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PII: S0032-5910(18)30867-2
DOI: doi:10.1016/j.powtec.2018.10.023
Reference: PTEC 13797
To appear in: Powder Technology
Received date: 22 May 2018
Revised date: 7 October 2018
Accepted date: 13 October 2018
Please cite this article as: Blake Fullenwider, Parnian Kiani, Julie M. Schoenung, Kaka
Ma , Two-stage ball milling of recycled machining chips to create an alternative feedstock
powder for metal additive manufacturing. Ptec (2018), doi:10.1016/j.powtec.2018.10.023
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Two-stage ball milling of recycled machining chips to create an alternative feedstock powder for
metal additive manufacturing
Blake Fullenwidera, Parnian Kianib, Julie M. Schoenungb, Kaka Maa,*
a
Department of Mechanical Engineering, Colorado State University, Fort Collins, CO 80523
b
Department of Chemical Engineering and Materials Science, University of California, Irvine,
California, 92697
* Corresponding author: Email: Kaka.Ma@colostate.edu Tel: (970) 491-3886
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Abstract
To explore alternative and sustainable feedstock production for metal additive manufacturing,
stainless steel powders were fabricated from recycled machining chips by ball milling. To achieve the
desirable powder characteristics for additive manufacturing, the effect of ball size on the powder
morphology change and particle size reduction was investigated through both theoretical analysis on the
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maximum deformation depth in the powder during ball milling and extensive experimental work. The
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modeling results suggest that large balls (diameter = 20 mm) efficiently break up machining chips to
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coarse powder particles while small balls (diameter = 6 mm) effectively modify the powder morphology
to near-spherical. Therefore, a two-stage ball milling approach, i.e., using large balls at the initial stage
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of milling followed by a second stage of milling with small balls, was proposed in experiments and
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successfully converted machining chips to powders with near-spherical shape and particle sizes ranged
from 38 to 150 microns. In addition, the nanoindentation hardness of the ball milled powder created
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from machining chips is 56% higher than the gas atomized powder. To verify the usability of the ball
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milled powder created from recycled machining chips in additive manufacturing, single tracks have been
Keywords
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Metal additive manufacturing; stainless steel; sustainability; ball milling; plastic deformation
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1. Introduction
Metal additive manufacturing (AM) has attracted increasing research interest because of its
capability to create near-net-shape parts in one step with computer aided design, which reduces the need
for subsequent machining and the use of hazardous cutting fluids [1]. Thus, metal AM is regarded as a
more sustainable process than the conventional processing such as casting [1–3]. Gas-atomized (GA)
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powder is the most common feedstock for AM attributed to its spherical morphology, and controllable
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particle size distribution. However, production of GA powders consumes large amounts of energy and
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inert gas [4]. Water atomized powder is also used when faster powder solidification rates and decreased
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production costs are desired [5–7]. Compared to GA, this technique produces powders with smaller
particle sizes, a wider particle size distribution and relatively irregular shape. Comparable mechanical
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properties were obtained when water atomized powder was used as feedstock in AM, suggesting that
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irregular (i.e., non-spherical) morphology is adoptable in metal AM [5,7]. However, production of gas
atomized powder or water atomized powder requires the melting of the metal prior to ejection from the
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atomization nozzles, which requires significant energy to account for the enthalpy difference between
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the liquid and solid states [8]. Typically, the feedstock powder is melted again in metal AM. This double
melting represents a significant waste of energy and cost. To overcome these challenges,
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additive manufacturing. Therefore, the present work aimed to produce powders from recycled
machining chips and to investigate the feasibility of using the powders created from machining chips in
additive manufacturing.
Mechanical milling presents a potential opportunity for sustainable powder production because it
can break down a variety of starting materials with different initial sizes into powder particles [9–11].
Mechanical milling is often conducted at room temperature or at cryogenic temperature [12–14]. Thus,
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the need for the aforementioned high energy consumption to achieve atomization temperatures is
eliminated [15]. In addition, the solid solubility of a metal element A in another metal B can be
increased to exceed the equilibrium limits [12,14]. Thereby, alloys otherwise unachievable by
atomization can be created by mechanical milling. Given the potential advantages, mechanical milling
was implemented in the present work to convert recycled metal machining chips to powders that are
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suitable for AM. The primary criteria to judge whether the powder is suitable for metal AM include
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acceptable morphology, chemical composition, and controllable particle size distribution [16–18].
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During ball milling, a typical mechanical milling process, the particle size refinement and morphology
evolution in the powders are predominantly determined by the impact forces between the balls and the
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powder particles. A lot of studies in the literature reported ball milling of gas atomized powder lead to
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powder shape change, grain refinement, phase change, and formation of composite powders. To name a
few here, Shashanka and Chaira reported that rock-like or flakey powders were formed when stainless
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steel powder were mechanically milled [19]. Another study showed that wet milling of titanium granules
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produced powders with flat and flakey morphology, which were subsequently sintered to form spherical
morphology for AM [20]. Yang et al. showed that spherical particle morphology was retained when gas
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atomized 316L stainless steel powder and TiB2 powder were mixed and ball milled for 8 hours. They
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also found that the morphology of water atomized 316L powder changed from irregular to a mixture of
flake-like and spherical when the powder was ball milled with Ti powder and C powder for 35 hours
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[21,22]. Both powders were successfully consolidated using selective laser melting. These two studies
demonstrated that ball milled powder generated from atomized powder can be applied as feedstock for
metal AM [21,22]. However, very limited studies investigated ball milling of machining chips. Enayati
et al. reported austenitic stainless steel chips transformed to powder with a primary martensitic structure
with a composition similar to 304L stainless steel [9]. Zhang et al. produced Al–Si–Mg alloy granules
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by mechanical crushing of machining chips [23]. The granules were subsequently ball milled to form
powders. Their study was focused on the microstructural change of eutectic Si particles inside the
powder rather than the morphology evolution of the whole powder particles [23]. Two additional studies
showed flattened powders were fabricated from cast iron chips by ball milling [10,24]. Nevertheless,
none of these studies reported the use of the powder generated from ball milling of machining chips in
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metal AM. Pinkerton et al. used machining chips directly as the feedstock material in metal AM to
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deposit thin walls [25–27]. The chips were sieved and only those with sizes below 425 μm were used in
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their study. They found surface oxides on the chips led to an increased corrosion rate in the final part
[25]. Review of the existing literature suggests that (1) a thorough understanding of the relationship
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between powder morphology change and the ball milling process parameters, especially the ball size, is
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not achieved yet; (2) use of the ball milled powder made from machining chips in metal AM is not
investigated yet.
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To fill the aforementioned gaps in this research area, the objectives of the present study include:
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(1) perform theoretical analysis of the impact force on a powder particle and the consequent maximum
deformation depth in the powder during ball milling to reveal the effect of ball size on powder
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morphology evolution, (2) use the theoretical analysis in conjunction with experimental work to convert
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metal machining chips to powders useful for metal AM, and (3) verify that the powder created from ball
milling of machining chips can be used as feedstock in metal AM. To achieve those goals, a novel two-
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stage ball milling strategy was proposed and applied. The ball milled powders created from the
machining chips were characterized in terms of morphology, particle size, and microstructure. To verify
the feasibility of using these ball milled powders in AM, single tracks were successfully deposited using
laser engineered net shaping (LENS®) and compared to single tracks that were deposited from GA
304L stainless steel was selected as the model material due to its wide use in AM for various
structural applications [28]. 304L stainless steel is desirable for metal AM because of its high strength,
high weldability, and corrosion resistance [29]. The starting material used in the present study was
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stainless steel 304L machining swarf provided by AK Steel (West Chester Township, Butler County,
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Ohio). The chemical composition of the swarf is provided in Table 1. The individual chips had
serrations along the length (5-20 mm) due to the previous machining operation, as shown in Fig. 1. Steel
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swarf was cleaned with ethanol to reduce contamination from the machining process. The machining
chips were then milled using a PQ-N04 planetary ball mill (Across International, Livingston, NJ) in
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cylindrical stainless-steel jars of 52 mm inner diameter. The center of the jars is 85 mm from the center
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of the main plate. Stainless steel balls of 20 mm diameter and 6 mm diameter, denoted as Φ-20 balls and
Φ-6 balls in the following sections, were used as the milling media with a consistent 15:1 ball-to-powder
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weight ratio. Approximately 50-60% of the jar volume was filled with the milling media. The maximum
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rotation speed achievable by the equipment, 500 rpm, was used to achieve a highest energy transfer rate
for the same ball-to-powder mass ratio. Five minutes on/five minutes off cycles were applied to prohibit
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over-heating of the milling media. To reduce surface oxidation, an argon environment inside the jars
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was maintained by sealing the jars inside a glovebox with less than 1 ppm oxygen content. Both milling
time and ball diameter were varied, in an effort to investigate the effect of the ball milling conditions on
the powder morphology evolution during milling. Four ball milling conditions were studied: BM-20-
ball milled powder, the second digit (6 or 20) refers to the diameter of the balls (2Stg stands for a two-
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stage milling process that uses Φ-20 balls initially, followed by milling with Φ-6 balls); “Int” denotes an
interrupted operation, and the final digit in the ID is the total milling time length. The interrupted two-
stage milling means the ball milling process was stopped at 12-hour intervals to collect powder samples
to investigate the morphology evolution. All powders were sieved for 15 minutes using a Ro-tap RX-29
sieve shaker (W.S. Tyler, Mentor, Ohio) and four standard testing sieves with mesh sizes of #400, # 200,
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#140 and #100, corresponding to 38 μm, 75 μm, 106 μm, and 150 μm, respectively. The powder with a
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particle size below 150 μm was used to study the morphology evolution, while the powder coarser than
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150 μm was further milled with a consistent ball-to-powder weight ratio.
To investigate the feasibility of using the ball milled powder in metal AM and to study the
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interaction between the laser and ball milled powder, single tracks were deposited in a LENS ®
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deposition system (Optomec® 750) using the ball milled powder created from machining chips as the
feedstock powder. Instead of injecting the powders through the nozzles, a powder bed was created on
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the substrate by spreading powder between two 150-μm-thick spacers with a straight edge. For
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comparison purposes, single tracks were also deposited using 304L GA powder using the same LENS®
deposition conditions (scanning speed and laser power). 304L GA powder was obtained from Carpenter
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Powder Products (682 Mayer Street, Bridgeville, Pennsylvania) with a particle size between 38-150 μm.
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These single tracks were characterized in terms of their continuity and width by optical microscopy.
Table 3 provides a summary of sample IDs for these single tracks and the corresponding processing
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conditions.
Particle size distribution of the milled powder was analyzed via sieving, as described in Section
2.1. The masses of the powder particles in different particle size ranges were weighed. Particles in the
size range between 38 and 150 μm are of particular interest for LENS® [28]. The ball milled powder
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was characterized in a JEOL 6500 FE scanning electron microscope (SEM) with an acceleration voltage
of 15 kV. The particle morphology was quantified using aspect ratios (the longest line that travels
through the center of a particle divided by the shortest). SEM images of one hundred particles from each
test were analyzed to calculate the average aspect ratio, as well as the 30th, 50th, and 80th percentile
(denoted as D30, D50, and D80, respectively) of aspect ratio. The powders were mounted in epoxy and
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polished to a final polishing step of 0.25 μm diamond suspension. The cross-section microstructure of
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the powders was characterized via SEM. Nanoindentation has emerged as a novel characterization
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method to study local mechanical properties of materials at a nanoscale, as well as to study the
mechanical properties of powders [30]. In the current study, nanoindentation tests were performed on
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the cross-sections of the as-received chips, 304L GA powder, and BM-2Stg-60hr powder samples to
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study the hardness of the powders using a Hysitron TI Primer with a Berkovich diamond probe. A
maximum load of 1 mN was used with a 10s-15s-10s loading time-hold time-unloading time profile. Six
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indents per particle were performed on ten individual particles for each sample. The indentation depth
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ranged from 70 nm to 100 nm, and the length of one side measured after indentation did not exceed 1
μm. The indents were spaced 5 μm apart to avoid the stress fields caused by previous indents. The
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Berkovich diamond indenter area function was calibrated using a standard fused quartz sample. The
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3. Theoretical analysis
The morphology evolution from chips to powders significantly depends on the impact forces
between the chips/powders and the milling balls [5,31–34]. The force per impact that a ball exerts on a
particle can be quantified using both the milling parameters and the planetary mill dimensions (Fig. 2).
The maximum force per collision between milling media results in stresses on the powder, which
subsequently lead to plastic deformation of the powder particles and alter the morphology and particle
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size of the chips or powders that are ball milled. While the ball to powder weight ratio determines the
overall energy that transfers from the milling balls to the particles, ball diameter is a critical milling
parameter that influences the force per impact, the stress per impact, and the impact frequency. Previous
studies have reported various morphologies (e.g., flakey or rock-like) and particle sizes for ball milled
powders when the ball milling parameters are varied [9,10,12,19,35]. However, few studies have
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performed quantitative analysis on how the selection of ball diameter affects the ultimate shape and
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particle size of the powder. In an effort to select appropriate ball milling parameters to create near-
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spherical particles with particle sizes of 38-150 µm, the desirable powder characteristics for metal AM,
Gusev’s model and Hertz’s model [36,37] are combined in the current study to evaluate the impact force
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and stress on the particle, as well as the resultant maximum deformation depth into the particle, when
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two different types of balls are used as the milling media: Φ-20 balls and Φ-6 balls.
Gusev et al. developed a model to estimate the maximum force per collision in a planetary ball
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where 𝑚 is the mass of the ball, 𝑎 is the acceleration rate, 𝑡 is time, 𝑥 and 𝑦 define the position
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relative to the center axis of the mill, 𝜔 is the angular speed of rotation, 𝑅 is the radius of the
main disk, and 𝑅 is the internal radius of the jar. According to Gusev’s model, the impact force
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increases as the ball approaches the furthest distance from the center axis. The maximum force per
impact from Φ-20 balls is 33 times greater than that from Φ-6 balls, as shown in Fig. 3.
Another model developed by Hertz defined that a simplified von Mises stress, 𝜎 , was dependent
on the pressure at a lateral distance (X) from the center, 𝑃(𝑋), and the distance from the impact into the
particle (Z), and the impact area (𝐴), as shown in Equations (2-4) [37] :
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𝜎 = |𝜎 − 𝜎 | (2)
( )
𝜎 = (4)
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Where 𝑃(𝑋) = 𝑃 √1 − ,𝑃 is the maximum pressure per impact between two spheres as a
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( )
function of force and impact area (𝐴): 𝑃 = . The impact area (𝐴) is a function of the impact
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force and material properties, as given in Eq (5) below [37]:
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( ) ( )
⁄ ( ⁄ )
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( )( )
𝐴= (5)
√
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where 𝜈 is the Poisson’s ratio, 𝐸 is the elastic modulus, and 𝐷 and 𝐷 are the diameters of the
To study the influence of various ball diameters on particle morphology evolution, the
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maximum deformation depth per impact is determined by applying the milling parameters outlined in
the experimental procedure to identify the Z depth at which the von Mises stress, 𝜎 , is equal to the
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yield strength of 304L (210 MPa [38]). Only the direct collision between a ball and a particle is
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considered in the model, as the stress resulting from the self-rotation of the balls and the powder
particles is negligible when compared to the direct impact stress. The modeling results suggest that the
maximum deformation depth per impact from Φ-6 balls, Φ-10 balls, and Φ-20 balls, is approximately 13
μm, 28 μm, and 81 μm, respectively. This maximum deformation depth increases as the difference
between feedstock particle size and ball size increases. When the maximum deformation depth is
normalized by the particle diameter near the ideal particle size range for LENS® (38-150 μm), the
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dependency of ball diameter on final particle morphology is demonstrated in Fig. 4. For example, the
20 ball is approximately 81% of the particle diameter; while that caused by the impact from a Φ-10 ball
and from a Φ-6 ball is 28% and 13% of the particle diameter, respectively. This reduction in normalized
maximum deformation depth indicates using Φ-6 balls is favorable in forming spherical morphology in
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the powders with particle sizes ranging from 38 μm to 150 μm, as a large deformation depth, particularly
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when it exceeds 50% of the particle diameter, tends to produce flakey or flattened particles. These
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modeling results suggested that large balls (Φ-20) should be chosen for breaking up machining chips to
coarse powder particles first and then small balls (Φ-6) should be used for powder morphology
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modification. This speculation based on the modeling is verified by experimental results provided in the
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next section. The modeling results based on the equations provided guidance on the selection of ball size
4. Results
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The morphology of the powder particles collected between sieves 100-140 mesh (nominally
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particle size 106-150 μm) is shown in Fig. 5. The aspect ratios are summarized in Table 4 to quantify the
circularity of the powder. The closer the aspect ratio is to 1, the more spherical the powder is. GA
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powder is generally described as spherical powder with a smooth surface, compared to water atomized
powder that exhibits relatively irregular morphology. BM-2Stg-60hr powder particles exhibited rounded
features and smoother surfaces than the powder particles created from single stage milling (Fig. 5a-b).
1% (number percentage) of the particles imaged from BM-2Stg-60hr were classified as flattened, while
the average aspect ratio was found to be 1.37. In contrast, the microstructure of BM-20-60hr (Fig. 5c-d)
showed that 38% (number percentage) of the particles were flattened. Near-spherical agglomerates with
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rough surfaces are observed in BM-6-60hr (Fig. 5e-f). BM-2Stg-60hr powder exhibited a coarser surface
than both GA and water atomized powders [5,6]. However, this powder has a higher volume fraction of
particles with near-spherical morphology than water atomized powder. As discussed in the Introduction,
the successful application of water atomized powder as a feedstock for metal AM suggests it is feasible
to use non-spherical powders, such as the ball milled powder generated from machining chips in the
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present work.
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The morphology evolution of BM-2Stg-Int-24hr, BM-2Stg-Int-36hr, BM-2Stg-Int-48hr, and
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BM-2Stg-Int-60hr powders is quantified in Table 4. Both the aspect ratio and the number percentage of
flattened particles in BM-2Stg-Int powder decreased with increasing milling time. The morphology of
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the feedstock (BM-2Stg-Int-24hr) for stage two can be described as flattened rock-like particles ranging
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from 100-700 μm in size (Fig. 6a). BM-2Stg-Int-36hr powder started to exhibit particles with rounded
features and smoother surfaces (Fig. 6b); but 92% of the particles remained flattened. BM-2Stg-Int-48hr
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powder started to exhibit spherical features such as increased thickness while maintaining the rounded
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features and smooth surfaces found in BM-2Stg-Int-36hr (Fig. 6c). However, 16% of the particles were
still flattened. BM-2Stg-Int-60hr particles exhibited near-spherical features and smooth surfaces when
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compared to single stage milling (Fig. 6d) while only 2% of the particles remained flattened. Both the
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aspect ratio, and the number percentage of flattened particles in the interrupted tests show a decreasing
trend with increased milling time. The near spherical shape combined with the smooth surface features
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found in the BM-2Stg-60hr powder indicate a more ideal particle morphology for metal AM is achieved
when using a two-stage milling approach, as opposed to the single stage milling approaches of BM-20-
60hr or BM-6-60hr.
The particle size distributions for the various milled powders are provided in Fig. 7. The yield of
the powder with particle sizes of 38 to 150 μm for BM-2Stg-Int-36hr, BM-2Stg-Int-48hr, and BM-2Stg-
Int-60hr was approximately 21 wt.%, 37 wt.%, and 53 wt.% of the initial input, respectively. Increasing
milling time with the Φ-6 balls increases the number fraction of powder particles with sizes between 38
and 150 μm. For the two-stage ball milling without interruption (BM-2Stg-60hr), the yield of powder
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with a particle size range from 38 μm to 150 μm is 69 wt.%. In contrast, BM-20-60hr and BM-6-60hr
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only yielded 2 wt.% and 3 wt.% of powder with a particle size of 38-150 μm, respectively. These results
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indicate that the two-stage milling process is more effective in reducing the particle size to below 150
μm than either single stage process for an equivalent total milling time (60 hr).
2Stg-60hr powder are shown in Fig. 8. Both austenite and martensite are identified from the peaks for
the as machined 304L steel swarf. The intensity of the austenite peaks was much greater than that of
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martensite. In BM-2Stg-60hr powder, the peaks corresponding to martensite were more intense than the
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austenite peaks. Plastic deformation induced phase transformation from metastable austenite to
martensite has been observed in fatigued [39–41] and ball milled 304L steel [9]. 304L steels that were
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processed by forging and rolling at room temperature also consisted of dominant metastable austenite
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with some martensite [42]. As a bulk part is machined, the 304L steel chips experience plastic
deformation, leading to an increase in the volume fraction of martensite. Severe plastic deformation
during ball milling also induces the austenite to martensite phase transformation.
The nanoindentation hardness values of the three materials, machining swarf, GA powder, and
the ball milled powder (BM-2Stg-60hr), are illustrated in Fig. 9. The GA powder exhibited an average
hardness of 5.9±0.4 GPa, while the machined chips exhibited an average hardness of 6.4±0.4 GPa. This
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previously. The two-stage milled powder exhibited an average hardness of 9.2±0.7 GPa, which is 56%
Representative optical images of the single tracks made from GA and BM-2Stg-60hr powder are
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shown in Fig. 10. All single tracks exhibit continuity with evidence of sufficient penetration into the
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substrate. Both ST-BM-410-1.7 and ST-BM-360-1.7 exhibit a uniform melt pool, including a circular
melt pool geometry, and uniform spacing between cooling lines, similar to the characteristics observed
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in ST-GA. Melt pool geometry and the continuity of the single tracks are of particular interest in
characterization as they are influenced by deposition parameters and determine the properties of the final
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parts [43–46]. The average width of ST-BM-410-1.7 and ST-BM-360-1.7 are 809±24 μm and 718±20
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μm, respectively. The average values were calculated based on 150 measurements for each single track.
In comparison, the average width of ST-GA-410-1.7 and ST-GA-360-1.7 are 780±24 μm and 698±19
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μm, respectively. Increasing laser power from 360 W to 410 W led to this slight increase in the width of
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the single track as the size of the melt pool is larger with increased energy input. Minimal difference in
the amount of splatter on the surface of the substrate is observed between ST-BM and ST-GA.
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5 Discussion
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current research, powder particle morphology is considered one of the most critical characteristics of the
feedstock material [5]. The modeling work described above provides useful insight into the effect of the
milling ball diameter on the plastic deformation in a powder particle in the planetary ball mill. Both
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modeling and experimental results suggest that a high frequency of low-force impacts on individual
struck from multiple random directions with low force impacts, it tends to form a spherical morphology.
This is evidenced quantitatively by the decrease in aspect ratio and qualitatively by the increase in
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In contrast, particle size refinement is achieved by impacts with high forces, as suggested in both
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the modeling results and the experimental observation. Particle size refinement occurs when a particle is
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cleaved into parts. This happens as a particle is either split by one large impact, or by the accumulation
of multiple impacts that propagate a crack through the particle. Nonetheless, high-force impacts can also
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be detrimental to particle size refinement when cold welding occurs, where the collision of multiple
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particles at the same time weld them together into a coarse particle or agglomerates. To efficiently
reduce the particle size, the modeling result reveals that the impact stresses need to be sufficiently high
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to propagate cracks through a particle while not exceeding the critical value leading to cold welding.
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The experimental results agree well with the modeling in terms of both particle size refinement and
morphology evolution.
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If the ball-to-powder weight ratio is maintained, changing the ball diameter not only affects the
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force per impact but also the frequency of the impacts. With a consistent ball-to-powder weight ratio,
when the ball diameter is increased to two times that of the previous value (e.g., from 6 mm to 12 mm),
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the impact frequency is decreased to 1/8 that of the previous value, while the force per impact is
increased to eight times that of the previous value. In addition, each impact results in an increase of the
maximum deformation depth to approximately three times that of the previous value. In order to refine
304L steel swarf with a length scale of millimeters to powders with a scale of 38-150 μm, using Φ-20
balls is necessary at the initial milling stage to provide sufficient plastic deformation to break the coarse
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chips into sizes that the Φ-6 balls can further refine. The phase transformation from austenite to
martensite also helps form the spherical particle morphology during this ball size transition as it
increases the yield strength of the material and decreases the maximum deformation depth. Once the
chips have been refined to a length scale of several hundred microns, the Φ-6 balls further break down
the intermediate particles to form suitable morphology (near-spherical) and particle sizes for AM more
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efficiently than the Φ-20 balls, as the Φ-6 balls impact the particles more frequently, and the maximum
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deformation depth is significantly reduced. As a particle is impacted by a high frequency of low forces
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from random directions, the aspect ratio of the particle decreases. Despite the inherent challenge of
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function of the ball diameter and the milling time indicates that milling with Φ-6 balls effectively refines
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the particle morphology to be comparable to that of GA powders. Though the powders created by ball
milling of machining chips were not fully spherical in the current study, significant improvement in
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powder morphology modification has been achieved compared to the flattened powders created by ball
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milling of machining chips or atomized powders in other studies [9,10,19–24]. It is worth noting that
perfectly spherical morphology is not necessary for metal AM as previous studies have shown that
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irregular powders such as water atomized powder and ball milled powder can be used in AM
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[5,7,21,22]. Also, producing perfectly spherical particles was not the objective of the present work.
Instead, it was aimed to investigate the possibility of converting recycled machining chips to powders
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that are useful in AM and ultimately identify sustainable feedstock alternatives for AM.
Comparing the results from the two-stage milling approach with those from the single stage
milling for an equivalent milling time, the particle size refinement and morphology evolution in the
experimental observation are consistent with the modeling results for the maximum deformation depth.
The two-stage ball milling of 304L steel swarf yielded 69 wt.% of the powder within the desired particle
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size range, 1% (number percentage) flattened particles, and an average aspect ratio of 1.37. In contrast,
the single stage milling of 304L steel swarf yields much less desirable powders. BM-20-60hr yields 2
wt.% powder with particle sizes 38-150 μm and 38% (number percentage) flattened particles with an
average aspect ratio of 2.15; BM-6-60hr yields 1 wt.% powder with particle sizes 38-150 μm with an
average aspect ratio of 1.39. Therefore, the proposed two-stage milling approach is more effective in
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recycling machining swarf to powders with the desired particle size and morphology that can be used as
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alternative feedstock in metal AM.
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5.2 Microstructure and hardness
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The nanoindentation hardness of the ball milled powder is 56% higher than that of the GA
powder. The increase in hardness is attributed to an austenite to martensite phase transformation [9,47],
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a reduction in grain size [12,35], and an increase in dislocation density [12,35]. Machined chips also
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exhibit a 9% increase in hardness when compared to GA powder. This may be attributed to an increase
in dislocation density and partial phase transformation induced by the plastic deformation of the
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The XRD patterns showed that the 304L machining chips consist of a primary austenitic phase
and a small amount of martensite. After the ball milling, the primary austenitic phase transforms to the
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martensitic phase in the ball milled powder, as illustrated by the higher intensity of the peaks
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corresponding to martensite than that for the austenite. The phase change is induced by the repeated
impact of the milling media on the particles at room temperature. The proposed model indicates that the
yield strength of the steel is surpassed with each impact and the dislocation density is increased due to
the plastic deformation. As the dislocations rearrange themselves to form subgrains and subsequently
high angle grain boundaries, the metastable austenite transforms into martensite [9,47]. The combination
of martensite formation and grain size reduction dramatically increase the hardness of the powder
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particles as evidenced by nanoindentation. As the hardness and strength of the particles increase during
the ball milling, the particles exhibit increasing resistance to further plastic deformation. Consequently, a
near-spherical morphology is achieved by the increased frequency of low-force impacts from the Φ-6
balls.
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The characteristics of the feedstock powder, including morphology, particle size, microstructure,
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and hardness, affect the powder-laser interactions and subsequently influence the feasibility of using the
powder in metal AM. A spherical morphology and controllable particle size are desired to achieve
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adequate flow through the powder feeder in LENS® [5]. Powder morphology and particle size also affect
the packing density and printing resolution in powder bed systems [7,48]. The ball milled powders
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created from the machining chips do not possess perfectly spherical particle morphologies in the current
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work. Nevertheless, controlled particle size and rock-like (near-spherical) morphology have been
successfully achieved. Feasibility of using these ball milled powders (BM-2Stg-60hr) as feedstock in
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metal AM has been verified by successful deposition of single tracks via LENS®. Single tracks made
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from milled powder exhibited adequate adhesion, a uniform melt pool geometry, continuity, and
minimal splatter. Minimal differences were observed between the single tracks made from BM-2Stg-
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60hr powder and the single tracks created from GA powder using identical LENS® deposition
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parameters. Therefore, it is potentially feasible to use ball milled powders created from machining swarf
microstructure of the single tracks and expansion to the deposition to larger builds is ongoing and
necessary to further validate the feasibility of this technique, but these aspects are beyond the scope of
6. Conclusions
In the present study, powders with near-spherical morphology and particle sizes of 38-150 μm
were successfully created from recycled machining chips by implementing a novel two-stage
mechanical milling approach. The viability of using the ball milled powders that were created from
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machining chips as alternative feedstock in metal AM was verified by successful deposition of single
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tracks in LENS®. The following key findings are concluded from this study.
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The modeling results suggest ball diameter is a primary factor that determines the particle size
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reduction and morphology evolution during ball milling. With a consistent ball-to-powder weight
ratio, large balls (diameter = 20 mm) efficiently break up machining chips to coarse powder
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particles while small balls (diameter = 6 mm) effectively modify the powder morphology to
near-spherical.
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Particle size refinement and morphology evolution observed in the experimental work agree well
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with the theoretical analysis. Φ-20 balls effectively break down the 5-20 mm machining chips
into particles with a size on the order of several hundred microns within 24 hours. Continued
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milling with Φ-6 balls increases the frequency of low-force impacts and reduces the powder
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particle size to the range of 38-150 μm, with a near spherical morphology.
A phase change from metastable austenite to martensite was observed in the ball milled powder
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due to severe plastic deformation. This austenite to martensite phase transformation, combined
with other strengthening mechanisms (grain size refinement and increased dislocation density),
lead to a 44% increase in the hardness of the ball milled powder particles compared to that of the
machining chips.
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The ball milled powder was successfully deposited into single tracks via LENS®. Minimal
differences in penetration and uniformity of melt pool geometry are observed between the single
tracks made from BM-2Stg-60hr powder and the single tracks created from GA powder using
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Acknowledgements
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The authors would like to acknowledge the financial support provided by NSF-CBET grant #1605392.
The authors are also grateful to Dr. Deliang Zhang at Northeastern University in China for the technical
discussion he provided.
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Tables:
Table 1: Nominal chemical composition (in weight percentage, wt.%) of the stainless-steel machining
swarf
Elements Fe Cr Ni C Mn Cu Si Mo V
wt. % Bal. 18.18 8.09 0.025 1.3 0.57 0.41 0.26 0.064
Elements W N P Nb Al B S Ti Ca
wt. % 0.059 0.038 0.027 0.013 <0.003 0.0026 0.002 0.002 <0.0005
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BM-2Stg-Int-60hr 24 36
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Note: BM means ball milled powder; 2Stg stands for a two-stage ball milling process that uses Φ-20
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balls initially, followed by milling with Φ-6 balls; “Int” means the ball milling was interrupted at
different milling time lengths to collect the powder for sieving. After sieving, only the powder that was
coarser than 150 μm was further milled. The last digit in the ID means the total milling time length.
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Table 3: Feedstock powder and deposition parameters used to deposit single tracks in LENS®.
Sample ID Feedstock powder Deposition parameters
Laser power (W) Scanning speed (cm/s)
ST-GA-410-1.7 Gas Atomized 410 1.7
ST-GA-360-1.7 Gas Atomized 360 1.7
ST-BM-410-1.7 BM-2Stg-60hr 410 1.7
ST-BM-360-1.7 BM-2Stg-60hr 360 1.7
Note: ST stands for single tracks; GA stands for gas atomized.
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Table 4: Comparison of the number percentage of flattened powder particles and the aspect ratio of the
powder particles among the various powder samples.
Sample ID Number Percentage Aspect Ratio
of Flattened Particles Average D30 D50 D80
BM-2Stg-Int-36h 92% 1.80 1.22 1.45 2.66
BM-2Stg-Int-48hr 16% 1.55 1.34 1.44 1.77
BM-2Stg-Int-60hr 2% 1.41 1.18 1.36 1.56
BM-2Stg-60hr 1% 1.37 1.21 1.34 1.55
BM-20-60hr 38% 2.15 1.62 1.91 2.70
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BM-6-60hr 1% 1.39 1.21 1.32 1.56
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Figure Captions:
Fig. 1: (a) Representative SEM image of stainless steel machining swarf. (b) Higher resolution SEM
image of the highlighted area in (a) showing the surface morphology of machining swarf.
Fig. 2: (a) Schematic diagram of the planetary ball milling setup; (b) schematic diagram showing the
impact between the milling ball and the powder/machining swarf.
Fig. 3: Modeling results of the maximum forces per impact from Φ-20 balls and Φ-6 balls as a function
of the turn angle in a PQ-N04 planetary mill.
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Fig. 4: (a) Modeling results of the normalized maximum deformation depth of a particle impacted by Φ-
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20, Φ-10, and Φ-6 milling balls as a function of the particle diameter. (b) Schematic representation of
the maximum deformation depth induced on a 100 μm particle by the impact from Φ-20 (red line), Φ-10
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(green line), and Φ-6 (blue line) balls.
Fig. 5: Representative SEM images of: (a,b) BM-2Stg-60hr, (c,d) BM-20-60hr, and (e,f) BM-6-60hr
powders, respectively, with a particle size between 105-150 μm.
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Fig. 6: Representative SEM images of: (a) BM-2Stg-Int-24hr, (b) BM-2Stg-Int-36hr, (c) BM-2Stg-Int-
48hr, and (d) BM-2Stg-Int-60hr powders, respectively.
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Fig. 7: Particle size distributions for various ball milled powders determined from sieving: (a) BM-2Stg-
Int-36hr, (b) BM-2Stg-Int-48hr, (c) BM-2Stg-Int-60hr, (d) BM-2Stg-60hr, (e) BM-20-60hr, and (f) BM-
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6-60hr.
Fig. 8: X-ray diffraction patterns of: (a) BM-2Stg-60hr powder, (b) GA powder, and (c) as-received
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machining chips.
Fig. 9: Average nanoindentation hardness of 304L GA powder, as-machined 304L chips, and BM-2Stg-
60hr milled powder. The error bars correspond to the standard deviations.
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Fig. 10: Optical images of single tracks: (a, e) ST-GA-410-1.7, (b, f) ST-BM-410-1.7, (c, g) ST-GA-
360-1.7, and (d, h) ST-BM-360-1.7.
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Highlights
Machining chips were converted to powder usable in additive manufacturing
Two-stage ball milling lead to near-spherical 38-150 μm sized powder
Effect of ball diameter on powder morphology change was analyzed by modeling
Ball milled powder shows a higher hardness than the machining chips
Continuous and uniform single tracks were deposited using ball milled powder
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