Numerical Study and Experimental Validation of Copper Powder Plasma Spheroidization Process

doi:10.21203/rs.3.rs-3085172/v1

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Numerical Study and Experimental Validation of Copper Powder Plasma Spheroidization Process

https://doi.org/10.21203/rs.3.rs-3085172/v1

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As the extensive research in Additive Manufacturing (AM) shows, the powder characteristics, such as particle size and geometry, play an important role in determining the quality of powder layer and part fabricated with powder-based AM processes. It has been found that spherical particles result in better powder flowability and spreadability. An attempt to improve particle sphericity is to process the powder using the plasma spheroidization process, where the particles heat up, melt, and reshape to spheres. Several research works have been conducted to study the plasma spheroidization process and understand particle-plasma reactions. Although researchers have turned to simulations to overcome the difficulty of experimental study of such reactions, they only sufficed to characterize the powder particle size without evaluating the particle geometries. In this work, the plasma spheroidization process of copper powder was numerically examined to assess the impact of plasma spheroidization process on powder geometry and particle size. For the first time in literature, a method was proposed to quantify the particle geometry at each particle residence time. The results of simulation matched well with those of experiments.

Plasma Spheroidization

Copper

Powder

Simulation

Ansys Fluent: Additive Manufacturing

Additive Manufacturing (AM) has innovated the part production methods by facilitating the fabrication of high-complex part geometries in a layer-by-layer fashion [1, 2], which has enabled the fabrication of high-complex geometry components with high accuracy and desirable part properties [3–6]. Powder-based AM has been extensively investigated in the past decade to overcome its related challenges [7, 8]. Despite implementation of some techniques to modify the part’s quality, the characteristics of the spread powder layer may impact the quality of fabricated parts [9–12]. Moreover, the process temperature should be controlled to avoid creation of low-quality parts [13–15].

Powder characteristics, such as particle geometry, particle size and distribution, powder density. etc., determine the powder performance, like flowability and spreadability. These powder properties play a significant role in creating a dense powder layer during the spreading step of powder-based AM methods [16, 17]. It has been found that powders with spherical particles show improved powder properties suitable for AM purposes [18]. Thus, the AM feedstock powder is recommended to have spherical geometries.

There have been different common methods for producing spherical powders, including gas atomization, plasma atomization, plasma rotating electrode process, etc. [19], in addition to the newly developed techniques, such as the granulation–sintering–deoxygenation process and the chemical vapor synthesis. These processes may pose negative effects on powder characteristics (like low chemical purity), have a limited functionality only for a specific range of powder size, or be inefficient from an economic viewpoint. As summarized in a comprehensive review paper by Sehhat et al. [20], a novel method for creating spherical powder is plasma spheroidization [21, 22], which outperforms other methods by yielding a higher amount of spherical powder at a lower price and less chemical impurity. The plasma high temperatures melt powder particles and reshape them to spheres using the surface tensions as they are falling under gravity in the spheroidization machine’s reactor chamber [23]. Due to this process’s provided high temperatures, the plasma spheroidization can be deployed to melt and spheroidize most materials.

Copper is used for fabrication of parts requiring high electrical and thermal conductivity. Application of copper powder in the AM processes and its related difficulties have been investigated in the literature [24]. The copper’s high thermal conductivity provides high cooling rates which transfers the heat of melt pool to the powder bed. Since the thermal conductivity of the solidified material is different than that of the powder bed, thermal contours are created which consequently can cause part deformation due to the generated thermal stress. Creation of keyhole porosity defects is also reported due to the simultaneous impact of high cooling rate and easy flow of molten material [25–27].

Although there have been several studies on the simulation of powder plasma spheroidization process, none of these works examined the impact of spheroidization process on the particle geometry (sphericity). After all, as the process name indicates, the goal of using spheroidization process is to reshape the particles to spheres. Therefore, if the particle sphericity has not been assessed, the efficiency of the spheroidization process cannot be evaluated. In this work, we proposed a method for examining the particle geometry in terms of aspect ratio using the simulations; the change in particle diameter was measured and converted to particle size reduction, which then was used to investigate the particle geometry.

In this study, the impact of plasma spheroidization process on the morphology properties of copper powder, in terms of powder sphericity and particle size distribution, was numerically investigated. As we already published the experimental results of this work in [23], in this paper we validated the simulation results with those of experiments. The copper powder was numerically subjected to high-temperature plasma and the reaction of particles at each residence time was tracked by measuring the particle temperature and diameter. Using our proposed method, the change in particle diameter was used to calculate the particle aspect ratio.

The material characterized was gas-atomized copper powder with oxygen-free and high thermal conductivity (99.95% purity and < 10 PPM oxygen content) as purchased from the powder manufacturer. The powder particle size distribution was measured as D10:57 µm, D50:74 µm, and D90:97 µm. The experimental runs were performed using an Inductively Coupled Plasma (ICP) System, TekSphero-15, providing maximum 15 kW power and high temperature around 10,000 K. The powder morphology was investigated using an ASPEX Scanning Electron Microscope (SEM). A particle size analyzer (Microtrac S3500) was used to measure the powder particle size based on laser diffraction method.

TekSphero-15 is an ICP machine that spheroidizes input powder, improves the powder’s flowability, removes chemical impurities, and reduces particle porosity [28, 29]. A major goal of spheroidization process is to reduce variations in powder properties and thus ultimately reduce uncertainty in the mechanical performance of manufactured parts. In the plasma spheroidization process the powder is injected into a high-temperature plasma under an inert atmosphere (cryogenic argon), to be melted for enhancing particle sphericity [30]. The temperature of plasma is in the range of 3,000–10,000 K. Depending on the particle size, material melting point, residence time of powder particles in plasma, and spheroidization process parameters, the powder particles could be melted and/or evaporated [31]. After powder particles are melted, they fall under gravity inside the plasma chamber, where they are quenched at the high cooling rates of ~ 10⁶ K/s [32]. The surface tensions will alter the powder particle geometries to spheres.

As shown in Fig. 1, the equipment has three collection bins of main chamber, cyclone bin, and nanofilter, with decreasing order for size of the collected powder from each bin. The main process parameters are flow rates of carrier gas and central gas, and the chamber pressure. Carrier gas carries the powder particles from the injector at the torch’s center through the plasma field and towards the reaction chamber and collection bin [33]. The decrease in carrier gas has been found to increase powder spheroidization. Central gas is the main plasma gas that determines the amount of generated plasma [34]. Chamber pressure affects the particles residence time and works in correlation with central gas flow rate to change plasma velocity distribution. A higher central gas flow rate and a lower chamber pressure resulted in a higher-velocity plasma, which provided less residence time for the powder particles to melt and spheroidize [20].

Following the function of each spheroidization process parameter and considering the properties of copper powder, the levels for spheroidization process parameters should be appropriately selected to both reshape particles to spheres as best as possible and yield powder mass as highest as possible. Based on the findings of previous spheoidization studies and as recommended by the machine’s manufacturer, the experiments were performed with carrier gas 3 lpm, central gas 10 lpm, and chamber pressure 15 psi.

After running the experiments, the powders were collected from the main collection bin. Then, the particles were deposited on a carbon tape to prepare SEM samples. Ten SEM images per each sample were then taken to analyze the particle shapes, collecting data of at least 500 particles per sample. The SEM images were analyzed in MIPAR image analysis software. The change in powder shape was quantified using the well-known metric of “aspect ratio”, which is defined as the ratio of the major axis to the minor axis of the bounding ellipse for a particle. Through this definition, the particle sphericity increases as the aspect ratio approaches unity. The experimental aspect ratio is reported in terms of cumulative percentage of powder particles; for example, AR₅₀ = x indicates that the 50% of particles of powder sample have aspect ratios smaller than or equal to x.

4.1. Computational Technique and Boundary Conditions

The governing equations for performing the simulations were defined in terms of the transport of mass, momentum, and energy:

Conservation of mass

$$\nabla .\left(\rho u\right)=0$$

Conservation of momentum

$\nabla .\left(\rho uu\right)=-\nabla p$ +$\nabla$.[µ($\nabla u$+$\nabla {u}^{T}$)-$\frac{2}{3}\mu \nabla .\left(uI\right)$]+ $\rho$g + $\text{J}\times \text{B}$(2)

Conservation of energy

$$\nabla .\left(\rho uh\right)=\nabla .\left(\frac{k}{{c}_{p}}\nabla \text{h}\right)+\text{J}\times \text{E}-\text{R}$$

where ρ is the density of plasma, p is the pressure, h is the enthalpy, T is the temperature, u is the velocity, k is the thermal conductivity, ${c}_{p}$ is the specific heat at constant pressure, µ is the viscosity, g is the gravitational force, E is the electric field, B is the magnetic induction, J is the current density induced in the plasma, and R is the volumetric radiative loss. The following assumptions were made: the flow was considered to be steady and laminar; the plasma was considered optically thin and in the commonly used conditions of local thermodynamic equilibrium (LTE); the energy impact of viscous dissipation term was ignored; and the displacement currents were neglected.

The simulation was performed in Ansys Fluent. The dense discrete phase model with argon gas as the primary phase and the inert copper particle as the secondary phase was deployed. The physical characteristics of argon gas are provided in the Fluent’s material database. The copper powder density was defined as 8978 kg/m³ with specific heat of 381 J/kg.K. The copper powder particle size distribution was defined as rosin-rambler with the same size range as measured using SEM, and the initial velocity of particles were set the same as the carrier gas flow rate. The energy equation was implemented to incorporate the effect of heat on particle temperature histories. The standard κ-ε turbulent model was used and PISO pressure-velocity coupling algorithm was set with a pressure relaxation factor of 0.3 and a speed relaxation factor of 0.7. The continuous-phase flow field was calculated by setting velocity-inlet and pressure-outlet boundary conditions; no-slip wall was set to the solid boundary by default. Provided by the experiment’s information, to create a stable plasma, the gas flow rates were set as 3 lpm, 10 lpm, and 50 lpm, for carrier, central, and sheath gases, respectively. To collect the particles in the collection bin when they touch its boundary, the bottom of collection bin was set as trap boundary.

4.2. Numerical Measurement of Particle Aspect Ratio

Although several research works in literature have been conducted on the simulation of powder plasma spheroidization process, none of the studies have evaluated the impact of plasma on particle geometries. Researchers have considered the initial particle geometries as spherical and only compared the particle size distribution. In this work, a method has been proposed to approximately determine the particle geometry (sphericity in terms of aspect ratio) at each residence time for a specific particle size (three size representatives of D10:57 µm, D50:74 µm, and D90:97 µm). First, the change in particle diameter at each residence time was tracked, then this diameter change was used to evaluate the particle geometry by following the same experimental image analysis method as described in section 3. To visually illustrate the process of geometry evolution for a particle, a simple square particle geometry was investigated as shown in Fig. 2, where the particle geometry was colored by the liquid and vapor fraction of particle at different subsequent residence times (t1 < t6). Time t1 shows the initial square geometry as created in the simulation, where the entire particle was composed of liquid with no vapor fraction. This should be noted that although the particle core is solid, it is still depicted as liquid due to the software limitations. As the particle residence time increases to t2, particle temperature goes beyond the melting point, and the particle starts melting and reshaping to spheres while there is still no evaporation. This procedure lasts for more particle reshaping (residence time t3). Keeping exposed to heating temperature for longer residence time of t4, the particle temperature increases beyond boiling point, where material melting, reshaping, and evaporation take place. This melting and evaporation last (t5) until the particle leaves the plasma heating zone (t6), after which the particle geometry remains unchanged. The particle aspect ratio was measured by considering the geometry of particle liquid fraction at each residence time. Following the same procedure, according to the as-received powder SEM images, the initial particle geometry was drawn in the simulation. Then, the aspect ratio of particle geometry was measured at each residence time. To evaluate the results reproducibility, this procedure was replicated for 10 particle samples per each size representative and their mean and standard deviations were reported, as discussed in section 5.2.

5.1. Particle Temperature and Size Reduction

To assess the particle heating and consuquent size reduction, three particle sizes of D10:57 µm, D50:74 µm, and D90:97 µm were tracked. As shown in Figure 3, due to exposure to high temperature plasma, the particle temperatures increase to reach the melting point, where the tempereture remains constant since the heating is spent on the latent heat of fusion. Particles heat up beyond this point to reach the boiling point, where the particle size strats shrinking. This shrinking continues as long as the particle is in the heating zone. Once the particle leaves the heating zone, the particle size remains constant while the particle starts cooling down (particle temperature is less than the boiling point). Figure 3(a) compares the temperature history for the three particle representatives; due to its smaller diameter, the 57 µm particle was heated up to the melting and boiling points faster, followed by 74 and 97 µm particles. Likewise, the 57 µm particle showed a faster cool-down.

The particle shrinkage was measured by tracking the particle diameter. As shown in Figure 3(b), once the 57 µm particle reached the boiling point (15.6 ms), its diameter started decreasing until the particle left the heating zone (30 ms), with around 16% diameter reduction. The 74 and 97 µm particles showed a similar pattern and started shrinking at 18 and 25 ms, with 6.8% and 0.62% diameter reduction, respectively (Figure 3(c) and (d)). These diameter reductions were used to characterize the particle geometry, results of which are discussed in the next section.

5.2. Particle Aspect Ratio

Figure 4 shows the particle aspect ratio per diameter reduction that the particle with specific size, i.e., 57, 74, and 97 µm, experienced. As mentioned earlier, per diameter reduction, the shown values of aspect ratio were the mean aspect ratio of 10 randomly selected particles with the specific size; thus, the appearance of horizontal error bars is attributed to the standard deviation of aspect ratio measurements of 10 different particles. For the 57 µm particle, as shown in Figure 4(a), the 16% diameter reduction improved the particle sphericity by decreasing the aspect ratio from 1.023 (initial particle geometry) to 1.008 (spheroidized particle geometry). The 6.8% diameter reduction for 74 µm particle reduced the aspect ratio from 1.024 to 1.013 (Figure 4(b)). The diameter of 97 µm particle reduced by 0.62%, resulting in improvement of aspect ratio from 1.025 to 1.018. Comparing these values across different particle sizes, it can be observed that for larger particles, the particle evaporation results in improving particle geometry (mostly by reshaping the particle outer surface) while for smaller particles, the particle evaporation results in decreasing particle size.

The proposed method of particle geometry evaluation resulted in generating the graphs shown in Figure 4, which can be used for predicting the particle aspect ratios; one may use the particle residence time to find the corresponding diameter reduction, based on which the particle aspect ratio can be determined. The proposed method was capable of evaluating the particle geometry for the first time in literature as no other research work has investigated it.

Thus far, to simplify the explanation of measurement procedure, the evaluation of particle geometry was limited to three sizes of 57, 74, and 97 µm. Following the same procedure, the aspect ratio of simulated particles was measured for the rest sizes in the particle size range of as-received powder (for the size range, look at the horizontal axis of charts in Figure 6). By incorporating the aspect ratio results from experiments [23] into the results of simulations, Figure 5 compares the aspect ratio of spheroidized powder, processed with experiments and simulation; the aspect ratio of as-received powder has also been included as a reference. Firstly, it can be observed that the results from both experiments and simulation show great improvement in the sphericity of particles compared to their as-received condition. Most importantly, the simulation results matched well with the experiments. These findings suggest that the proposed method for quantifying the particle geometry has contributed to predicting the particle sphericity without performing experiments. In addition, future researchers can use this proposed technique as a basis for advancing the particle geometry quantification.

5.3. Particle Size Distribution

The particle size distribution of spheroidized powder collected from the collection bin was measured both experimentally and numerically, results of which are shown in Figure 6. The particle size distribution of as-received powder was also shown in Figure 6(a) as a reference. As can be seen, the percentage of smaller particles were reduced after the spheroidization process due to the material melting and evaporation. The particle size distribution of spheroidized powder out of simulation was shown in Figure 6(c). By comparing the results of experiments and simulation, it can be observed that the particle size distribution of simulation matched well with that of experiments for medium and larger sizes. The size distribution of simulation differs from the experiments only for very small particles, which could be due to the simplifying assumptions in the simulation software.

The plasma spheroidization process of copper powder was simulated using Ansys Fluent software. A method for tracking the particle geometry was proposed for the first time in the literature. Based on tracking the particle diameter per residence time during the spheroidization process, the change in particle diameter was calculated. This particle diameter reduction was then used to measure the particle aspect ratio. In addition to quantifying particle geometry, the particle size distribution was also examined. The spheroidized powder, as observed experimentally and numerically, had less amount of smaller particles than that of as-received powder, which was due to the material melting and evaporation during the spheroidization process.

a. Funding

This work was funded by ISAM Lab at Missouri University of Science and Technology, Rolla, MO, United States.

b. Conflicts of interest/Competing interests

The authors declare that they have no conflict of interest.

c. Author Contributions

Conceptualization: M. Hossein Sehhat, Ming C. Leu.

Data curation: M. Hossein Sehhat.

Investigation: M. Hossein Sehhat.

Formal analysis: M. Hossein Sehhat.

Funding acquisition: Ming C. Leu.

Writing – original draft: M. Hossein Sehhat.

Writing – review & editing: M. Hossein Sehhat, Ming C. Leu.

d. Availability of data and material

The raw/processed data required to reproduce these findings will be made available on request.

e. Code availability

The raw/processed data required to reproduce these findings will be made available on request.

Compliance with ethical standards

f. Ethics approval

The manuscript contains original ideas which have never been published before in other journals.

g. Consent to participate

This study is not a human transplantation study. No consent needed for this paper.

h. Consent for publication

The authors declare their consent for publication.

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Numerical Study and Experimental Validation of Copper Powder Plasma Spheroidization Process

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Abstract

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1. Introduction

2. Material and Methods

3. Experimental Procedure

4. Simulation Procedure

4.1. Computational Technique and Boundary Conditions

4.2. Numerical Measurement of Particle Aspect Ratio

5. Results and Discussion

6. Conclusion

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