To ensure safety when transporting dangerous goods, it is important to specify the flow properties of the respective solid filling substance of the packagings. For this purpose, the angle of repose is currently used for the UN approvals in Germany. Measurements were carried out on 12 powdery or granular substances applying the angle of repose measuring methods customary in the test centres. The results of the methods differ significantly from each other. In addition, some of the techniques cannot be applied for very cohesive or coarse‐grained materials. The results for the angle of repose show a strong scatter for some constellations (coefficient of variation more than 20%). Safety during transport of dangerous goods cannot be guaranteed with this currently practised system of measuring the angle of repose. As a consequence, an alternative parameter to characterize the flow properties of bulk materials should be used in the recognized test centers for dangerous goods packagings, such as the Hausner ratio. This approach leads to more precise test results for the substances examined (maximum coefficient of variation 2.8%). It also has advantages in terms of applicability and occupational safety. Since the flow properties are safety‐relevant, both in terms of mechanical safety and safety against the release of dangerous substances, the testing practice in the recognized test labs should be improved and standardized.

https://onlinelibrary.wiley.com/doi/pdfdirect/10.1002/pts.2678

Flow properties of powdery or granular filling substances of dangerous goods packagings—Comparison of the measurement of the angle of repose and the determination of the Hausner ratio

One novel important application of sinter‐based additive manufacturing involving binder jetting is copper‐based products. Three different variants of nominally pure copper powder having particle size distributions with D90 < 16, 22, or 31 μm were investigated in this study. The packing behavior and the flow properties using dynamic test and shear cell, as well as specific surface area were evaluated. The analyses employed illustrate the multidimensional complexity. Because different measurements capture different aspect of the powder, it is imperative to apply a characterization approach involving different methods. Surface chemical analysis by means of X‐ray photoelectron spectroscopy (XPS) showed that all powder variants were covered by Cu2O, CuO, and Cu (OH)2, with Cu2O being dominant in all cases. The finest powder with D90 < 16 μm tended to have higher relative amount of copper in divalent state. The average apparent oxide thickness estimated by XPS depth profiling showed that the two coarser variants had similar overall average oxide thickness, whereas the finest one possessed smaller oxide thickness. The surface chemistry of the powder grades is found to be related to their rheological behavior in dynamic condition. Considering the specific surface areas in combination with the average oxide thicknesses, the amount of surface bound oxygen was estimated to be about ~220 ppm for all three variants. Specific concerns need to be taken during the sintering of powder to keep oxygen level below that of electrolytic pitch copper (400 ppm).

/pdf/surface-chemical-and-geometrical-properties-of-pure-copper-132b37ep.pdf

Surface chemical and geometrical properties of pure copper powder intended for binder jetting and sintering

Our work describes an optimised procedure for granulating nanometric and fine micrometric particles by spray-drying to achieve ready-to-print α-Al2O3 powders. The study started by identifying raw materials suited for the process through complete characterisation of particles shape, size, and surface properties. Then, dispersion in diluted and concentrated water-based suspensions was achieved thanks to polyethyleneimine and the effect of gradual dispersant addition was assessed by determining ζ potential and aggregates size variation. Suspensions rheology was studied and modelled through Krieger-Dougherty equation to identify the maximum solid loading allowing sufficient feeding through the spray-dryer nozzle. Finally, optimisation of the granulation conditions was performed. The procedure has allowed to achieve size distributions with D90 < 50 μm and Hausner ratio <1.3 ensuring sufficient flowability. The granulated powders were printed and the porosity evolution of the samples after sintering was studied by mercury intrusion porosimetry and SEM analysis. 

https://re.public.polimi.it/bitstream/11311/1228598/1/1-s2.0-S2666539522000906-main.pdf

Tailoring α-alumina powder morphology through spray drying for cold consolidation by binder jetting

How to measure the angle of repose of hazardous substances in the test centres for dangerous goods packagings

The efficiency of the fabrication and the cost of feedstock materials are important constraining factors for a wider application of the laser powder bed fusion (LPBF) process in the industry. Therefore, it is necessary to investigate the feasibility of using different particle size distributions (PSD) combined with higher layer thickness for achieving higher building efficiency and cost-effectiveness. This paper focuses on the effect of PSD (0–53, 15–53, 15–75, and 15–105 μm) on the print quality and mechanical properties of the LPBF-processed Ti-6Al-4V at a layer thickness of 60 μm. The results show that volumetric energy density (VED) range, which allows the coarse powder to reach full density, becomes relatively narrower but is still capable of producing fully dense parts when the parameters are properly adjusted. Among the fully dense specimens, the surface roughness varies slightly with the increase of VED and PSD. In the case of proper parameter selection, specimens made of coarse powder can still achieve low surface roughness. Only slight differences in mechanical performance are found for specimens produced using different PSD powders as they have almost identical microstructures. The issue of the anisotropic mechanical properties of the as-built specimens is resolved after annealing treatment at 800 °C for 2 h. This study provides a guideline for producing high-quality Ti-6Al-4V parts using a higher layer thickness and coarser powders.

/pdf/effect-of-particle-size-distribution-on-the-printing-quality-1vjmfq6s.pdf

Effect of Particle Size Distribution on the Printing Quality and Tensile Properties of Ti-6Al-4V Alloy Produced by LPBF Process

The flow behavior of powders has an essential role in many industrial processes, including powder bed additive manufacturing. The characterization of the flow behavior is challenging, as different methods are available, and their suitability for an application in additive manufacturing is still controversial. In this study, six standardized methods (measurement of bulk density by ISO 60 and by ASTM B329, angle of repose by ISO 4324, discharge time by ISO 6186 and by ASTM B964–16, and Hausner Ratio by ASTM 7481–18), the rotating drum method (by GranuDrum) and powder rheometry (Anton Paar powder cell), were applied to five size fractions of a crushed quartz sand powder and compared. A statistical approach is proposed and discussed to correlate the obtained flowability indexes with the packing density of powder beds deposited layer-by-layer, and these correlations are compared between methods. Overall, the measurement of bulk density by ASTM B329 showed the best correlation with the powder bed density. Advanced methods such as the rotating drum method and powder rheometry did not demonstrate particularly good correlations, however they provided complementary information which can be useful to assess the dynamic behavior of powders.

Ilaria Baesso

Papers

Characterization of powder flow behavior for additive manufacturing