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At least 109 records · Page 6

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DOE OSTI2025

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↗

DOE OSTI2020

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↗

NASA NTRSDate not supplied

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↗

NASA NTRSDate not supplied

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↗

NASA NTRSDate not supplied

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

Porosity area fraction↗

NASA NTRSDate not supplied

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↗

NASA NTRSDate not supplied

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↗

DOE OSTI2022

Synergistic Porosity and Charge Effects in a Supramolecular Porphyrin Cage Promote Efficient Photocatalytic CO 2 Reduction**

Abstract We present a supramolecular approach to catalyzing photochemical CO 2 reduction through second‐sphere porosity and charge effects. An iron porphyrin box ( PB ) bearing 24 cationic groups, FePB‐2(P) , was made via post‐synthetic modification of an alkyne‐functionalized supramolecular synthon. FePB‐2(P) promotes the photochemical CO 2 reduction reaction (CO 2 RR) with 97 % selectivity for CO product, achieving turnover numbers (TON) exceeding 7000 and initial turnover frequencies (TOF max ) reaching 1400 min −1 . The cooperativity between porosity and charge results in a 41‐fold increase in activity relative to the parent Fe tetraphenylporphyrin ( FeTPP ) catalyst, which is far greater than analogs that augment catalysis through porosity ( FePB‐3(N ), 4‐fold increase) or charge (Fe p ‐tetramethylanilinium porphyrin ( Fe‐ p ‐TMA ), 6‐fold increase) alone. This work establishes that synergistic pendants in the secondary coordination sphere can be leveraged as a design element to augment catalysis at primary active sites within confined spaces.

An, Lun↗

DOE OSTI2022

Synergistic Porosity and Charge Effects in a Supramolecular Porphyrin Cage Promote Efficient Photocatalytic CO 2 Reduction**

We present a supramolecular approach to catalyzing photochemical CO 2 reduction through second-sphere porosity and charge effects. An iron porphyrin box (PB) bearing 24 cationic groups, FePB-2(P), was made via post-synthetic modification of an alkyne-functionalized supramolecular synthon. FePB-2(P) promotes the photochemical CO 2 reduction reaction (CO 2 RR) with 97 % selectivity for CO product, achieving turnover numbers (TON) exceeding 7000 and initial turnover frequencies (TOF max ) reaching 1400 min -1 . The cooperativity between porosity and charge results in a 41-fold increase in activity relative to the parent Fe tetraphenylporphyrin (FeTPP) catalyst, which is far greater than analogs that augment catalysis through porosity (FePB-3(N), 4-fold increase) or charge (Fe p-tetramethylanilinium porphyrin (Fe-p-TMA), 6-fold increase) alone. In conclusion, this work establishes that synergistic pendants in the secondary coordination sphere can be leveraged as a design element to augment catalysis at primary active sites within confined spaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

High-throughput surface characterization to identify porosity defects in additively manufactured 316L stainless steel

In the present study, a high throughput (HT) methodology is applied to rapidly assess the surface characteristics of 83 additively manufactured 316L stainless steel. The variation in surface roughness (S a ) showed a good correlation with a dimensionless number (π) and provided direct linkages to the internal porosity defects. Lack-of-fusion regime relates to high surface roughness (S a > 5 µm), low dimensionless number (π < 61), and the presence of cavities in between the melt pool tracks. Balling regime correlates to high surface roughness (S a > 5 µm), intermediate dimensionless number (61 < π < 146), and non-uniform melt pool track width. Keyhole regime shows low surface roughness (S a < 5 µm), high dimensionless number (π > 146), and a curved melt pool track. This approach accelerates the process parameter discovery and minimizes the porosity defects for the LPBF process. The impact of the defects on the as-processed tensile mechanical properties demonstrates that samples with porosity exhibit up to 10% less tensile strength and 30% less ductility than optimal samples.

316L stainless steel↗

DOE OSTI2021

Impact of electrode porosity architecture on electrochemical performances of 1 mm-thick LiFePO4 binder-free Li-ion electrodes fabricated by Spark Plasma Sintering

Thick electrodes with high active material loadings have been intensively studied over the last couple of decades in pursuit of achieving high energy density systems. To optimize and enhance the electrochemical performance of such electrodes, one has to control the pore morphology by, for example, varying the pore size and shape, and the level of porosity. In the present work, the fabrication of thick binder-free LiFePO4 (LFP) electrodes with two different pore sizes (12 and 20 mu m) and porosities (21 vol% and 44 vol%) using Spark Plasma Sintering (SPS) and templating approach is reported. The well-controlled porous architecture inside the thick electrodes is realized by fine-tuning experimental parameters. The impact of porosity architecture on electrochemical performance is quantified and correlated with the 3D tortuosity values determined from both micro-computed tomography and electrochemical impedance-based experimental methods. Based on the micro-computed tomography data analysis, estimated tortuosity values along X, Y, and Z axes reveal an anisotropic effect perpendicularly to the SPS compression axis (Z-direction). This is particularly profoundly observed in the samples with larger pores (20 mu m). The correlation between morphological properties and the rate capability performance is established indicating that the capacity loss happens mainly due to the Li-ion diffusion limitations.

Cathode material↗

DOE OSTI2025

The Role of Bedrock Circulation Depth and Porosity in Mountain Streamflow Response to Prolonged Drought

Quantitative understanding is lacking on how the depth of active groundwater circulation in bedrock affects mountain streamflow response to a multi-year drought. We use an integrated hydrological model to explore the sensitivity of a variety of streamflow metrics to bedrock circulation depth and porosity under a plausible extreme drought scenario lasting up to 5 years. Endmember depth versus hydraulic conductivity relationships and porosity values for fractured crystalline rock are simulated. With drought, a deeper circulation system with higher drainable porosity more effectively buffers minimum flow and significantly limits perennial stream loss in comparison to a shallow circulation system. Streamflow buffering is accomplished through extensive groundwater storage loss. However, deeper circulation systems experience prolonged recovery from drought in comparison to storage-limited shallow systems. Research highlights the importance of characterizing the deeper bedrock hydrogeology in mountainous watersheds to better understand and predict drought impacts on stream ecosystem health and water resource sustainability.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Towards directed energy deposition of metals using polymer-based supports: porosity of 316L stainless steel deposited on carbon-fiber-reinforced ABS

Directed energy deposition (DED) is increasingly valuable to many industries because of its high deposition rates relative to other metal additive manufacturing processes, but the design space of DED is limited. For instance, steep overhangs are difficult or impossible to manufacture. Polymer-based support structures could help address this challenge. The viability of DED on polymer composite substrates has begun to be explored, specifically with 316L stainless steel on carbon-fiber-reinforced ABS substrates. Monolithic metal components can be deposited on the polymer, but it was found that gas release during polymer degradation causes porosity due to gas entrapment in the metal. An interlayer cooling time was introduced to reduce polymer degradation and decrease the porosity due to gas entrapment, but this led to porosity from lack of fusion. The results of this work provide insight into process parameter selection and scan strategy development to enable the use of polymer support structures in blown-powder DED.

Kurfess, Rebecca↗

DOE OSTI2020

Critical instability at moving keyhole tip generates porosity in laser melting

Laser powder bed fusion is a dominant metal 3D printing technology. However, porosity defects remain a challenge for fatigue-sensitive applications. Some porosity is associated with deep and narrow vapor depressions called keyholes, which occur under high-power, low–scan speed laser melting conditions. High-speed x-ray imaging enables operando observation of the detailed formation process of pores in Ti-6Al-4V caused by a critical instability at the keyhole tip. We found that the boundary of the keyhole porosity regime in power-velocity space is sharp and smooth, varying only slightly between the bare plate and powder bed. The critical keyhole instability generates acoustic waves in the melt pool that provide additional yet vital driving force for the pores near the keyhole tip to move away from the keyhole and become trapped as defects.

47 OTHER INSTRUMENTATION↗

DOE OSTI2021

In-situ Radiography of Hydrogen Porosity Growth and Development in Aluminum Welds

In aluminum welding, hydrogen contamination is the main cause of the welding defect, porosity. Porosity in welds can adversely affect the mechanical properties such as tensile strength, fatigue life and ductility. There have been a variety of solutions to help reduce porosity in aluminum welds including finding the source of hydrogen. However, in some cases the amount of hydrogen may be drastically reduced but impossible to completely eliminate. Another approach to this issue is to understand where a pore originates and how it moves and grows within the weld pool. This information may lead to a more innovative method for pore elimination during gas tungsten arc (GTA) welding of aluminum.

42 ENGINEERING↗

DOE OSTI2024

Predicting Fracture Porosity Evolution in Sandstone (Final Report)

To better understand porosity, strength, chemical reactivity, and patterns of fractures, we developed methods using mineral deposits to unravel how fracture growth and diagenesis interact to create and destroy fracture porosity. Quartz and dolomite cement textures and associated fluid inclusion assemblage sequences and thermal histories provided data to infer the duration and rates at which fractures open. We developed and tested a model that accounts for how fracture porosity and rock properties change as a function of thermal exposure and how fracture size and arrangement evolve. Effects of cement deposits on growth were investigated with new geomechanical models and new methods to quantify fracture spatial arrangement. We tested these concepts in a wide range of rock types using outcrop and core-based datasets. We documented opening histories of fractures and fracture arrays in contrasting tectonic and thermal regimes. Our methods set a new standard for fracture characterization and our diagenetic-geomechanical model accurately predicts fluid flow characteristics of fractured rocks based on coupled effects of diagenesis and deformation. Results represent a significant advance in fundamental understanding of fractures in the Earth and have application to improving subsurface engineering operations in a wide range of contexts including geothermal and sequestration applications. The breakthrough of successfully reconstructing the timing and opening rates of parts of single fractures and portions of fracture arrays to document the growth and linkage of fracture arrays was an accomplishment of this grant that is being followed up in our current BES grant DE-SC0022968, ‘Reconstructing and Predicting Fracture Pattern Evolution‘

58 GEOSCIENCES↗

DOE OSTI2024

Influence of Spatter on Porosity, Microstructure, and Corrosion of Additively Manufactured Stainless Steel Printed Using Different Island Size

Specimens of 316 L stainless steel were printed using laser powder bed fusion (LPBF), a popular metal additive manufacturing (AM) technique, with varying island sizes. Not many researchers have considered the impact of spatter while optimizing LPBF printing parameters. In this research, the influence of spatter was considered while also investigating the effect of varied island size on the microstructure, surface roughness, microhardness, and corrosion resistance of LPBF-316 L. No correlation was observed between surface roughness or microhardness and minor variations in island size. However, a correlation was drawn between varied island sizes and porosity in LPBF-316 L. The specimens associated with larger island sizes showed significantly enhanced corrosion resistance due to fewer manufacturing defects and reduced porosity, attributed to the minimal influence of the spatter. Based on analysis, the LPBF parameters were revised, which lead to superior corrosion resistance of LPBF-316 L, attributed to high density and reduced porosity.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Measurement of density and porosity of lunar rocks based on samples of Luna 16 automatic lunar station

Three fragments of holocrystalline igneous rocks of the gabbro type, weighing 30 to 50 mg each, were investigated. The density of the fragments was established with a mercury pycnometer and was found to be 3.05 to 3.12 g/cu cm, with a relative error not more than 2 percent. The porosity was found for the difference between the volumes determined with the mercury and with the gas techniques; for all three samples together it was 13 percent, and the error of determination was 70 percent owing to the small volumes. It can be anticipated that the porosity of the rock in bulk will be higher than the value obtained based on small fragments. The porosity of lunar rocks can markedly affect the isostatic distribution of rocks and must be taken into account when developing models of lunar structure.

Volynets, V. F.↗