromechanical models or more recent approaches, in particular, for small cavity sizes. More precisely, it is found that if the mean free path appears to have a major effect in this system in the temperature and porosity distribution range of interest, the variation of the specific heat at the surface of the cavity is predicted to be essential at very low temperature and small sizes for sufficiently large porosity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Phase stability, porosity distribution and microstructural evolution of amorphous Al{sub 50}Ti{sub 50} powders consolidated by electrical resistance sintering

The effect of intensity and duration of the electrical resistance sintering process on the phase stability, porosity distribution and microstructural evolution of Al{sub 50}Ti{sub 50} amorphous powders is studied. The phase transformations during the consolidation process were determined by X-ray diffraction. The porosity distribution was observed by optical and scanning electron microscopy. The amorphous phase is partially transformed to the crystalline phase during the sintering process, and formation of AlTi and AlTi{sub 3} intermetallic compounds occurs for temperatures higher than 300 °C. Finally, it is observed that the compacts core have lower porosity and a higher tendency to the amorphous-crystalline phase transformation than the periphery.

36 MATERIALS SCIENCE↗

POROSITY AND BAND-STRENGTH MEASUREMENTS OF MULTI-PHASE COMPOSITE ICES

We use experimental mid-infrared optical constants and extended effective medium approximations to determine the porosity and the band strengths of multi-phase composite ices grown at 30 K. A set of porous H{sub 2}O:CH{sub 4} ices are taken as a prototypical example. As a benchmark and proof of concept, the stoichiometry of the ice constituents is retreived with good accuracy from the refractive indices and the extinction coefficients of the reference binary ice mixtures with known compositions. Accurate band strengths are then calculated from experimental mid-infrared spectra of complex ices. We notice that the presence of pores has only a small effect on the overall band strengths, whereas a water dilution can considerably alter them. Different levels of porosity are observed depending on the abundance of methane used as a gas contaminant premixed with water prior to background deposition. The absorption profiles are also found to vary with deposition rate. To explain this, we use Monte Carlo simulations and we observe that the deposition rate strongly affects the pore size distribution as well as the ice morphology through reorganization processes. Extrapolated to genuine interstellar ices, the methodology presented in this paper can be used to evaluate the porosity and to quantify the relative abundances from observational data.

74 ATOMIC AND MOLECULAR PHYSICS↗

Structural analysis of cortical porosity applied to HR-pQCT data

Purpose: The investigation of cortical porosity is an important aspect of understanding biological, pathoetiological, and biomechanical processes occurring within the skeleton. With the emergence of HR-pQCT as a noninvasive tool suitable for clinical use, cortical porosity at appendicular sites can be directly visualizedin vivo. The aim of this study was to introduce a novel topological analysis of the cortical pore network for HR-pQCT data and determine the influence of resolution on measures of cortical pore network microstructure and topology. Methods: Cadaveric radii were scanned using HR-pQCT at two different voxel sizes (41 and 82μm) and also using μCT at a voxel size of 18 μm. HR-pQCT and μCT image sets were spatially coregistered. Segmentation and quantification of cortical porosity (Ct.Po) and mean pore diameter (Ct.Po.Dm) were achieved using an established extended cortical analysis technique. Topological classification of individual pores was performed using topology-preserving skeletonization and multicolor dilation algorithms. Based on the pore skeleton topological classification, the following parameters were quantified: total number of planar surface-skeleton canals (N.Slabs), tubular curve-skeleton canals (N.Tubes), and junction elements (N.Junctions), mean slab volume (Slab.Vol), mean tube volume (Tube.Vol), mean slab orientation (Slab.θ), mean tube orientation (Tube.θ), N.Slabs/N.Tubes, and integral (total) slab volume/integral tube volume (iSlab.Vol/iTube.Vol). An in vivo reproducibility study was also conducted to assess short-term precision of the topology parameters. Precision error was characterized using root mean square coefficient of variation (RMSCV%). Results: Correlations toμCT values for Ct.Po were significant for both the 41 and 82 μm HR-pQCT data (41: r{sup 2} = 0.82, p < 0.001, 82: r{sup 2} = 0.75, p < 0.001). For Ct.Po.Dm, only the 41 μm data were significantly predictive of μCT values (r{sup 2} = 0.72, p < 0.01) Data at both HR-pQCT voxel sizes were strongly predictive of the μCT values for N.Slabs (41: r{sup 2} = 0.93, p < 0.001; 82: r{sup 2} = 0.84, p < 0.001), N.Tubes (41: r{sup 2} = 0.94, p < 0.001; 82: r{sup 2} = 0.84, p < 0.001), and N.Junctions (41: r{sup 2} = 0.93, p < 0.001; 82: r{sup 2} = 0.78, p < 0.001), though proportional bias was evident in these correlations. Weak correlations were seen for iSlab.Vol/iTube.Vol at both voxel sizes (41: r{sup 2} = 0.52, p < 0.01; 82: r{sup 2} = 0.39, p < 0.05). Slab.Vol was significantly correlated to μCT data at 41 μm (r{sup 2} = 0.60, p < 0.01) but not at 82 μm, while Tube.Vol was significantly correlated at both voxel sizes (41: r{sup 2} = 0.79, p < 0.001; 82: r{sup 2} = 0.68, p < 0.01). In vivo precision error for these parameters ranged from 2.31 to 9.68 RMSCV%. Conclusions: Strong correlations betweenμCT- and HR-pQCT-derived measurements were found, particularly in HR-pQCT images obtained at 41 μm. These data are in agreement with our previous study investigating the effect of voxel size on standard HR-pQCT metrics of trabecular and cortical microstructure, and extend our previous findings to include topological descriptors of the cortical pore network.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Reduction of Porosity in Cementitious Waste Forms to Reduce Effective Diffusivity

Although current practices meet regulations for grout waste forms, development of sequestration materials and techniques for contaminants of concern could expand the use of grout waste forms and reduce risk to established processes from future compositional changes. There are contaminants in waste streams that are not permanently and completely sequestered in current grout waste forms under certain conditions. These contaminants include methyl mercury, 129 I, 99 Tc, and nitrate. Each of these species have minor fractions that are not permanently and completely isolated from the environment and therefore potentially contribute to long-term environmental impacts. An approach of interest includes the technique of reducing porosity to result in reduced leachability of all contaminants simultaneously. The current Savannah River Site (SRS) saltstone formulation was used to evaluate the relationship between leachability and porosity reduced waste forms by altering the water-to-binder ratio. Results indicated decreasing the water-to-binder directly reduced porosity and resulted in the waste form’s ability to more effectively immobilize nitrate. This work was funded by the Department of Energy Office of Environmental Management (DOE-EM) Technology Operations Office (TOO) Project # HQ221818.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Effect of laser power on roughness and porosity in laser powder bed fusion of stainless steel 316L alloys measured by X-ray tomography

The quality of metal objects fabricated via laser powder bed fusion are highly affected by process parameters, and their influence on final products is yet to be fully explored. In this work, pyrometry signals of the melt pool were collected from a set of stainless-steel samples during manufacturing and the effect of laser power on porosity and roughness of final printed parts was analyzed. Results show that the melt pool pyrometry signal of contours increases with higher laser power, whereas it is lower and decreases for the infilled part. Post-built X-ray computed tomography imaging reveals that porosity decreases while sample roughness increases upon increasing laser power. The decrease in porosity with increasing laser power is attributed to the larger size of the contour welds that were printed first, leading to an increase in dimension of the final products.

36 MATERIALS SCIENCE↗

In-Situ Detection of Process-Induced Porosity During Cure of Out-of-Autoclave Composites

Composite materials offer unique benefits in aerospace applications and are becoming increasingly used by industry manufacturers. Current manufacturing and processing methods can lead to defects in the composites, which are identified after fabrication using inspection methods.This study utilized a high-temperature ultrasonic inspection system to detect process-induced porosity in an out-of-autoclave (OOA) composite panel. An ultrasonic scanner was enclosed in a nitrogen-cooled insulating box that prevented thermal damage from the industrial oven to the temperature-sensitive electronics. Inspection of the composite part was performed through the bottom of the enclosure, which served as the tool plate for the part. In this study, a porosity gradient was introduced through a misfit of the part and caul plate. Using the data obtained from B-scans and amplitude C-scans throughout the cure cycle, the high and low porosity regions within the composite laminate were detected and localized. OOA tests aided the transition of this system to an autoclave, which is the primary method of curing aerospace-grade thermoset composites.

In-process, Defect Detection, Cure Monitoring, Por↗

Porosity Area Fraction Analysis of Bonded Borosilicate Specimens From in-Situ Optical Imagery

Image segmentation methods are routinely used to analyze data derived in nondestructive testing scenarios. A typical problem in this area is to estimate porosity from X-ray Computed Tomography (CT) inspections. This investigation aims to understand the effectiveness of open-source image segmentation methods for porosity estimation from optical images in the context of strength analysis of bonded materials and provides a benchmark of performance against a standard commercial software package. The rank ordering of the specimens by porosity area fraction is consistent across both methods.

Porosity area fraction↗

Porosity Area Fraction Analysis of Bonded Borosilicate Specimens From in-Situ Optical Imagery

Image segmentation methods are routinely used to analyze data derived in nondestructive testing scenarios. A typical problem in this area is to estimate porosity from X-ray Computed Tomography (CT) inspections. This investigation aims to understand the effectiveness of open-source image segmentation methods for porosity estimation from optical images in the context of strength analysis of bonded materials and provides a benchmark of performance against a standard commercial software package. The rank ordering of the specimens by porosity area fraction is consistent across both methods.

Porosity area fraction↗

Near Infrared In-situ Measurements for the Detection of Keyhole Porosity in Autogenous Ti-6AL-4V Welds

Certification of additive manufactured metal parts requires nondestructive evaluation (NDE) to ensure build quality. NDE can be performed during the build process or post build. For large parts with complex geometries, post build NDE can be challenging. In-situ NDE potentially provides a way to perform the inspection layer by layer. This work explores the use of a high speed near infrared (NIR) camera that is focused in-line with a laser to obtain high spatial and temporal resolution thermal imagery of the melt pool and associated cooling areas. The thermal data is obtained during a laser melting process using Ti-6AL-4V plate and of particular interest is the detection of keyhole porosity. Keyhole porosity can result from non-optimal build conditions, such as excessive laser power at a given laser scanning speed, that creates an entrapped bubble. The NIR measured melt pool and cooling areas are processed to detect keyhole porosity. The results are compared to X-ray CT results for validation.

additive manufacturing↗

Near Infrared In-situ Measurements for the Detection of Keyhole Porosity in Autogenous Ti-6AL-4V Welds

Certification of additive manufactured metal parts requires nondestructive evaluation (NDE) to ensure build quality. NDE can be performed during the build process or post build. For large parts with complex geometries, post build NDE can be challenging. In-situ NDE potentially provides a way to perform the inspection layer by layer. This work explores the use of a high speed near infrared (NIR) camera that is focused in-line with a laser to obtain high spatial and temporal resolution thermal imagery of the melt pool and associated cooling areas. The thermal data is obtained during a laser melting process using a Ti-6Al-4V plate and of particular interest is the detection of keyhole porosity. Keyhole porosity can result from non-optimal build conditions, such as excessive laser power at a given laser scanning speed, that creates an entrapped bubble. The NIR measured melt pool and cooling areas are processed to detect keyhole porosity. The results are compared to X-ray CT results for validation. Small keyhole pores buried deep were not detectable with this technique, however, some larger subsurface elongated pores along with some open surface pores did show some promise for detectability.

additive manufacturing↗

High frequency acoustic microscopy for the determination of porosity and Young's modulus in high burnup uranium dioxide nuclear fuel

During irradiation UO{sub 2} nuclear fuel experiences the development of a non-uniform distribution of porosity which contributes to establish varying mechanical properties along the radius of the pellet. Radial variations of the porosity and of elastic properties in high burnup UO{sub 2} pellet can be investigated via high frequency acoustic microscopy. Ultrasound waves are generated by a piezoelectric transducer and focused on the sample, after having travelled through a coupling liquid. The elastic properties of the material are related to the velocity of the generated Rayleigh surface wave (VR). A 67 MWd/kgU UO{sub 2} pellet was characterized using the acoustic microscope installed in the hot cells of the Institute of Transuranium Elements: 90 MHz frequency was applied, methanol was used as coupling liquid and VR was measured at different radial positions. By comparing the porosity values obtained via acoustic microscopy with those determined using ceramographic image analysis a good agreement was found, especially in the areas close to the centre. In addition Young's modulus was calculated and its radial profile was correlated to the corresponding burnup profile. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗