Powder sphericity
The impact of powder type on sphericity of particles are individually compared. For each factor, first the comparison plots of powders collected from the main bin are discussed, followed by the same discussion for powders from the cyclone bin. To always have a comparison basis between as-received (shown as AR in the plots) powder and the powder spheroidized with different process parameters, the as-received powder’s curve is included in all plots.
As-received of all powders
Before comparing the spheroidized powders, first the powder characteristics in their pre-spheroidization conditions (as-received) should be characterized. Figure 2 shows the analysis of sphericity for the as-received conditions of all three types of powder. The used powder in the EB-PBF process shows almost the same sphericity as the virgin powder. Such finding can be desirable since from a particle geometry viewpoint, the particles were not deteriorated even after 20 times of recycling with the EB-PBF process. Based on this result, the powder can be reused for the next EB-PBF builds without concerning about particle sphericity. For the reconditioned powder (the oxygen-reduced used powder), the sphericity got worse, suggesting that during oxygen reconditioning treatment some detrimental effects were occurred to the particles’ sphericity.
Virgin powder
Figure 3 illustrates the particle geometries of virgin powder before and after spheroidization. The virgin powder is perfectly spheroidized in the main chamber while the spheroidized virgin powder collected from the cyclone bin shows irregular geometries. The sphericity of virgin powder in its as-received and spheroidized conditions can be seen in Figure 4. The sphericity of powder collected from the main bin after spheroidization is shown in Figure 4a, and that of the powder collected from the cyclone bin is displayed in Figure 4b. The powder particles collected from the main bin show considerably higher sphericity after the spheroidization process while the powders in the cyclone bin show similar sphericity to that of their as-received condition. The sphericity deterioration of cyclone’s powder can be explained by the smaller particle size for powder in cyclone bin; the smaller molten droplets adhered to each other and created non-spherical particles. Having said that, it should be noted that even the least spherical powder in this comparison, i.e., the virgin as-received powder particles, is still very spherical with aspect ratio values close to unity.
Used powder
The SEM images corresponding to each powder condition are shown in Figure 5. Appearance of several largely welded particles in the used1-main powder is observable; it seems several particles were adhered together during the melting step of spheroidization process and have created some large particles with satellites. In contrast, the used1-cyclone particles show high sphericity with small particle size; the appearance of satellites is rare in the used1-cyclone. As mentioned, it should be noted that the used1-main powder was fed as the as-received condition of the second round of spheroidization. The used2-main powder is composed of large particles with sharp edges; the solidification striation lines are left on particle surfaces at the intersection areas of welded multi-particles which are caused by the impact of second round of particle re-heating and surface tension re-creation. The same is true for used2-cyclone with smaller sizes.
The sphericity of used powder in three conditions of as-received, after first round of spheroidization (called spheroidized-used), and after second round of spheroidization (called spheroidized-used2) are shown in Figure 6. First the used as-received powder was fed into the machine and the spheroidized-used powder was collected from both the main and cyclone bins. Then, the spheroidized-used powder collected from the main bin was fed into the machine for the second round of spheroidization. For the used powder, the sphericity of particles kept improving by re-spheroidizing the powder collected from the main bin; the order of powder sphericity from highest to lowest for used powder from the main bins is spheroidized-used2 > spheroidized-used > as-received, as shown in Figure 6a. It should be noted that the plots display the cumulative distribution of aspect ratio. During powder spheroidization the smaller particles evaporate due to the plasma high temperatures. By removing these small-size particles which are usually in irregular geometries, the remained powder is only composed of large-size particles which are usually spherical. When considering the particles’ aspect ratio in a cumulative manner, the removal of small-size particles plays an important role. Thus, the increase in sphericity of particles after re-spheroidization shown in Figure 6a is mainly due to the removal of small-size particles and not necessarily reshaping the particles. For the powders collected from the cyclone, the first round of spheroidization significantly improved the particles’ sphericity due to the evaporation of small-size particles with irregular geometries, as shown in Figure 6b. Although the second round of spheroidization caused partially better sphericity than the as-received condition, the second round of spheroidization resulted in worse sphericity than the first round of spheroidization. This can be explained by two facts. Firstly, it should be noted that the input powder for the second round of spheroidization was the used1-main; there is a possibility that if the second round of spheroidization was performed with the used1-cyclone, the results may have looked different. Since no data is available with that regard, no further discussion can be made. Secondly, the used2-c has fewer small-size particles than used1-m (the fed powder for the second round of spheroidization), thus, the first cumulative percentiles of the used2-c powder (until 70 percentile) shows higher sphericity than that of the as-received condition; however, after 70 percentile, the used2-c powder shows worse sphericity since after two cycles of evaporation, the used2-c powder has lost several particles and is left with only large particles with geometries less spherical than that of the as-received condition.
Reconditioned powder
The SEM images of reconditioned powder before and after spheroidization are shown in Figure 7. Reconditioned-main powder shows high sphericity while the sphericity of reconditioned-cyclone powder is perfect. The sphericity of reconditioned powder is compared in Figure 8 for powders collected from both main and cyclone bins. The reconditioned powders showed higher sphericity after the plasma spheroidization in both main and cyclone bins.
Spheroidized of all powders
To make a deeper comparison and discussion among the three types of powder, Figure 9 shows the spheroidized conditions of all powders in both main and cyclone bins. The baseline material, i.e., virgin powder in its as-received condition (AR-virgin) is also included in the plots to facilitate making an inclusive comparison. For powders collected from the main bin, the spheroidized-virgin powder resulted in the highest spherical particles. The first round of spheroidization on the used powder made the particles more spherical compared to the AR-virgin; in other words, the spheroidized-used powder showed higher sphericity than the AR-virgin. The second round of spheoidization (spheroidized-used2) improved powder sphericity compared to as-received-virgin while it shows comparable sphericity to that of spheroidized-used1. The spheroidized-reconditioned powder shows improvement in its sphericity. These changes in powder sphericity can be correlated with the change in powders’ oxygen content, as discussed in the next sections.
For the powders collected from the cyclone bin (see Figure 9b), the spheroidized-virgin powder showed slightly higher sphericity than the AR-virgin powder. The first round of spheroidization on the used powder improved the powder sphericity considerably while the second round of spheroidization deteriorated the powder sphericity to the same level of AR-virgin powder. The sphericity of reconditioned powder was improved to the similar sphericity of spheroidized-used1 powder, indicating that the hydrogen-treatment had no impact on the sphericity of particles collected from the cyclone bin. In other word, although the reconditioned powder had less oxygen content than the used powder, they both showed same sphericity after the spheroidization process.
Particle size distribution
As highlighted in the previous sections, one of the important factors in the powder spheroidization process is the powder evaporation which changes particle size distributions through vaporizing the fine particles. Thus, besides the particle sphericity, the particle size distribution should be studied. Following the same discussion layout for the powder sphericity, in the below sections first the particle size distribution of powders in their as-received conditions are compared followed by an individual discussion on each type of powder.
As-received of all powders
The comparison for all types of powder in their as-received conditions are shown in Figure 10. The virgin powder has more small-size particles than that of the used and reconditioned powders. As the reconditioned powder is the same used powder but with less oxygen, the used and reconditioned powders have similar particle size and are larger than the virgin powder; this is confirmed by a shift in particle size peak to larger values.
Virgin powder
Figure 11 shows the particle size distribution for virgin as-received powders collected from the main and cyclone bins. For the main chamber, not only the spheroidized powder has fewer small-size particles, but also several particles are enlarged to greater sizes (Figure 11a). This could be due to both evaporation and particle reshaping to spheres during the spheroidization process. For the cyclone bin, the particle size decreased considerably as can be seen in both Figure 11c and Figure 11d. The spheroidization machine operates in way that smaller size particles will be entrained and collected in the cyclone bin.
Used powder
The comparison for the used powder from the main and cyclone bins in three conditions of as-received, after the first round of spheroidization (called spheroidized-1), and after second round of spheroidization (called spheroidized-2) is shown in Figure 12. For the powders collected from the main bins, the spheroidized-1 powder has fewer small-size particles and a greater number of large-size particles. This suggests that the finer particles were evaporated and some of the large particles were melted and agglomerated with other particles to create even larger size particles during the spheroidization process. Second round of spheroidization increased the number of finer particles although it should have been reduced due to the second evaporation round of finer size particles. For the powders collected from the cyclone bin, the particle size of spheroidized-1 decreased while the particle size of spheroidized-2 increased; this can be caused by feeding spheroidized-1-main as input for the second round of spheroidization, confirmed by the similarity in particle size distribution of spheroidized-1 with spheroidized-2-cyclone as can be compared by looking at Figure 12a and Figure 12b.
Reconditioned powder
The impact of spheroidization process on powder particle size distribution of oxygen-reduced powder for both main and cyclone bins is shown in Figure 13. For powders collected from the main bin, spheroidized powder shows fewer small-size particles and the particles are reshaped to larger ones. For the powders collected from the cyclone bin, the particles reshape to smaller sizes, as shown in Figure 13b.
Spheroidized of all powders
For a comparison among all the spheroidized powders in terms of their particle size distributions, powders collected from both main and cyclone bins of all spheroidized powders were compared as shown in Figure 14. The virgin as-received powder is also included in all plots as a comparison baseline. For the powders collected from the main chamber, the virgin spheroidized powder shows fewer small-size particles compared with the virgin as-received powder. The same is true for the used1, used2, and reconditioned powders. The used2 powder shows a greater number of smaller particles than that of the used1. The reconditioned powder, however, shows even smaller sizes than those of both used1 and used2. For the powders collected from the cyclone (see Figure 14b), the spheroidized virgin is composed of more small-size particles than any other powder type. The first round of spheroidization has several small-size particles while the second round of spheroidization shifted particle size to greater values. The reconditioned powder has fewer small-size particles than that of the used1 powder.