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Manufacturing Letters 32 (2022) 54–58

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Manufacturing Letters
journal homepage: www.elsevier.com/locate/mfglet

Letters

Production of powders for metal additive manufacturing applications


using surface grinding
Harish Singh Dhami, Priti Ranjan Panda, Koushik Viswanathan ⇑
Dept. of Mechanical Engineering, Indian Institute of Science, Bangalore, India

a r t i c l e i n f o a b s t r a c t

Article history: Metal powders for additive manufacturing (AM) applications are commonly produced using atomization
Received 1 November 2021 techniques, which are known to be expensive, capital intensive and highly inflexible. In this work, we
Received in revised form 15 February 2022 explore an alternative route for producing metal powders by the use of surface grinding. We demonstrate
Accepted 21 February 2022
the production of nearly monodisperse AISI 52100 steel powders for AM applications. The formation of
Available online 19 March 2022
these powder particles is analyzed using material characterization techniques. We then evaluate the
usability of the produced powders for metal AM using a custom-built directed energy deposition setup.
Keyword:
Post-process analysis of laser-assisted deposition tracks shows that our powders perform just as well as
Additive manufacturing
Metal powders
conventional gas-atomized powders, resulting in void and inclusion-free metallurgical bonding.
Directed energy deposition Ó 2022 Society of Manufacturing Engineers (SME). Published by Elsevier Ltd. All rights reserved.
Powder manufacturing

1. Introduction 304, we use grinding with an abrasive wheel to produce powders.


While there have certainly been past reports of spherical particles
Metal powders are the starting point for a host of net and near- occurring in grinding swarf [9,10], particularly with steels, the pre-
net shape manufacturing processes, ranging from powder metal- cise mechanism of their formation has remained unclear [11–14].
lurgy to metal additive manufacturing (AM) [1–3]. Powders for Explanations ranging from chip melting to charge imbalance-
these applications are produced predominantly by atomization, induced chip curl have been proposed by workers in the grinding
which involves breakup of a molten metal stream into fine droplets community. Furthermore, their utility for AM has never before
via the use of impinging air or water jets. These droplets, com- been explored.
monly under 150 lm in size, then fall under gravity and solidify Here, we present a method for the production of these powders,
rapidly, resulting in spherical or nearly spherical metal powders and describe their formation using a multi-step model. Our calcu-
[4]. Variants of this process are also commercially in use, such as, lations are confirmed by experimental observations of individual
for instance, centrifugal or ultrasonic atomization, that nonetheless powder particles. Furthermore, we demonstrate the utility of our
work on the same principle of jet breakup. powders for metal AM using a custom-built directed energy depo-
However, atomization based processes are plagued by large sition (DED) system. Single deposition tracks made using these
production costs, the resulting powders often cost 3 to 10 the powders are practically indistinguishable from those obtained
price of a cast sample of the same weight. They are also inherently with conventional gas atomized powders. We believe that our
inflexible in that they cannot be easily or economically adapted to results should open the door for a new class of scalable powder
different material or alloy systems [5,6]. A more complete eco- generation techniques that would eventually lead to significant
nomic analysis of the feed-stock and final part produced in additive reduction in costs and, potentially, ensure even wider adoption
manufacturing has been carried out in Ref. [7]. Furthermore, signif- of metal AM technologies. We also hope that this work will serve
icant shape variations are often seen in the final powders, due to to spur more comprehensive studies of complete cradle-to-grave
either convective effects or inefficient ligament breakup [8], fur- manufacturing capabilities within the AM context, and potentially
ther reducing powder yield and adding to the cost. within a single facility.
In this work, we demonstrate an alternative route for the pro-
duction of metal powders as feedstock for AM. Working with both
plain carbon steel AISI 52100 and an austenitic stainless steel SS 2. Methods

⇑ Corresponding author. We produced powders of high-carbon steel AISI 52100 by dry


E-mail address: koushik@iisc.ac.in (K. Viswanathan). surface grinding (without coolant) and post-processing, see

https://doi.org/10.1016/j.mfglet.2022.02.004
2213-8463/Ó 2022 Society of Manufacturing Engineers (SME). Published by Elsevier Ltd. All rights reserved.
Harish Singh Dhami, Priti Ranjan Panda and K. Viswanathan Manufacturing Letters 32 (2022) 54–58

Fig. 1. A 52100 steel workpiece was first cleaned and mounted on aperture and standoff distance of 12–14 mm. The powder delivery
an automatic surface grinding machine. A physical clamp was used was effected via a nitrogen gas line at 3 bar pressure and the
for workholding in lieu of a magnetic chuck, in order to avoid any particle-gas stream was fed using flexible 6 mm tubing. The four
unintentional magnetization of removed particles. A 170 mm lateral nozzle feeds were focused on the substrate and a fiber laser
diameter alumina grinding wheel was used for surface grinding source (1 kW 1070 nm, Max Photonics) was used to melt the
and rotated at a constant speed of 2800 RPM, grinding velocity incoming powder and effect deposition on the substrate. For the
25 m/s. The depth of cut was fixed at 50 lm in each pass and the experiments described in this work, the laser power was fixed at
wheel fed automatically. These particular grinding conditions (in- 300 W (CW mode) with spot size 50 lm and a powder mass flow
cluding the use of an alumina wheel) were chosen based on the rate of  18 g/min. The performance of the produced powders
predictions of an analytical model described in Refs. [15,16]. The was evaluated by printing single layer tracks of 30 mm length on
model predicted maximum temperatures in the chip as a function a steel substrate, and evaluated using post-processing characteri-
of process parameters, and the parameters chosen here were found zation techniques. Single track experiments using gas atomized
to result in the largest temperatures, a necessary condition as SS304 powder were used to qualitatively evaluate the performance
described in the next section. of our powders with commercially available sources.
A collection bin was placed at the end of the feed axis to collect For post-processing and deposition characterization, the speci-
the material removed from the substrate (swarf). This was then men was cut along the cross section, perpendicular to the deposi-
sieved using a 105 lm sieve to remove stringy chips resulting from tion direction, using wire EDM. The cross sections were
grinding, as well as potential loose abrasives. The mean abrasive subsequently polished and etched to directly reveal the grain dis-
size was much larger (200 lm) than the metal powder produced tributions. A 10% Nital solution (10 ml HNO3 in 90 ml of ethanol)
so that any loose abrasives were automatically removed during was used for 3-5 s dwell time while swabbing manually for etching
sieving. Moreover, imaging of randomly sampled stock material the specimens. Initial microstructure analysis was carried out
after sieving was carried out using optical microscopy and scan- using an optical microscope (Euromex bscope). Additional analyses
ning electron microscopy to visually confirm the absence of any were performed using scanning electron microscopy (SEM) with
abrasives. The resulting powder was heated in an oven to 75  C energy dispersive spectroscopy (EDS, Zeiss Ultra55), X-ray diffrac-
to remove any moisture. It was found that this step was crucial tion (XRD) and transmission electron microscopy (TEM, Titan The-
for ensuring the required flowability of the final powders since mis 300 kV). XRD (Rigaku Smartlab) was performed on the
the presence of even ambient moisture caused the powder parti- powders after sieving. Data was acquired at 1°/min scan rate.
cles to agglomerate. TEM samples were prepared using focused ion beam milling—a
The heated powder was then loaded into a twin–hopper pow- thin sample of 15 lm10 lm2 lm was sliced from a spherical
der feeder that was connected to a powder nozzle head (Precitec particle and further thinned down to 50 nm. Hardness measure-
YC30) via a four-way distribution manifold, see schematic in ments were made using FM800 (Future Tech). A 200kgf load was
Fig. 1. The deposition head was rated for 2 kW maximum power, applied for 10 s dwell time for carrying out the hardness
with minimum powder focus spot diameter of 2 mm, 28 mm free measurements.

Fig. 1. Schematic of the powder production method via grinding. (a) Material removed by surface grinding is collected, sieved and heated, prior to use in a DED process. The
corresponding SEM images show the distribution of spherically-shaped particles in the resulting powder. (b) SEM image of a single particle showing perfectly spherical shape
and dendrites on the surface. (c) Particle size distribution in the final powder shows a size range of  20  100 lm.

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Harish Singh Dhami, Priti Ranjan Panda and K. Viswanathan Manufacturing Letters 32 (2022) 54–58

3. Results and discussion the chip to be  600  C, which is far from the melting temperature
of Fe or any steel. Consequently, the powder particles cannot pos-
We present the results of our powder generation experiments sibly be formed from molten drops exiting the grinding zone.
as well as data on their performance in a DED based AM process. Details of this calculation are provided in our earlier work [15].
It is therefore clear that melting of material removed during
3.1. Powder properties grinding must most likely occur as it transits through the air due
to the highly exothermic oxidation reaction of Fe. The following
Powders produced using the grinding process were analyzed at simple consideration is in order. Consider a solid chip with an
each step shown in Fig. 1(a). Firstly, given the choice of process equivalent spherical shape of radius R. If a thin spherical shell of
parameters, material removed from the workpiece contained sig- thickness d ’ 0:01R on the outer surface is subject to oxidation,
nificant fraction of spherically shaped particles, along with stringy the energy released is sufficient to increase the temperature of
and chip-shaped material. Sieving removed many of the latter and the entire spherical volume to well above the melting point.
resulted in predominantly spherical powders, see second SEM Numerical values for the attendant heat release and corresponding
image in Fig. 1(a). This process is therefore capable of producing calculations for oxidation reaction kinetics are presented in our
high powder yield. The resulting powders were heated and stored prior work [15,16]. In fact, this oxidation driven melting mecha-
at 75°C to remove any ambient moisture and aid flowability. nism in grinding has also been postulated by other research
Secondly, an analysis of particle size distribution is shown in groups, albeit qualitatively [9]. Grinding parameters reported in
Fig. 1(c), with particles varying from 10  100 lm in diameter. Fur- the previous section were chosen to maximize spherical powder
ther sieving could make this distribution narrower and more occurrence in accordance with the calculations in [15,16].
monodisperse at the expense of lowering powder yield. Thirdly, a Experimental analysis of the particle surface clearly attests to
high resolution SEM image of a single powder particle is presented this route, see Fig. 2. A cross sectional image of a single particle,
in Fig. 1(b). The occurrence of dendrite-like microstructures on the obtained using focused ion-beam milling, is shown in Fig. 2(a). Sev-
surface is clearly evident. Coupled with the perfectly spherical eral features are evident at once. Firstly, corresponding spec-
shape, this feature of the powder particles makes it clear that they troscopy data (yellow box) shows the presence of a very narrow
must have been formed by solidification from the melt. Finally, we oxide layer on the surface of the powder. The thickness of this layer
note that grinding itself is analogous to machining, except for the is barely 1 lm, as expected from the energy considerations
fact that it uses abrasives that are stochastically distributed, with described above. Secondly, this SEM image also shows the occur-
a range of large negative rake angles and depths of cut. Hence, if rence of voids inside the powders, likely the analogue of solidifica-
melting is to occur as the particles are removed from the work- tion shrinkage. The corresponding X-ray diffraction images with
piece, the local chip temperature must reach in excess of 1500°C. the complete powders show the occurrence of both oxide (Fe3O4)
Unfortunately, the nature of the grinding process makes direct and a-Fe (BCC) peaks, see Fig. 2(b). Compared to BCC iron, these
measurement of these temperatures very challenging. This situa- additional oxide peaks occur at 2h values of 29:6 ; 34:8 ; 55:9
tion is further encumbered by the fact that conventionally used and 61:4 . That a-Fe occurs immediately below the thin oxide layer
models of temperature rise in grinding almost always neglect heat is confirmed by TEM SAD and HRTEM images taken near the top
lost to the chip [17,18], rendering even theoretical order-of- surface, see Fig. 2(c). The TEM image corresponds to a ½112 zone
magnitude estimates impossible. To address this issue, we used a axis, and the resulting diffraction spots are shown indexed in the
four-body heat partitioning scheme to estimate the maximum figure.
temperature rise in the removed chip, based on the work of Ju At this juncture, it is certainly noteworthy that in plain carbon
et al. [19]. We found the maximum possible temperature rise in steels, atomized powders do also show thin oxide layers and

Fig. 2. Properties of final powder particles. (a) SEM image and associated EDS spectrum showing presence of thin oxide layer on the surface. (b) X-ray diffraction results on
the powders show the occurrence of both a-Fe and Fe3O4 peaks. (c) TEM SAD and HRTEM images of section just below the surface show that the powder particles are indeed
primarily a-Fe.

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Harish Singh Dhami, Priti Ranjan Panda and K. Viswanathan Manufacturing Letters 32 (2022) 54–58

internal voids, just as with our powders. In fact, commercial use of micrograph (top right panel) shows that the deposited material is
atomized powders often first involves suitable treatment in a metallurgically bonded with the substrate with no internal voids
reducing environment (such as dissociated ammonia) to reduce during deposition. Any potential effect of the thin oxide layer is
the oxide content [20]. This is particularly pertinent in situations also not evident in the final track, cf. EDS data shown in the bottom
where even tracer oxide inclusions are unacceptable in the final left panel. This spectrum was taken completely inside the track
deposited tracks. (yellow box) and shows no trace of oxygen.
A detailed microstructural image of the track and substrate
3.2. Powder performance in laser-based DED cross section was obtained by metallographic etching, see Fig. 4.
The micrograph in panel (a) shows typical lath martensite struc-
We used the produced powders in a custom-built directed ture that is commonly observed in Fe-C alloys [23]. This is the
energy deposition (DED) setup, as described in Section 2. Single result of a diffusionless phase transformation that occurs due to
track experiments were performed using nitrogen as the carrier high cooling rates in the DED process [24]. Microstructure of the
and shielding gas. The properties of the deposited track are shown individual sections near the head (red) and base (yellow) of the
in Fig. 3. The SEM image in the top left panel shows a top view of track show uniform martensite structure, and uniform bonding
the track, with a few attached satellite particles, as expected. The between track and substrate, respectively. The main micrograph
track thickness is nearly constant  300 lm, and is indistinguish- in panel (a) also shows the near triangular heat affected zone of
able from an equivalent one produced using gas atomized powder extent  1 mm, typical of DED processes.
(see bottom right panel). The longitudinal ‘striations’ are a com- Finally, micro Vickers hardness measurements along the track
mon occurrence in DED processes when process conditions are cross section and into the substrate are shown in Fig. 4(b). The
sub-optimal, and have no bearing on the performance of the pow- error bars in this plot represent the maximum and minimum hard-
der themselves [21,22]. Furthermore, a polished cross sectional ness values obtained from 3 indents in a given region. The hardness

Fig. 3. Single track deposition experiments show the utility of the produced powders. SEM image of a single track shows consistent width of the track (top left panel).
Complete metallurgical bonding is confirmed by the cross sectional micrograph (top right panel). Elemental mapping of the deposited track shows the absence of any
significant oxygen (bottom left panel). Single DED track using gas atomized SS304 powder is shown for comparison (bottom right panel).

Fig. 4. Cross section and properties of deposited track. (a) Etched microstructure of the cross section clearly shows the heat affected zone. Higher magnification micrographs
of the track (red) and the substrate (yellow) show uniform martensite microstructure and uniform metallurgical bonding, respectively. (b) Hardness variation along the
transverse cross section shows uniformly high hardness (380–420 HV) in the deposited track, transitioning to lower hardness (< 300 HV) outside the heat affected zone. Note
that error bars correspond to maximum and minimum measured over 3 indents in the vicinity of the particular location.

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Harish Singh Dhami, Priti Ranjan Panda and K. Viswanathan Manufacturing Letters 32 (2022) 54–58

is nearly constant within the track itself and decreases sharply out- References
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cial interests or personal relationships that could have appeared
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Acknowledgments
investigation on the effect of powder recycling on the microstructure and
mechanical properties of AISI 316L produced by Directed Energy Deposition.
The authors would like to acknowledge financial support from Mater Sci Eng: A 2019;766:138360.
the Science and Engineering Research Board (SERB), Govt. of India [30] Terrassa KL, Haley JC, MacDonald BE, Schoenung JM. Reuse of powder
feedstock for directed energy deposition. Powder Technol 2018;338:819–29.
under grant CRG/2018/002058. Financial support from the Indian
Institute of Science, Bangalore is also gratefully acknowledged.

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