Virgin Powder Research Articles

Effect of recycling powder on the fatigue properties of AM Ti6Al4V

Additive manufacturing (AM) techniques offer significant advantages with respect to conventional manufacturing (CM) ones such as the realization of highly customized components both dealing with their geometry and their mechanical properties. An important advantage of AM is the significant reduction of wasted material with respect to CM. However, AM techniques, such as the powder bed fusion, involve during the production an amount of powder higher than that needed to realize the final component even if the excess of powder in not interested by the melting process and can be recovered and used again. However, it is obvious to expect that the new powder feedstock that include this reused powder has different morphology characteristics since it has been subjected to a thermal history in the building chamber. These changes in the material feedstock can results in a different morphology of defects and consequently in different fatigue properties even for AM components realized with the same design geometry and same process parameters. In the present study, the effect of the use of recycled powders on the fatigue properties of AM Ti6Al4V has been investigated by considering specimens realized from virgin powder and recycled powder. The specimens fracture surfaces are investigated to correlate the effect of the powder on fatigue properties with the effect on the defects’ morphology.

Influence of 17-4 PH stainless steel powder recycling on properties of SLM additive manufactured parts

Metal Additive Manufacturing (AM) processes are developing quickly. These processes have several attractive qualities, however, the quality of manufactured parts still remains a major issue that needs to be addressed if it is to become a prevalent technology in the industry. In some powder bed fusion techniques, such as Selective Laser Melting (SLM), there is a portion of initial powder that does not melt and it can be recycled to ensure the economic and environmental viability of the process. In previous research, we demonstrated the morphological, chemical and microstructural change suffered by 17-4 PH stainless steel powder after reusing it in a SLM manufacturing process. In this work, the properties of 17-4 PH stainless steel parts, printed from powder in different recycling states (virgin powder (P0) and 20 times reused powder (P20)), were evaluated, in order to establish good recycling procedures and optimise the SLM process performance. Analyses of the properties revealed a slight decrease in roughness and pore size with powder recycling. The external porosity of the samples is similar in both powder states; however, internal porosity decreases by increasing the number of reuse cycles. Regarding the microstructural analysis, a slight increase in the γ-phase is observed with the powder recycling, which leads to a slight increase in ductility and decrease in hardness of the samples. Therefore, it is concluded that the 17-4 PH powder recycling process in SLM manufacturing is adequate and recommended to ensure the economic and environmental viability of the process without adversely affecting the properties of the parts.

Sintered powder oxidation variation as a function of build height for titanium alloy produced by electron beam powder-bed fusion

• Virgin Ti-6Al-4V feedstock was shown to have oxygen content variability as a function of build height. • Powder morphology between low-oxygen and high-oxygen content particles show no differences across singular builds. • Due to the elevated temperatures in PBF-EB, Ti-6Al-4V may be gettering the build chamber during the initial build layers. It is well-established that titanium alloy (Ti-6Al-4V) powder oxidizes during electron beam powder-bed fusion (PBF-EB) due to the high background temperatures resulting from layer preheating and sintering of the powder bed before melting. However, it is not known if oxidation is homogeneous throughout the entire build area. This work investigates the potential for variation in powder oxidation as a function of build height for PBF-EB Ti-6Al-4V, up to build heights of 35 mm. Thin-walled cylindrical powder capsules were printed in proximity to solid parts in order to capture the sintered powder for controlled chemical sampling. Powders collected from the bottom 3 mm and top 3 mm of the powder capsules show no morphological differences from the virgin powder. Higher oxidation is observed at the bottom of the powder capsules, and decreases with build height to approximately zero at 35 mm height. This magnitude of oxidation and change with build height was consistent across multiple locations in multiple builds, suggesting build height is the main factor in oxidation magnitude. An increase in oxygen content of 0.02 wt.% in a single build is significant when considering the maximum allowable oxygen is only 0.13 wt.% in material specifications (ASTM F3001-14). The predominant source of oxygen must be transient. This helps prioritize some potential sources of oxygen (e.g. powder moisture) over others when developing mitigation techniques. All of these observations from this work motivate scrutiny of powder handling and mixing procedures as well as development of oxidation mitigation techniques.

Oxide dispersion strengthened IN718 owing to powder reuse in selective laser melting

Considering the high cost of powder, powder reuse is necessary for economic and sustainable selective laser melting (SLM). Since powder quality is a key factor in determining the mechanical properties of SLMed parts, it is essential to understand the effects of powder reuse on the powder quality and SLMed parts. In this study, we investigated the effects of IN718 powder reuse on SLM-processed microstructures and their mechanical properties. The SLM process was repeated 10 times using the virgin powder supplement method. As the number of powder reuses increased, the average particle size of the reused powder also increased. Additionally, the powder was oxidized by repeated reuse and resulted in oxide spots on the powder surface. The SLMed parts were recrystallized by homogenization heat treatment at 1065 °C, and the recrystallization fraction decreased with increasing extent of oxidation, i.e., the number of powder reuses. In the 10th SLM process conducted with powder reuse, the increased oxide fraction contributed to the dispersion hardening effect and simultaneously improved tensile strength and elongation.

Online monitoring of an additive manufacturing environment using a time-of-flight mass spectrometer

Laser-based Directed Energy Deposition (L-DED) is a promising additive manufacturing technology, which has broad application prospects and practical value in many fields. The nondestructive testing technology of L-DED work piece quality monitoring requires high accuracy and capability for real-time process. This work developed an online monitoring system based on a miniature electron impact ion source time-of-flight mass spectrometer (EI-TOF) and a high-speed camera, which monitored the atmosphere above the molten pool area. The number of spatters was measured using a high-speed camera. The composition of the samples and spatters was measured by using element analyzer, inductively coupled plasma mass spectrometry, and electron spectroscopy. The variation in the atmosphere was measured using EI-TOF, and the results confirmed that the O2, N2 and H2O content decreased during the L-DED process. At the laser power of 400 W, the oxygen consumptions were 92.5% and 86.4% compared with those at the laser power of 500 W and 600 W, respectively. During the L-DED process, the number of spatters decreased when the laser power was increased from 400 W to 600 W. And at the laser power of 600 W, the average number of spatters was reduced to 59.3% compared with the laser power of 400 W. It can be found that dust contained a large amount of virgin powder and little spatters. It also can be found that at the laser power of 400 W, 500 W and 600 W, the amount of oxygen in the dust was 0.544%, 0.242% and 0.159%, respectively. The relative content of oxygen in the cross section of the seam was 35.58%, 43.79% and 44.30%, respectively. The deviation of the monitoring results (H2O, N2, O2) are significant at the same power when different materials was used as the substrate.

Effect of AlSi10Mg0.4 long-term reused powder in PBF-LB/M on the mechanical properties

Laser-based powder bed fusion (PBF-LB/M) is a well-established additive manufacturing (AM) process capable of producing high quality parts with excellent mechanical properties. Industrial applications of additively manufactured parts require the usage of fresh powder which makes the process expensive, especially in case of AM machines with enlarged build envelopes. Processing long-term reused powder fits to economic yields with the drawback of increased porosity and incorporated oxides.In this study, a detailed analysis of components made of virgin and long-term reused AlSi10Mg0.4 powder is provided. The experiments reveal that process parameters qualified for the virgin powder are not working offhand for the reused powder, as an increase of porosity from less than 1% up to 3% and a decline of tensile strength as well as yield strength of about 15% are observed. The results indicate that powder degradation, which is based on the formation of hydroxides and oxides, has a significant impact on as-built microstructure as well as mechanical properties of additively manufactured parts. The amount of hydrogen and oxygen is measured for different powder conditions and the powder ageing process of AlSi10Mg0.4 is discussed in detail.

Characterization of Spatter and Sublimation in Alloy 718 during Electron Beam Melting.

Due to elevated temperatures and high vacuum levels in electron beam melting (EBM), spatter formation and accumulation in the feedstock powder, and sublimation of alloying elements from the base feedstock powder can affect the feedstock powder’s reusability and change the alloy composition of fabricated parts. This study focused on the experimental and thermodynamic analysis of spatter particles generated in EBM, and analyzed sublimating alloying elements from Alloy 718 during EBM. Heat shields obtained after processing Alloy 718 in an Arcam A2X plus machine were analyzed to evaluate the spatters and metal condensate. Comprehensive morphological, microstructural, and chemical analyses were performed using scanning electron microscopy (SEM), focused ion beam (FIB), and energy dispersive spectroscopy (EDS). The morphological analysis showed that the area coverage of heat shields by spatter increased from top (<1%) to bottom (>25%), indicating that the spatter particles had projectile trajectories. Similarly, the metal condensate had a higher thickness of ~50 μm toward the bottom of the heat shield, indicating more significant condensation of metal vapors at the bottom. Microstructural analysis of spatters highlighted that the surfaces of spatter particles sampled from the heat shields were also covered with condensate, and the thickness of the deposited condensate depended on the time of landing of spatter particles on the heat shield during the build. The chemical analysis showed that the spatter particles had 17-fold higher oxygen content than virgin powder used in the build. Analysis of the metalized layer indicated that it was formed by oxidized metal condensate and was significantly enriched with Cr due to its higher vapor pressure under EBM conditions.

A Melt Pool Temperature Model in Laser Powder Bed Fabricated CM247LC Ni Superalloy to Rationalize Crack Formation and Microstructural Inhomogeneities

This study of the laser powder bed fusion (LPBF) of γ′-strengthened Ni superalloy CM247LC focuses on the development of a melt pool temperature model to predict crack density within the alloy. This study also analyzes spatter and elemental evaporation, which might cause defects and inhomogeneities, at different melt pool temperatures. The melt pool temperature model provides more accurate predictions than the widely used energy density model. Spatter particles were collected and characterized to study their sizes and chemical compositions, compared with the virgin powder, recycled powder, and as-built samples, to probe the impact of their entrapment into the melt pool. This study also investigated Al evaporation, revealing that its extent does not correlate with the laser energy density and is believed to be rather limited by comparing the chemistry of the virgin powder and the build. Last, the impact of LPBF process parameters on the formation of these inhomogeneities, and accordingly crack formation, was studied using finite element analysis by estimating the maximum melt pool temperature and correlating it with the formation of the microstructural inhomogeneities. The morphology of the various cracking modes was associated with the process parameters.

Preparation of Cu-Cr-Zr Alloy by Laser Powder Bed Fusion: Parameter Optimization, Microstructure, Mechanical and Thermal Properties for Microelectronic Applications

Laser powder bed fusion (LPBF) technology is beneficial for the fabrication of thermal conductive materials, integrating with the predesigned structure, which shows a great potential for high heat dissipation applications. Here, a Cu–Cr–Zr alloy with relative density of 98.53% is successfully prepared by LPBF after process optimization. On this basis, microstructure, phase identification, precipitates, mechanical and thermal properties are investigated. The results demonstrate that the surface morphology of microstructure is affected by laser energy density, the α-Cu is the main phase of the LPBF sample and the virgin powder, the size of Cr spherical precipitates in some areas is about 1 μm, and the tensile fracture mode is a mixed ductile–brittle mode. Furthermore, the Vickers hardness of the LPBF Cu–Cr–Zr sample is 70.7 HV to 106.1 HV, which is higher than that of LPBF Cu and a wrought C11000 Cu, and the difference in Vickers hardness of different planes reflects the anisotropy. Ultimately, the two types of Cu–Cr–Zr alloy heat sinks are successfully fabricated, and their heat transfer coefficients are positively correlated with the volume flow. The heat dissipation performance of the cylindrical micro-needle heat sink is better, and its maximum heat transfer coefficient is 3887 W/(m2·K).

Investigation on Properties Deterioration of GF PA3200 Powder in Laser Sintering Process

This study is designed to investigate the Glass-filed GF polyamide (PA3200) GF, nylon 12 behaviour due to deterioration of the powder. For describing and understanding these causes to find systematic approach to improve the quality of parts and to reduce the orange peel texture. The thermal behaviour and melt flow rate (MFR) of the virgin and recycled were studied by differential scanning calorimetry (DSC), and melt flow rate testing (MFR). DSC results indicated that the three transitions temperatures were affected by reprocessing (number of cycles). MFR testing showed that the melt flow rate of glass filled (PA3200) powder was decreased by the temperature, time and reprocessing. The main problem related to this practice is how to choose the right amount of recycled powder to be blended with virgin powder, in order to obtain materials that have good properties, do not show significant variation from the virgin powder, without greatly deteriorate the properties of the final material with respect to the virgin one. However its quality was degraded due long hours expose at elevated temperature caused molecular chain structure and thermal properties have changed. For this reason and according to the EOS and 3D systems companies this investigation used 50% old blended with 50% virgin powder.

Laser Powder Bed Fusion of Chromium Bronze Using Recycled Powder

Laser powder bed fusion (LPBF) of Cu-0.5Cr was carried out using recycled powder taken out from the LPBF machine after previous printing. Various volumetric defects characterized the powder wherein particle size distribution was the same as virgin powder. Using recycled powder resulted in extra spherical pore formation after the LPBF process. Despite that, a relative density of 99.2% was achieved by LPBF parameters optimization. Solidified microstructure with a small volume of defects consisted of an oversaturated dendritic Cu matrix and nano-sized Cr precipitations providing strengthening mechanism occurrence. The possibility of a satisfactory level of mechanical properties with σ0.2 = 136.8 MPa, UTS = 187.4 MPa, along with 15.5% of elongation achieving, was shown.

Investigation on selective laser sintering of PA12: dimensional accuracy and mechanical performance

Purpose Selective laser sintering (SLS) has passed other techniques, thanks to its high print resolution, its ability to print microscale geometries without any additional support, its surface quality and its long-term thermal stability. However, despite the many advantages of SLS compared to fusion deposition modelling, there are still today some limitations on the materials to be printed. A limit critical from an industrial point of view is the aging of PA12 powder, i.e. the degradation of its physical and chemical performances, due to the high temperatures and the long printing cycles, thus involving a decrease of the mechanical properties of the printed parts. The purpose of this study was to charaterize mechanically and dimensionally specimens printed in PA12 through SLS by means of virgin or aged powder, i.e. powder just used for five printing cycles. Design/methodology/approach To achieve this aim, a set of specimens were designed, built, measured and mechanically tested; the obtained results were put into relationship with the values of the process parameters used to print them. Statistical tools to design the experiments and to analyse the obtained results were used. Findings The results show that the SLS process carried out through a Sintratec machine on PA12 powder has a good repeatability. To obtain the best dimensional and mechanical performances, it is needed to use virgin powder and place the part in the central zone of the printing area. Originality/value There are no scientific articles dealing with the influence of both the aging of the powder and the manufacturing parameters on the dimensional and mechanical characterization of specimens printed with SLS technique in PA12.

XPS and SEM characterization for powder recycling within 3d printing process

In recent years, recycling the powder leftover within the additive manufacturing process has been attractive for both research, development and industry production. Powder recycling can significantly enhance the sustainability of the manufacturing process, reduce the cost and avoid producing metallic waste as a potential environmental hazard. The first step in reusing the recycled powders in the 3D printing process is to characterize the microstructure and surface quality of the powder for oxidation and impurity analysis. Here, scanning electron microscopy (SEM) and x-ray photoelectron spectroscopy (XPS) have been used for the morphology and surface composition analysis of the 316L powders within the Aconity 3D printer. A new powder collection strategy has been introduced to collect powders from different locations in the powder bed: from the top most and surface of the parts and powder bed after the print terminated, from between the printed parts at different heights. The XPS measurements revealed that oxidation is a common in all the powders compared to virgin powder and more oxidation was detected from the powders collected on the very top of the leftover powder and from surface of the bed. The size of the particles does not change much but larger particles remained at the topmost surface. This finding would help in designing a protocol for collecting the recycled powder from the powder bed and it is suggested to follow a a procedure of collecting powders from the different sections of the powder bed in order to avoid mixing the most and least affected particles.

Evaluation of Inconel 718 Metallic Powder to Optimize the Reuse of Powder and to Improve the Performance and Sustainability of the Laser Powder Bed Fusion (LPBF) Process

In this paper, a detailed assessment of Inconel 718 powder, with varying degrees of degradation due to repeated use in the Laser Powder Bed Fusion (LPBF) process, has been undertaken. Four states of IN718 powder (virgin, used, overflow and spatter) were characterized in terms of their morphology, flowability and physico-chemical properties. Studies showed that used and overflow powders were almost identical. The fine particle-size distribution of the virgin powder, in which 50% of particles were found to be below the nominal particle-size distribution (PSD), was recognized as the main reason for its lower flowability and the main cause of the differentiation between virgin, used and overflow powders. Only spatter powder was found to be degraded enough to preclude its direct LPBF reuse. The oxygen content in the spatter powder exceeded the limit value for IN718 by 290 ppm, and aluminum oxide spots were found on the spatter particles surfaces. Laser absorption analysis showed 10 pp higher laser absorption compared to the other powders. The results of evaluation showed that IN718 powder is resistant to multiple uses in the LPBF process. Due to the low degradation rate of IN718 powder, overflow powder can be re-enabled for multiple uses with a proper recycling strategy.

Prediction of SLS parts properties using reprocessing powder

Purpose Owing to the operating principle of powder bed fusion processes, selective laser sintering (SLS) requires effective management of the mixture ratio of processed material previously exposed to the high temperatures of processing with new virgin material. Therefore, this paper aims to fully understand the effect that the successive reprocessing has in the powder material and to evaluate its influence on the properties of SLS parts produced at different building orientations. Design/methodology/approach Polyamide 12 material with 0%, 30% and 50% of virgin powder and parts produced from them were studied through five consecutive building cycles and their mass, mechanical, thermal and microstructural properties were evaluated. Then, the experimental data was used to validate a theoretical algorithm of prediction capable to define the minimum amount of virgin powder to be added on the processed material to produce parts without significant loss of properties. Findings Material degradation during SLS influences the mass and mechanical properties of the parts, exhibiting an exponential decay property loss until 50% of the initial values. The theoretical algorithms of reprocessing proved the appropriateness to use a mixture of 30% of virgin with 70% of processed material for the most common purposes. Practical implications This paper validates a methodology to define the minimum amount of virgin material capable to fulfil the operational specifications of SLS parts as a function of the number of building cycles, depending on the requirements of the final application. Originality/value The use of theoretical models of prediction allows to describe the degradation effects of SLS materials during the sintering, ensuring the sustainable management of the processed powder and the economic viability of the process.

Oxygen balance during laser powder bed fusion of Alloy 718

The generation of spatters during laser powder bed fusion (L-PBF) of Alloy 718 is known to be detrimental for the re-use of the feedstock powder and the quality of the final product. In this study, dedicated powder sampling from different positions within the build chamber and powder bed was performed. The results clearly indicate the importance of the surface-to-volume ratio of the built components on powder degradation, as demonstrated by the analysis of the powder using capsules filled with dense lattice structures. Extensive formation of Al- and Cr-rich oxides on the entrained powder deposited on the gas inlet and outlet was detected. Significant oxygen pick-up by spatter particles compared to the virgin powder was measured (>300 ppm O2); while the as-built material experienced a slight loss (~30 ppm O2). The change in the microstructure of spatter particles in comparison to the virgin powder, namely the primary dendrite arm spacing, indicates significantly higher cooling rate during spatter solidification, estimated to be of about 108 K/s, compared to around 106 K/s for the virgin powder and 107 K/s for the L-PBF component. These findings allows to evaluate the extent of powder degradation during L-PBF and establish the oxygen balance of the process.

A technical review of the challenges of powder recycling in the laser powder bed fusion additive manufacturing process

Laser powder bed fusion (L-PBF) is one of the most widely used additive manufacturing techniques for fabrication of components with complex geometries for various industrial applications including aerospace, medical and automotive. The unconsumed powder after part manufacturing is often recovered and recycled to improve process efficiency. However, some of the particles in the recycled powder can have different physical and chemical properties from those in the virgin powder owing to their exposure to the complex environment during the manufacturing process. In addition, some contaminants can be introduced in the recycled powder due to poor process control. A number of studies have been published in the past few years revealing the effects of powder recycling on the build properties. The present work aims to highlight the key phenomena during the manufacturing process that caused degradation to the recycled powder. Further to this, some comments, gaps and areas that deserve further detailed studies are also highlighted.

Oxygen Balance During Laser Powder Bed Fusion of Alloy 718

The generation of spatters during laser powder bed fusion (L-PBF) of Alloy 718 is known to be detrimental for the re-use of the feedstock powder and the quality of the final product. In this study, dedicated powder sampling from different positions within the build chamber and powder bed was performed. The results clearly indicate the importance of the surface-to-volume ratio of the built components on powder degradation, as demonstrated by the analysis of the powder using capsules filled with dense lattice structures. Extensive formation of Al- and Cr-rich oxides on the entrained powder deposited on the gas inlet and outlet was detected. Significant oxygen pick-up by spatter particles compared to the virgin powder was measured (>300 ppm O2); while the as-built material experienced a slight loss (~30 ppm O2). The change in the microstructure of spatter particles in comparison to the virgin powder, namely the primary dendrite arm spacing, indicates significantly higher cooling rate during spatter solidification, estimated to be of about 108 K/s, compared to around 106 K/s for the virgin powder and 107 K/s for the L-PBF component. These findings allows to evaluate the extent of powder degradation during L-PBF and establish the oxygen balance of the process.

The Effects of Virgin and Recycled PA12 Powders in SLS Processes on Occupational Exposures

Particulate matter and ultrafine particles are emitted during the pre-processing and post-processing activities of selective laser sintering (SLS) processes, which is major concern to operators exposed to the powders. This study aims to determine the occupational exposure (in terms of the total particle concentration and respirable particulate concentration) during the pre-processing and post-processing activities of SLS processes using virgin and recycled polyamide 12 (PA12) powders. Personal air sampling was performed for each activity according to the NIOSH 0500 and NIOSH 0600 methods. Based on the results, both powders were uniform spheres with a particle size of 40–60 μm. The total particulate concentration was most significant during the following pre-processing activities: 1) pouring powder into the mixing machine and 2) transferring the powder to the SLS AM machine. The total particulate concentration and respirable particulate concentration were slightly higher for the virgin powder for these activities. In conclusion, the virgin and recycled PA12 powders were both inhalable and respirable, which poses serious health hazards to the SLS AM operators. Hence, it is essential for operators to use suitable personal protective equipment (including respirators) and the working practices need to be improved by automating

Degradation of AlSi10Mg powder during laser based powder bed fusion processing

Knowledge concerning powder degradation during additive manufacturing (AM) processing is essential to improve the reusability of the powder in AM and hence maximize feedstock powder reuse and economy of the process. AlSi10Mg powder degradation in Concept Laser XLINE 2000R machine over the total period of 30 months was analyzed in order to understand the extent and mechanism affecting powder aging. Thereby, detailed analysis of the powder morphology, microstructure and surface chemistry was performed by SEM, TEM and XPS. The results show an increase in volume fraction of heavily oxidized spatter particles up to 3% in 30 months. XPS analysis of the powder surface chemistry indicates that powder particles are covered by uniform oxide layer, formed by Mg- and Al-based oxides, average thickness of which increased from ~4 nm in case of the virgin powder up to about 38 nm in case of the reused for about 30 month powder, established by XPS. Analysis of the oxide characteristics were consistent with the observed oxygen content in the sampled powder. Columnar oxide scale formation on spatter particles was revealed as well, reaching up to 125 nm in thickness measured using STEM. Results of the XPS and STEM-EDX analysis of oxide composition are shown to be in agreement with the thermodynamic calculations confirming that oxide scale on sputter particles is formed by MgAl2O4 spinel and Al2O3 (corundum) oxides.