Powder Technology 441 (2024) 119815

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Review

Research progress of the metal powder reuse for powder bed fusion additive
manufacturing technology
Jiwen Li a, *, Wei Liu a, Jie Shen b, *, Xin Zhang a, c, Shunjie Li a, Zhenshuai Wang a
a
Material Science & Engineering School, Henan University of Science & Technology, Luoyang 471023, China
b
Department of Computer& information Science, University of Michigan-Dearborn, Dearborn 48128, United States
c
School of Intelligent Manufacturing, Nanyang Institute of Technology, Nanyang 473004, China

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• The stronger interaction results in the

characteristics changes of recycled
powder.
• Understanding thermal history of the
powder is helpful for powder
characterization.
• Timely tuning of process parameters is
useful to powder recycling and part
quality.

A R T I C L E I N F O A B S T R A C T

Keywords: Additive manufacturing (AM), epitomized by powder bed fusion (PBF), has emerged as one of the fastest-
Additive manufacturing (AM) growing, most dynamic, and highly focused techniques within the advanced manufacturing sector. Neverthe­
Powder bed fusion (PBF) less, as the primary factor determining cost and quality of PBF-produced parts, amounts of metal powder
Recycled powder
feedstock remains unused and requires recycling after each PBF build. Due to the unique thermal history
Reused powder
Characteristics of used powder
experienced by individual particles during manufacturing, recycled powders exhibit variations in chemical
High quality products composition, particle morphology, size, size distribution, microstructure, and even thermal-physical properties.
Moreover, these alterations are influenced by the inherent properties of the metal powder, machine setup, and
manufacturing process. Consequently, the repeatability and reproducibility of the recycled powders cannot be
defined uniformly. Using Ti6Al4V, Inconel 718, AlSi10Mg, and stainless steel metal powders as examples, this
paper reviews recent literature specifically addressing recyclability and reusability of the recycled powders, in
particular the subsequent effects of the reused powder on powder beds, process operation, and product properties
in PBF builds. By exploring the interaction between energy beam, powder and melt pool, we discuss the for­
mation mechanism and composition of the recycled powders, and analyze the impact of powder building cycles
and varying powder characteristics on powder bed properties, manufacturing processes, part microstructures,
and mechanical properties. Additionally, we discuss the solutions for identifying end-of-life powder and intro­
duce strategies to enhance powder reusability. In doing so, we seek to provide a comprehensive understanding of
powder feedstock for building an optimized processing window, with a view to contributing to extending the
service life of metal powders.

* Corresponding authors.
E-mail address: ljwzq@[Link] (J. Li).

[Link]
Received 29 November 2023; Received in revised form 20 April 2024; Accepted 27 April 2024
Available online 3 May 2024
0032-5910/© 2024 Published by Elsevier B.V.
J. Li et al. Powder Technology 441 (2024) 119815

1. Introduction institutes and production enterprises. Our emphasis is to fill the inter­
action information gap between the reused powder, build cycles and
Additive manufacturing (AM) technology, successfully digitized the part properties in the PBF process. Moreover, the key research fields and
design and manufacturing process, has been regarded as one of the topics related to the metal powder in the future are prospected.
driving engines of the next generation industrial revolution [1]. Metal
additive manufacturing, a significant aspect of AM technology, facili­ 2. The formation mechanism and composition of recycled
tates the fabrication of objects by successively printing layers upon powder
layers, allowing designers to develop customized or intricate models in a
single step. Furthermore, rapid solidification at cooling rates of PBF process can be subdivided into laser beam (PBF-LB), electron
approximately 106 K/s enables fabricated builds to achieve a non- beam (PBF-EB), and infrared light (PBF-IrL). By the end of 2022, PBF-LB
segregation effect, maintain internal structural uniformity, and opti­ have led the market and accounted for a 23.77% share of the global
mize the balance between mechanical properties and material utiliza­ revenue [3,6]. Given this paper’s emphasis, our attention is focused on
tion. Consequently, AM is emerging as an innovative and essential the PBF-LB and PBF-EB. PBF-LB differs from PBF-EB primarily in terms
manufacturing method within the metal processing domain. Particularly of the energy source and chamber environment. In a controlled inert gas
in the fabrication of high-quality end-use products such as aerospace environment, PBF-LB utilizes an Nd: YAG fiber laser or carbon dioxide
engine components, medical apparatus and instruments, and new en­ laser as a heating source to achieve layer-by-layer formation and pro­
ergy equipment components, AM demonstrates exceptional value and duce higher precision parts with superior as-built surface quality [9].
vast application potential due to its ability to process complex structural For PBF-EB technology, a high-energy electron beam serves as the heat
parts and cater to the efficiency demands of specific industries. This has source. In a vacuum environment, the pre-spread powder is preheated
spurred the rapid development of metal AM processes. According to the and melted, solidified, and stacked layer-by-layer to manufacture near
Wohlers Report 2023, in 2022, the global revenue of AM products and net shape metallic components [10].
services reached about $18 billion, an increase of 18.3% from a year ago When performing PBF-LB or PBF-EB process, the laser or electron
[2]. beam is irradiated into the powder bed according to the designed pro­
IDTechEx predicts that innovation in metal AM will propel the cess, and is rapidly absorbed by the selected powder particles. Subse­
market to hit $18.5 billion by 2032, with a compound annual growth quently, these selective powder particles are melted quickly to create a
rate of 18.8% [3]. At present, Powder bed fusion (PBF) technology has melt pool. The high temperature liquid metal then further traverses
emerged as one of the most prominent directions in the field of metal through the powder bed under the action of thermo-capillary, and
AM, and PBF machines have accounted for 54% of the metal AM market rapidly solidifies. Once a layer is formed, the powder bed descends by a
[4]. PBF technology has also promoted the rapid growth of the powder predetermined layer thickness. The energy beam then melts the new
feedstock. Nonetheless, the manufacturing cost of metal AM remains layer, merging it with the previously solidified layer to realize the
high, primarily due to the rising price of metal powder feedstock. For metallurgical combination. This process repeats until the parts are
instance, in the case of titanium alloy, aluminum alloy, and stainless finished [11]. So, the forming mechanism of PBF-LB and PBF-EB process
steel metal powders, the price of metal powder feedstock varies between inferred that the manufacturing is a highly complex process involving
$50 and $520 per kg [5]. In comparison to traditional subtractive numerous physical phenomena, including but not limited to: the ab­
methods, raw material costs differ by a factor of 10 to 100. Fortunately, sorption and scattering of input energy, chemical reactions, heat trans­
there are potential approaches to reduce powder feedstock consumption fer, melt liquid flow behavior, solidification, as well as phase transition.
and costs. A widely adopted practice is to recycle the unused powder for Domröse and Grünberger [12] discovered that the laser-induced
reuse in subsequent buildings. Sartin [6] discovered that only 6.7% of metal vapor can be generated due to the interaction between laser and
powder was used in the production of the AM parts. In the PBF process, powder. Lawrence Livermore National Laboratory researchers [13]
10 vol% -20 vol% of powder feedstock is melted to fabricate parts, and explained that the vapor cloud has a larger temperature and pressure
the rest should be recycled [4]. Even with the relatively high utilization than the build chamber atmosphere, creating a downward force on the
rate of directed energy deposition (DED), only half of the powder melt pool called recoil pressure. The recoil momentum is dominated by
feedstock (50.2 vol%) is utilized to the component [7]. Thus, it can be the temperature gradient and Marangoni effect of the melt pool, leading
inferred that a very small proportion of powder is used in each to the denudation zone by pulling in the melt-pool-adjacent particles.
manufacturing cycle, necessitating the recycling of the majority of un­ The vapor cloud also generates local pressure-driven flow currents,
used powder. named as vapor entrainment, which drags particles from the surround­
Serving as one of the crucial factors in controlling cost and pro­ ing powder bed into the path of the laser beam, forming a denudation
moting the widespread application of PBF process, the recycled powder zone around the melt pool. Matthews [13] indicated that denudation is
and its reusability have a significant influence on the economy of the highly dependent on the gas flow pressure and laser parameters, and can
process and the consistency of part properties. LPW Technology Ltd. be expressed by the Knudsen number (Kn). Kn value can be used to
reported that material costs could be reduced by 92% if a batch of determine the trend of powder particles in denudation area. Powder
powder was reused 15 times [8]. However, the recycled powder covers particles can be drawn into the melt pool or ejected upward when Kn <
some process-affected particles that physical and chemical properties 1; while for Kn > 1, the vapor flume expands, pushing the particles
have changed compared to the virgin powder. Whether it can continue outward. Fig. 1 illustrates the interaction between the energy beam,
to be reused needs further assessment. Thus, recycling strategies such as powder and melt pool [14–16]. While the melt pool solidifies into
sieving, regeneration or reconditioning technologies are introduced in forming, the interaction can bring some side effects, leading to powder
order to convert the recycled powder into the reused powder. Up to now, contamination, such as the generation of spatter and condensate parti­
a pressing question in PBF process is how to improve the utilization rate cles, partial fusing, agglomeration, and oxidation.
and service life of the reused powder under the premise of the contin­ Thus, based on the interaction between energy beam, powder and
uous operation and the stability of the product quality. melt pool, the powder bed can be divided into three zones according to
In this paper, we focus on the recycled powder and its reusability in the distance between the location of powder particles and energy beam:
PBF process. We provide an extensive discussion on the formation direct interaction zone, heat-affected zone and free from affected zone.
mechanism and composition of the recycled powder, characteristics In the direct interaction zone, the powder particles are irradiated by the
variations of the reused powder and its subsequent effects on powder energy beam and fully melted to form the melt pool. Due to the high
bed, and the influence of usage amount and reuse cycles on product degree of superheat under high energy beam irradiation, a heat-affected
quality. All based on recent research advancements from international zone dominated by denudation phenomenon is easily formed around the

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J. Li et al. Powder Technology 441 (2024) 119815

melt pool. In the heat-affected zone, powders can be divided into the termed droplet spatters, is formed by the ejection of molten metal under
cold and hot ejections according to their interactions with heat sources recoil pressure. Because of vaporization, expansion and shock waves
(energy beam and melt pool) [17]. Cold ejected particles are entrained caused by the interaction between the laser and the melt pool, small
by the vapor plume and swept upward with high speed in the opposite droplets in front of the laser beam are ejected only a short distance and
direction of the laser motion, thus forming spatter or condensate parti­ then deposited on the powder bed to form Type III particles. Type III
cles. Hot ejections are also entrained by the plume but directly interact particles can condense directly on the powder bed to form individual
with the heat source, contributing to melt pool formation. In the free particles, bond with the particles on the powder bed, or adhere to other
from affected zone, the powder particles are far away from the heat- spatter particles, thus affecting the morphology and microstructure of
affected zone and maintain their initial morphology. After each build­ the recycled powder.
ing, all unmelted powder particles remaining in the building chamber
can be recycled, except for the melted powders. 3. Characteristics of the recycled powders
Wang [14] and Pinto [18] suggested that these recycled powder
particles can be classified into three groups. The unmelted particles far 3.1. Morphology, particle size and particle size distribution (PSD) of the
away from the heat-affected zone are the Group I, which is the main recycled powder
composition due to the largest proportion in the recycled powder. Group
II consists of particles near or in contact with the heat-affected zone. In recent years, studies on the recycled powders in PBF have
Owing to agglomeration by sintering or partial fusing, changes in shape, demonstrated that the reuse times of the powder greatly impact the
size or microstructure may occur for these particles [19]. Condensate morphology, particle size, and PSD [20–25]. The changes exhibit some
and spatter particles ejected and deposited on the powder bed are regularity, despite varying degrees. As cycling times increase, the
regarded as Group III, classified into three types according to their for­ roundness of powder particle decreases, transforming from spherical to
mation mechanism, known as Types I, II, and III. Type I is the metallic irregular, with crushed, elongated, and adhered appearance. Recycled
jet, which is formed by the ejection inside the incident laser beam. Due powder surfaces become rough, and some large powder particles exhibit
to being expelled out from the laser beam and then rapidly solidified, satellite particles or oxides (Fig. 2). Furthermore, the changes of the
these particles have a spherical shape and smooth surfaces. Type II, powder morphology can also be reflected by the typical morphologies of

Fig. 1. Illustration of interaction between the energy beam, powder and melt pool during the PBF process [14–16].
(a) PBF-LB, (b) PBF-EB.

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J. Li et al. Powder Technology 441 (2024) 119815

(a) (b) Satellites

Irregular shaped
Satellites Satellites Crushed
Elongated

Bonded particles
Satellites

Bonded particles

Fig. 2. Various SEM images of PBF-LB/M/316 L recycled powders [25].

residual powders, shown in Fig. 3, including large particles, irregular PSD, and overflow and spatter powders exhibited a right shifted PSD,
particle, bonded and agglomerated particles, and particles attached proving that distributions shifted towards the larger particles [28].
condensate, spatter or satellites. Similar results were observed for Ti6Al4V powders produced by PBF,
Fig. 4 displays the PSD changes of five typical alloys (17–4PH, 316 L, where the PSD became slightly narrower with reuse times [23,29]. In
AlSi10Mg, Inconel 718, and Ti6Al4V) under different PBF processes. The summary, the choice of metal materials, PBF process and process pa­
experimental information in literature [23,26–29] shows that these rameters, and even experiment details not described, can affect the PSD
recycled powders have been treated by the sieving process before the change of the recycled powder.
PSD measurement. It can be seen that powder reuse has various effects The reason for the narrowing of the PSD is due to the melting of fine
on the PSD. Both increases and decreases in PSD have been reported in particles in the manufacturing or their removal during sieving process,
the literatures. When using the PBF-LB process to fabricate 17–4PH thereby resulting in the continuous decrease in the quantity of fine
stainless steel after 10–20 building cycles, the PSD notably widened particles during successive reuse. Simultaneously, powder coarsening,
[26]. After thirty powder reuses of 316 L in PBF-LB, a slightly wider size resulting from agglomeration or sintering, leads to an increase in the
distribution shifting towards larger particles was observed [21]. For average particle size [7,23]. Sieving process contributes to eliminate the
PBF-LB/M/AlSi10Mg, the PSD of reused powder gradually shifted larger, bonded, partially sintered particles that exceed the size specifi­
slightly to the left with reuse, indicating a progressive reduction in the cations required by the process regulations, resulting in a narrower PSD
volume of the larger particles [27]. However, when PBF-LB/M/Inconel [19,30]. Notably, in the PBF-EB process, the molten finer particles and
718 powder was reused after 20 cycles, the used powder had a narrower coarsened particles are present in relatively larger quantities because of

Fig. 3. Typical morphologies of the PBF-LB/M/17–4PH stainless steel residual powders [26]. (a) large particles, (b) and (c) irregular particles deformed by the roller,
(d) bonded particles, (e) and (f) accumulations of particles with different sizes, (g) and (h) particles adhere to condensate or spatter, and (i) particles with satellites.

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J. Li et al. Powder Technology 441 (2024) 119815

Fig. 4. PSD for the typical recycled powders in PBF process. (a) 17–4 PH stain steel in PBF-LB [26], (b) PBF-LB/M/316 L [21], (c) PBF-LB/M/AlSi10Mg [27], (d) PBF-
LB/M/Inconel 718 [28], (e) PBF-E/M/Ti6Al4V [23], and (f) PBF-LB/M/Ti6Al4V [29].

the high temperature chamber atmosphere, leading to a narrower PSD metal powders but are also influenced by the dynamic behavior of
for the recycled powders during subsequent processing [23]. Addition­ powder sintering. Chandrasekar [24] compared the recycling behavior
ally, Powell [4] suggested that the narrow PSD may also be due to the of Ti6Al4V and Inconel 718 powders in PBF-EB using process log data.
fact that the PBF-EB recycled powder is treated by blasting to break the For Inconel 718 powder, an increase in number of large-sized particles
bonds tween particles, compared to that of only being sieved in the PBF- and a corresponding increase in average powder size were observed.
LB. Conversely, Ti6Al4V recycled powders exhibited the insignificant
There are conflicting opinions on why the PSD shifts towards larger change in particle sizes. Utilizing process log data, he discovered that the
particles and increases with reuse. Andani [31] proposed that although average building time for Ti6Al4V was 38 s per layer, while for Inconel
some recycled powders have grown in particle size, they are still small 718 was 84 s per layer, indicating that the sintering kinetics of Ti6Al4V
enough to pass through the process specified sieve, potentially shifting were at least twice that of Inconel 718. The slow sintering behavior of
the PSD towards larger particles. Jacob [32] concurred that a high Inconel 718 powder tends to agglomerate over multiple recycling cycles;
proportion of fine particles causes agglomeration effects, but also there in contrast, Ti6Al4V powder appears to sinter rapidly, irrespective of
are small particles more likely to vaporize and melt during the build recycling. In addition, it should be noted that although only Inconel 718
process or to be removed during recycled powder post-process. Mean­ and Ti6Al4V in PBF-EB process are taken as examples, the influence of
while, the majority of larger particles may be removed by the recoating sintering thermodynamic behavior can be extended to PBF-LB process
arm, causing a higher proportion of small particles to be utilized and the and other alloy powders to study their morphological changes.
larger particles to be recycled repeatedly [33]. As a result, the recycled
powders exhibit a gradual but consistent increase in the proportion of
large particles, and a reduction in the number of small particles, leading 3.2. Chemical composition of the recycled powders
to a slightly broader PSD shifted towards the large particles.
It is worth noting that changes in particle shape, size, and PSD of The change in the chemical composition of the recycled powder must
recycled powder are not only associated with the inherent properties of be the result of the chemical reaction. The active substances (such as
oxygen, nitrogen or carbon) remained in the powder particles and the

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powder bed allow the chemical reactions to occur due to the interaction though the liquid rapidly solidified, it was still sufficient time for
between the powders, energy beam and melt pool during the PBF for­ available O and N to react with the high temperature molten metal, thus
mation. The result of the chemical reaction is either creating a stable increasing the O and N contents. The second reason attributed to the
oxide layer around particles, dissolving deeper into the particles or occurrence of the turbulent phenomenon in the melt pool on a very small
forming particulates on the surface of particles [4]. Although chemical scale, in which molten droplets were ejected and reacted with the O and
reactions can be minimized in PBF-LB processes by introducing inert gas N in the surrounding atmosphere. These ejected particles then fell into
into the build chamber or maintaining high vacuum in the PBF-EB the powder bed and contributed to the increase in O and N content of the
process, this can only mitigate rather than eradicate. Metal powders recycled powder, intensifying with powder reusing. The third reason is
are prone to chemical reactions is due to two unavoidable factors: large the contribution of the heat-affected zone (HAZ) to powder degradation.
specific surface area of the powder and an elevated temperature during Depending on the particles size and the surrounding temperature, the
formation [4]. In PBF process, metal powders with a high sphericity chemical composition, morphology, and microstructure of the powder
expose a larger surface area, thus increasing chemical reactivity as there in the HAZ can be altered.
is a greater region to react with contaminants. On the other hand, the In the PBF-EB process, the chemical composition of the recycled
build chamber is held at an elevated temperature during the build powder located in a vacuum can also be changed. The contamination of
process. Even if the PBF-LB process does not require preheating, a rise in recycled powder mainly originates from four aspects. First, contamina­
temperature allows chemical reactions to occur more easily. tion derives from residual hydrocarbons in the virgin powder. These
In addition, Harkin [34] found that 20–35 vol% of the powder bed carbonaceous materials can be broken under the electron beam, deposit
could be occupied by the ejected particles due to its deposition back into on or react with the hot layer of the powder bed. The second is the
the powder bed. Spatter formation is small droplets of molten material decomposition of residual water molecules in the powder leading to the
ejected from the melt pool due to dynamic melt flow patterns [14–16]. increase of hydrogen and oxygen content in the recycled powder. The
Spatter particles generally differ from the virgin powder in chemical third is the sublimation loss of some low-melting elements caused by
properties, which includes an increase in oxygen content, oxide forming, high vacuum, high energy beam and high temperature environment.
hydrogen and nitrogen increase, or the variations of other alloying Lastly, it is worth mentioning that the residual gas remaining in the
element [26,31,39,and]. When the spatter particles landed back into the virgin powder and powder bed can intensify the oxidation of the powder
powder bed and then had the potential to be incorporated into melt pool under the intense the interaction between the energy beam, powder and
formation, the oxides surrounded on the spatter particles can be trans­ melt pool. The oxidizing elements such as Ti, Si, and Al are prone to form
ferred to other powder particles, or the oxides could be melted into the oxides on the powder surface, thereby increasing the oxygen content and
rest of the consolidated material, thus changing the chemical reducing the content of oxidizing alloying elements on the surface of the
composition. recycled powder.
In the PBF-LB process, the manufacturing chamber is controlled by Petrovic [38] investigated the chemical composition of Ti6Al4V
an inert gas protected environment, filled with high gas content in the powder during 16 build cycles in PBF-EB process. The results showed
chamber and powder bed. In addition, during the processes of powder that the oxygen content increased linearly from 0.14 wt% to over 0.20
preparation, transportation, storage, sieving, regeneration, mixing, and wt%. Notably, under the influence of high vacuum, high steam pressure,
contact with humid air, the moisture content of the powder can increase. and high-temperature environment, low melting point Al element is
Therefore, the laser beam can cause gas and water electrolysis or ioni­ prone to oxidation and sublimation loss, resulting in an oxide layer on
zation during the process, leading to an increase in the content of oxy­ the reused powder surface after 10 reuse cycles in the PBF-EB /M/
gen, hydrogen, nitrogen, and other gas elements in the building chamber Ti6Al4V process [39]. The chemical composition changes of nickel alloy
and melt pool. This in turn intensifies chemical reactions and powder powder in PBF-EB is similar to that of Ti-based alloy. Elements such as
contamination, which is reflected in the variations of the surface Ni, Cr, Al, Fe, and Ti have a high tendency to form oxides in the presence
chemical composition of the recycled powder. Sartin [6] collected 228 of oxygen, potentially leading to the formation of NiO, Cr2O3, Al2O3,
samples of 316 L powder after thirty-one builds, and found that the FeO/Fe2O3 or TiO/TiO2. According to Gruber’s investigation [40], the
surface chemical composition of the recycled powder exhibited signifi­ oxygen content of Inconel 718 recycled powder increased from 146 ppm
cantly higher content of oxygen and hydrogen, and the compositions of to 266 ppm after 14 reuse cycles, and Al2O3 nanoparticles were formed
oxygen, hydrogen, carbon, sulfur, and titanium were widely distributed. on the surface of the powder particles after 70 h of successive reuse.
Pablo [26] studied 17–4PH stainless steel powder and discovered that Moghimian [41] compared the variation of oxygen content in
carbon concentration remained stable with reuse. Whilst the concen­ Ti6Al4V powder per reuse cycle between PBF-LB and PBF-EB process.
tration of oxygen and nitrogen increased with reuse, with oxygen con­ Despite the influence of several factors and process parameters, the
tent increasing by 13.8% after 10 cycles and 10.3% after 20 cycles. The average increase of oxygen content was 10 ppm per cycle in the PBF-LB
increasing concentration of oxygen can be explained by the formation of process compared to that of 70 ppm in the PBF-EB process. The seven-
alloy oxides, including Fe2O3, Cr2O3, NiO, Cu2O, SiO2, and MnO2 on the fold difference is due to two primary factors. The first reason lies in
surface of the reused powder. By the same mechanism, Oscar [29] also the difference of the operating temperature. It is widely known that the
found that the oxygen content of Ti6Al4V powder increased from 0.09 affinity between titanium and oxygen increases with temperature. In
wt% to 0.13 wt% after 31 cycles in PBF-LB processes. Notably, Al-based contrast to the 200–300 ◦ C temperature of the PBF-LB process, PBF-EB
alloys with strong affinity for oxygen and hydrogen exhibit a significant powder is exposed to a high-temperature environment of over 650 ◦ C,
variations in chemicals after reuse. Raza [35,36] investigated the promoting the oxygen absorption process. The second reason is the
degradation behavior of recycled AlSi10Mg powder and reported that ionizing radiation of residual water molecules within the chamber, the
~3 vol% of spatter particles had the oxide layer with a thickness ranging probability of water molecules undergoing radiolysis by an electron
from 50 nm to 125 nm after reusing the powder for about 30 months. beam is much higher than that of a laser beam, contributing to the
Meanwhile, hydrogen measurements showed an increase of 50 ppm increased oxygen content in recycled PBF-EB powder [41].
from 80 ppm to 130 ppm. In conclusion, the variation of the chemical As can be seen from above mentioned, oxidation may be unavoid­
composition primarily depended on the sensitivity of the alloying ele­ able. According to the equilibrium partial pressure of the oxygen
ments, operating temperature, environmental composition and reuse threshold (10− 58 atm in Ellingham’s diagram), below which no oxida­
times. tion should occur. However, even at near vacuum pressures used in
LPW Company [37] elucidated the mechanisms of chemical varia­ electron beam, the corresponding oxygen partial pressures (2 × 10− 8 - 2
tion in the recycled powder during the PBF-LB process. The first reason × 10− 9 atm) were still higher than the oxidation threshold [39,40].
is the continuous formation of the high-temperature melt pool. Even Although the oxidation could be reduced by evacuating the chamber

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before flooding with high purity Ar in PBF-LB process, oxidized particles undergone a heat treatment due to the elevated build chamber tem­
were still observed in the recycled powder, indicating that this is a tricky perature. Combined with the change of chemical composition of pow­
problem. der, its microstructure will be inevitably changed. This is especially true
In addition, the interaction between the energy beam and the powder for titanium alloy, where the oxygen content in reused powder is higher
can cause the evaporation of some alloying elements, which involves the than in virgin powder. Oxygen atoms occupy interstitial sites in the HCP
change of alloying element content [10]. The evaporation of alloying lattice, causing slight tetragonal lattice distortion, with microstructure
elements is mainly due to the strong input of energy [14–16]. Further­ ranging from near-virgin martensitic alpha to heavily coarsened alpha
more, the vacuum of the PBF-EB process decreases the evaporation platelets with intergranular beta. Both the coarsening and the range of
temperature and increases the evaporation of lightweight elements [23]. microstructure distribution increased with the reuse cycles. Addition­
For this reason, the recycled powder may have a lower alloy element ally, Wei [43] observed that, compared to the virgin powder’s micro­
content than the original powder. For example, with the increase of structure (primarily α and α/ phases), the β phase became visible after
oxygen content from 0.08 wt% to 0.19 wt%, the Al content decreased one reuse, near-equiaxed prior β grains appeared after the fourth reuse,
from 6.47 wt% to 6.37 wt%. The V content also registered a slight and α phase boundaries disappeared after five reuses. Following six re­
decrease [23]. Although these minor changes remain within alloy- uses, the microstructure transformed into a lamellar α + β phase, fol­
specific values, they can not be underestimated. lowed by lamellar colonies and Widmanstätten structures after the
On the other hand, the variation of alloying elements on powder seventh reuse. Wei concluded that the increase in oxygen content from
surface is related to their affinity with oxygen. With the increase of the 0.12 wt% to 0.15 wt% was the main reason for the phase transformation
build cycles, the content of oxygen increases. Correspondingly, non- in recycled powder. The changes in microstructure with the reuse are
metallic inclusions can be formed on the surface of the powder, thus shown in Fig. 5.
altering the content of the alloying element. For the PBF-LB/M/316 L In the PBF-LB process, the variation of microstructure and phase
recycled powder, owing the increase of oxygen and carbon content, a structure is also influenced by thermal history and the distance between
slight increase in Cr, Ni, Mn, P, S, N, and a slight decrease in Fe, Mo, and particles and heat-affected zones. Microstructure changes were observed
Si in the reused powder were detected. Accordingly, reused particles had in PBF-LB/M/304 L and 316 L stainless steel recycled powder, as non-
a much higher distribution of 79.5 nm nodules scattered along a 4.4 nm equilibrium conditions driven by high cooling rates led to sufficiently
thin SiO2 layer. Furthermore, due to a depletion zone formed by large undercooling, facilitating the formation of metastable phases.
segregating species (Si, Mn, Cr) that have a high affinity for O, a Ni-rich Consequently, the ejected particles contained ferrite (δ) phase due to
layer was discovered just beneath the surface [21]. being supercooled. For example, δ phase constituted 7.8 vol% in PBF-
LB/M/304 L spatter particles, compared to 0.6 vol% in virgin powder
[44]. In PBF-LB/M/316 L powder, the virgin powder and reused powder
3.3. Microstructure and phase structure of the recycled powder for 30 cycles contained less than1 wt% and 1–2 wt% of the δ phase,
respectively [21]. Slotwinski [19] investigated the microstructure evo­
In the PBF process, it can be concluded that the recycled powder lution of 17–4PH stainless steel powder, observing an increase in α phase
mainly consists of unused particles away from the heat-affected zone, a up to 45 vol% along with a decrease in austenite (γ) phase down to 55
minority of condensed droplets, spattered particles, and the near heat- vol% in the sieve residue powder. In contrast, as the austenite-stabilizing
affected zone powders. The unused powders away from the heat- character of the nitrogen-containing inert gas was used in the PBF-LB
affected zone experience less interaction, and their microstructure re­ process, the γ phase of the 17–4PH recycled powder showed a slight
mains largely unchanged. However, the spatter and condensate particles increase [26]. For AlSi10Mg recycled powder, phase structure also
originated by the violent interaction are bound to cause deviation in differed between condensate powder and powder away from the heat-
microstructure due to having undergone the liquid-solid phase trans­ affected zone [45]. In terms of condensate powder, the matrix
formation. As for particles near the heat-affected zone, they undergo appeared as the plates (islands) of silicon phase with short and thin arms
thermal cycling, which affects their microstructure. The extent of these and exhibited more interconnection, potentially related to the thermal
changes depends heavily on the specific thermal history of individual history during the PBF-LB manufacturing. Furthermore, thermal cycling
particles and the distance from the heat-affected zone [42]. promoted the diffusion of silicon phase, and intensified the diffusion and
In the PBF-EB process, for unused powders not involved in part precipitation of silicon phase in the α-Al matrix. The microstructure
manufacturing, the recycled powder can be considered to have

Fig. 5. Cross-sectional images of Ti6Al4V powder with reuse times [43]. (a) virgin powder, (b) 1th reuse, (c) 2th reuse, (d) 3th reuse, (e) 4th reuse, (f) 5th reuse, (g)
6th reuse, (h) 7th reuse. The red arrows indicate the observed martensitic microstructure. (For interpretation of the references to colour in this figure legend, the
reader is referred to the web version of this article.)

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J. Li et al. Powder Technology 441 (2024) 119815

showed that the volume fraction of silicon phase increased, and basically during the PBF process. For example, in Fig. 7, internal pores in PBF-EB
covered the aluminum matrix. X-Ray Diffraction (XRD) patterns of the recycled powder could be crushed after repeated cycles [43], and voids
condensate powder showed that the lattice constant of α-Al phase in PBF-LB recycled powder were non-spherical, taking on more elon­
decreased and the peak value of α-Al phase shifted slightly to the right gated shapes [46]. This highlights the potential challenges and com­
due to the precipitation of silicon phase from the matrix (see Fig. 6). plications when reusing powder in PBF processes, as these defects can
It is important to note that the microstructure variation of the impact the overall quality and performance of the final printed parts.
recycled powder are affected by the cycling times and the volume
fraction of reused powder. The volume fraction of coarsened particles, 3.4. Surface hardness of the recycled powder
spatter, and condensate particles in the recycled powder increases with
the cycling iterations. Consequently, significant phase structure changes The surface hardness of the powder particles has an impact on the
occur when the volume fraction of spatter and condensate particles in particle interactions during spreading. The higher surface hardness of
reused powder is large. Therefore, different results can be obtained the reused powder can increase the repulsive forces between the powder
when there are few coarsened powder and spatter particles in the particles, thus reducing the tap density of the powder bed [21]. The
recycled powder or fewer cycling times. Gorji [25] investigated the surface hardness of the recycled powder varies with the changes of its
phase and crystallinity of PBF-LB/M/316 L recycled powder through surface chemical composition and microstructure. For example, in the
XRD analysis, detecting that all peaks were austenitic phase with FCC case of PBF-EB/M/Ti6Al4V powder, an oxide layer forms on the surface
structure and no change in phase. He suggested that reusing powder >10 of the recycled powder, leading to a noticeable increase in surface
times has an impacts on the microstructure of the recycled powder, hardness. As shown in Fig. 8, after 10 cycles, the oxide layer on the
while less reuse is not obvious. surface becomes thicker, the particle surface roughens, and the surface
In addition to microstructure and phase structure changes, internal hardness enhances correspondingly. The formation of titanium oxide,
microscopic defects can also occur in the recycled powder. Internal aluminum oxide, and iron oxide on the local regions of the surface can
cavities are easily generated in the recycled powder with larger particle be considered as the main reason for these changes. Furthermore, the
sizes. The reasons for these microporous primarily come from three thickness of the oxide shell layer and the degree of surface hardening
aspects: entrapped gas in the melt pool trapped in spatter particles, voids increase with the cycles [42].
formed by unfused particles, and voids in partial melted agglomerations Similar results have been realized for PBF-LB recycled powder. In the
of particles [28]. Moreover, the shape of gas pores can be distorted PBF-LB/M/316 L process, after thirty reuses, with the increase of the

Fig. 6. Cross sectional SEM images of the AlSi10Mg powders [45]. (a) and (d) virgin, (b) and (e) condensate powder, (c) and (f) recycled powder, (g) XRD patterns.

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J. Li et al. Powder Technology 441 (2024) 119815

Fig. 7. Cross-sections SEM images of the powders in different processing states. (a)- (c) is the PBF-EB/M/ Ti6Al4V powders [42], (d) and (e) is the PBF-LB/M/MS1
powders [46]. (a) surface connected pore after 1 cycle, (b) internal pore after 30 cycles, (c) crushed pore after 30 cycles, (d) the cavity in the virgin powder, (e) the
elongated pore in the reused powders, respectively.

and magnetic moment [21]. The primary reason for this is the phase
transition, which alters the magnetic behavior of the recycled powder
[33]. The increase of δ phase content in the recycled powder leads to a
decrease in coercivity, indicating less resistance to magnetization
changes [21]. Pinto [18] investigated the phase structure of PBF-LB/M/
316 L powder after 16 cycles and found that the recycled powder had
about 6 vol% of δ phase compared to the whole γ phase of the virgin
powder, thus increasing the magnetism. In the PBF-LB/M/ATI 718
process, recycled powder also exhibited soft magnetic behavior, pri­
marily due to the presence of surface films and oxide spots [47].
It is essential to note that the mean size of magnetic particles is finer
than non-magnetic powder particles. Furthermore, the ferromagnetic
interaction can drive the clustering of magnetic particles more serious
Fig. 8. Schematic diagram of surface microstructure changes of PBF-EB/M/
[18]. This can lead to the formation of grooves and voids defects during
Ti6Al4V powder [39]. (a) Virgin particle having a native oxide layer, as
shown with red arrows. (b) Oxides formed on local regions of the reused
powder spreading, resulting in non-uniformity of the powder bed layers.
powder surface after 10 cycles. (For interpretation of the references to colour in As a result, laser beam turbulence and melt pool instability are inten­
this figure legend, the reader is referred to the web version of this article.) sified, affecting the quality of the built parts. However, the attractive
magnetic interaction of the particles can be weakened when the heating
thickness of thin SiO2 layer on the recycled powder from 3.7 nm to 79.5 temperature is higher than the Curie temperature (TC) during recycled
nm, the average Vickers hardness correspondingly enhanced from 2.56 powder post-treatment, and the ferromagnetic particles are transformed
GPa to 2.97 GPa [21]. The surface hardening mechanism in PBF-LB into paramagnetic ones, which enhance the powder flowability [18].
process is similar to that of PBF-EB process, which is related to the Finally, we can use Hiden’s findings to summarize the formation of
ingress of the oxygen and the formation of the oxides on the surrounding the recycled powder and the evolution of the characteristics, seen the
of the recycled powder [42]. Fig. 9. This diagram clarifies the interaction between the laser with the
powder and the melt pool, reveals the formation mechanism of spatter
and condensate particles, identifies the source and constituents of
3.5. Other characteristics of the recycled powder recycled powder, and explains the variations in particle morphology,
chemical composition, and microstructure and phase structure. The
Research on the characteristics of stainless steel recycled powder complex thermal history during PBF process can lead to changes in
showed that the magnetic properties changed with reuse, which per­ metal powder characteristics and even degradation, which has been
formed as an obvious improvement in powder magnetic susceptibility

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J. Li et al. Powder Technology 441 (2024) 119815

Fig. 9. Particle-laser interactions and the changes of powder characteristics in the PBF-LB/M/316 L process [21].

generally accepted by current literature. Gaining insight into the evo­ reduced apparent density and tap density [49]. The conflicting results
lution behavior during the PBF process and finding ways to avoid or may be related to the material intrinsic properties, the PBF process and
slow down the degradation of metal powders will be the focus of future process parameters, even the means of characteristic measurements.
research. In addition, it is also necessary to pay attention to variations in
spatter particles, oxygen content, moisture, magnetism, and surface
4. Characteristics of the reused powder bed hardness of the reused powder. Powder degradation caused by these
factors will inevitably be detrimental to the flowability, spreadability,
4.1. Influence on the flowability, spreadability and bulk density of the and tap density of the reused powder bed. The first contaminant is the
reused powder bed growing oxide layer on powder particles, as well as spatter, condensate
and its accumulation during successive PBF processes. The growing
It is well known that powder bed characteristics are governed by the oxide layer enhances the surface hardness of the reused powder and
powder characteristics. Therefore, variations in the characteristics of impacts particle interactions during spreading, thus reducing the pack­
reused powder will certainly affect the flowability, spreadability, bulk ing density of the powder bed [21]. Besides oxides, liquid bridges be­
density, and other characteristics of the powder bed. However, with the tween the particles can be generated due to the moisture and other
build cycles of the reused powder, the degradation on the particle shape gaseous constituents present on the powder surface, which contribute to
does not necessarily have a bad effect on the spread of the powder bed. adhesive forces and agglomeration, thereby decreasing the flowability
Instead, it shows the enhancement in the flowability and spreadability, and tap density of the powder bed [50]. The third factor is the magne­
and the decrease in the tap density. The reason is that the PSD plays a tism enhancement caused by the variation of phase structure in the
more dominant role in the flowability behavior than irregularly shaped reused powder. The improvement of magnetism leads to the decrease of
particles [22]. The shift of the PSD to the coarsen particles and the the flowability and the subsequent formation of grooves and voids in the
reduction of the finer particles usually lead to an increase in fluidity and powder bed, resulting in a lower tap density of the powder bed [18,19].
a decrease in bulk density. Nevertheless, different materials have In the subsequent building process, the degraded characteristics of the
different effect degree on these properties. Cordova [22] measured the powder bed can cause an unstable melt pool behavior and create a vi­
characteristics of Inconel 718, Ti6Al4V, AlSi10Mg, and Scalmalloy to cious cycle of powder degradation.
determine the impact of powder reuse on the flowability, true density,
and tap density changes of the reused powder bed. The results showed 4.2. Influence on the thermal properties of the reused power bed
that AlSi10Mg appeared to be the most sensitive to reuse, followed by
Inconel 718; in contrast, Ti6Al4V showed the lowest influence. In the In general, the heat conduction during PBF process mainly depends
case of Scalmalloy, the changes were negligible. on the structure of the powder bed rather than the thermal conductivity
However, it is worth noting that due to powder characteristics being of the material, which is more controlled by the porosity of the powder
subject to various parameters, conflicting results can be obtained in bed. Since the porosity of the powder bed is determined by the char­
other studies. Tang [23] revealed that there was no change in the acteristics of powder such as the morphology, PSD, surface composition,
apparent density, while the tap density gradually decreased in PBF-EB/ and particles surface hardness, variations in these characteristics inev­
M/Ti6Al4V powder. Boley [48] reported that both the apparent and tap itably affect particles flowability and the filling of inter-particle voids,
densities increased simultaneously with reuse in PBF-LB/M/AlSi10Mg which ultimately impact the absorption and heat conduction of the
powder. Nevertheless, the reused PBF-LB/M/316 L powder had a powder bed.

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J. Li et al. Powder Technology 441 (2024) 119815

As for the effect of particle size and PSD, blending fine particles with deterioration phenomena of degrading reused powder [7,29,35,and]. In
a broader PSD can provide beneficial effects towards improving powder fact, establishing the relationship between powder characteristics, pro­
packing density. Moreover, the higher the concentration of fine powder, cess parameters and product quality is a huge project, which requires a
the higher the probability of particle surfaces being irradiated, which is lot of work. At present, the results are relatively limited, and no mature
conducive to increasing the number of particles under beam irradiation conclusions can be copied. However, the following conclusions can still
and enhancing beam absorption. However, excessive blending of fine be summarized from current literatures.
particles could introduce drawbacks on flowability due to the incense­
ment of powder cohesion and inter-particle forces, which is not favor­ (1) The variation of the reused powder particles size and PSD. In
able for packing density, absorption, and heat transfer. In general, the general, much coarser particles with narrow PSD can decrease the
bimodal powder exhibited a higher tap density compared to Gaussian packing density of the reused powder bed, which leads to forming
grades and also obtained higher energy absorption [48]. a small and shallow melt pool [29,44,54,and]. Correspondingly,
Zhao [51] and Yang [52] studied the influence of powder sphericity the input energy density should be adjusted to increase. On the
on energy absorption in the PBF process. Non-spherical powder particles other hand, the packing density of reused powder bed increases
changed the incident angle of the energy beam, leading to multi- with the wider PSD and the amount of fine particles, which is
reflection phenomena due to higher roughness of the particles, which beneficial to the absorption and heat transfer, thereby forming a
improved energy absorption. Sartin [6] showed that as the amount of wide and deep melt pool [19,32]. However, the large amount of
crushed particles and irregular particles increased, the scattering rate of fine powders in the reused powder leads to high bulk density and
the powder bed decreased, thus yielding higher values for absorptivity. high thermal conductivity of the powder bed, resulting in a high
However, the powder bed formed by the imperfect spherical powder had temperature and a steep temperature gradient of the melt pool
lower packing density and fluctuating energy absorption. Therefore, [11,54]. When optimizing the subsequent process parameters, it
excessive melting in the partial powder bed can be occurred, which can is necessary to reduce the input energy density and adjust the
lead to an unstable melt pool flow that promotes the formation of defects scanning strategy. Liu [55] reported that better 316 L part
in the built parts. densification resulted in the wider distributed powder at scan
The effect of chemical composition on thermal properties of the rates >150 mm/s, while the narrower grade performed better at a
powder bed is mainly reflected in the oxide layer of the powder particles. slower scan speed (100 mm/s) in PBF-LB process.
The increase in oxygen content of the recycled powder and the presence (2) The variation of reused powder morphology. Generally, the
of the ejected particles can lead to a certain thickness of oxide films amount of non-spherical powders in the reused increases with the
surrounding powder particles. The energy transport between powder build cycles. The non-spherical reused powder is detrimental to
particles varies with the different heat transfer coefficients of oxides the packing density and the thermal conductivity of the layer,
phase. The change of the laser absorption of the spatter particles is indicating that the energy absorption rate of the reused powder is
probably due to its surface condition. For example in the PBF-LB/M/ lower than that of the virgin powder. Meanwhile, the energy
Inconel 718 reused powder, owing to the enhanced oxygen content absorption of the irregular powder is usually fluctuating, which is
and the Al2O3 films formed on the localized particle surfaces, the laser difficult to guarantee the stability and continuity of the melt pool
absorption rate for the entire available wavelength spectrum (900–1100 [10,11,15,and]. For example, at lower energy density (64 –84 J/
nm) increased from 68.8% to 76.1% compared to the virgin powders mm3), spherical powder produced denser 17–4 PH specimens
[28]. The same result was observed in PBF-LB/M/Inconel 625 powder, than the irregular powder in PBF-LB process. Nevertheless, when
where surface oxidation caused an increase in laser absorbance from enhancing energy density (≥ 104 J/mm3), part density was in­
0.40 to 0.86 [53]. dependent of the powder morphology [54].
In conclusion, the characteristics of the reused powder have signif­ (3) The variation of contaminants in the reused powder. Reused
icant effects on the thermal properties of the powder and powder bed, powder usually contains some oxide phase, which can be present
including energy absorption, packing density, and melt pool stability. A either as an individual particle or as the oxide films surrounding
better understanding of these relationships is essential for optimizing the surface of the particles. It is generally assumed that a high
the PBF process and ensuring high-quality parts are produced. amount of oxide content degrades the packing density of the bed
layer as well as the energy absorption. Meanwhile, it can enhance
5. The process parameters and the parts quality of the reused the melting point of the reused powder particles, thereby result­
powder ing in incomplete melting of the particles. At this point,
enhancing energy density is required to ensure full melting
5.1. Selection and optimization of process parameters for the reused [10,54]. But on the other hand, the oxide phase can also improve
powder the energy absorption rate of the powder particles. Therefore,
only increasing energy density can only strengthen the interac­
In general, the characteristics of powder and powder bed play an tion between the energy beam and the melt pool for a long time,
important role in determining the selection and optimization of the creating the excessive melt pool temperature and larger gradient
process parameters. Previous work has shown that the energy absorp­ that may further lead to higher residual stresses accumulated in
tion and transmission are affected by the change of the characteristics of the solidified part. In this case, removing the oxide phase from the
powder and powder bed [17,21,48,51,and]. So, it can be expected that if reused powder, or not use too high energy power and too low
the process parameters did not change with the characteristics of the scanning rate is the recommended process parameters [48,54,56,
reused powder and powder bed, but kept the static parameters in the and].
successive manufacturing procedure, the consistency and stability of the
melt pool would be destroyed, resulting in the variations of product In short, with the increase of the build cycles and the variations of the
surface roughness, microstructure, mechanical properties and other reused powder characteristics, the appropriate adjustment of the process
qualities [21,23]. parameters is conducive to the stability of the operation and slow down
Up to that point, it is essential that the operator must be familiar with the degradation of the parts quality. However, it cannot be simply
the characteristics of the reused powder prior to each operation, and deduced that as the build cycle increases, the energy density is mono­
then appropriately adjust the process parameters for the specific pow­ tonically increasing or decreasing. In practice, when establishing the
der. The purpose of readjusting the process parameters is to ensure the process parameters, we must consider not only the single effect of the
formation of continuous and stable melt pool, and weaken the characteristics but also the comprehensive characteristics of the reused

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J. Li et al. Powder Technology 441 (2024) 119815

powder. transfer efficiency, allowing faster cooling rate ability associated with
the finer microstructure of the parts. Averyanova [67] compared the
5.2. The influence of the reused powder on the parts surface quality effect of powder size on the microstructure of 17–4 PH parts, where the
martensitic phase content of fine powder (38 vol%) was higher than that
Most PBF parts appear a stair-step structure due to the characteristics of coarse powder (6 vol%). Another study by Olakanmi [68] reported
of layer-by-layer forming. Thus, Mumtaz [57] highlighted that the that the bimodal Al-Si powder due to exhibited high heat dissipation
roughness of the top surface perpendicular to the build direction is capability achieved the refined dendritic feature. However, excessive
mainly generated by the rippling motions of the melt pool, while the side fine particles instead lead to quicker melting and prolong the life of the
roughness parallel to the build direction may be the result of melt melt pool, resulting in coarser grain structures. In addition, as the
segregation to the layer edges under the effects of Marangoni convection degraded particles occupied a relatively high proportion in the reused
and surface tension. Tan [54] indicated that in order to achieve the powder, the low packing density led to poor thermal conductivity,
smoother surfaces, sufficient laser energy density should be inputted to resulting in slow cooling rate and relatively coarse grain [69].
flatten the melt pool and enhance the wettability and spreadability of Nevertheless, when there is no significant difference in the charac­
the melt pool. Therefore, it can be deduced that the surface quality of teristics between the virgin and reused powders, the effect on the
PBF parts is determined by the melt pool behavior, and any factor microstructure can be negligible. Sun [70] found that after mixed 15 vol
affecting its behavior is related to the surface roughness. % virgin powder with the reused powders, the maraging steel exhibited
In terms of the powder and powder bed characteristics, the surface similar microstructure with that of virgin powders after 113 building
quality of PBF parts is mainly affected by the powder shape, the spatter cycles. In addition, the influence of reused powder characteristics on the
or the oxide particles and the powder packing density [54]. Corre­ microstructure of parts is also related to the inherent properties of ma­
spondingly, the parts surface quality will gradually decline with the terials. Tan [54] suggested that subtle changes in the microstructure
successive degradation of the reused powder. In general, finer particles affected by powder characteristics are easier to be observed in materials
contribute to be more fully melted and generate a stable smoother melt with better thermal conductivity, such as Al alloy, Cu alloy and W alloy.
pool surface, thus producing better surface quality [58]. So, in practice, Overall, although there is no consensus on the degree of relationship
it is recommended to add finer particles during configuring reused between the reused powder and the microstructure of parts, due to the
powder to reduce the stair-stepping effects and ensure surface quality strong affinity between the process cooling rates and the thermal
[59]. Furthermore, a wider PSD with fine powder can produce parts with properties of the powder, any factors to the thermal properties and the
better surface quality than that of a narrower PSD powder [55]. How­ amount of reused powder should be paid attention to before re-mixing.
ever, when building parts with an overhang structure, fine powder may Another important factor affecting the microstructure of products is
have a chance to produce the defect of burn-on sand and result in the chemical composition, phase structure of the reused powder. The
rougher surface owing to the heat accumulation effects [60,61]. In presence of oxide films enhanced the laser absorptivity, correspondingly
addition, the spatter and oxide particles in the reused powder needs to created a steeper thermal gradient in the melt pool, which generated a
be emphasized because it contributes to elevate melt pool oxygen con­ greater degree of undercooling for rapid solidification, resulting in finer
tent, which can form an oxide film on the surface of the melt pool to grain size in Fe parts [71]. For the 17–4 PH products manufactured by
reduce the wettability and spreadability of the melt liquid, thereby the PBF-LB process, when nitrogen atomized powder is used or nitrogen
eventually producing rougher surface. Moreover, spatter particles can is used as an inert gas in the chamber for manufacturing, the final parts
fall back into the melting region and may deposit over the previously contains most of the austenite structure (>96 vol%) due to the strong
formed melt track, increasing the roughness of the melt track [34]. austenization of nitrogen element [26,72]. Averyanova [73] studied the
Furthermore, the rougher melt tack decreased flowability of the powder effect of the chemical composition and phase structure of powders on
while easily causing inconsistent spreading of the powder bed and, the microstructure of PBF-LB/M/17–4 PH steel products. Although the
subsequently, of the inferior surface roughness [51]. virgin powder is in the full martensitic phase, high austenitic stable el­
In terms of the influence of PBF process on the surface quality, PBF- ements (4.06 wt% Cu, 3.42 wt% Ni) make it possible to manufacture
LB and PBF-EB follow the same rules due to the successive degradation parts with 62 vol% of residual austenite. While, when manufactured by
of the reused powder. For Ti6Al4V, a significant increase in the surface the powder with 86 vol% austenite, the microstructure of the final
roughness in parts fabricated with the reused powder was observed products is composed of 94 vol% austenite and 6 vol% martensite. In the
[62,63]. Studies conducted on PBF-LB/M/316 L components showed PBF-EB/M/Ti6Al4V samples after recycled 30 times, because the oxygen
that the reused powder after 6 cycles produced rougher components content of the reused powder increased linearly from 0.14 wt% to 0.36
[64,65]. For the Al-Mg-Sc-Zr alloy processed by PBF-LB, the surface wt%, the basketweave structure of the final part was obviously coars­
roughness (Ra) increased from 28.6 ± 3.8 μm to 30.8 ± 3.3 μm after 4 ened. That is, the alpha lath width increased, while the prior beta width
building cycles [66]. remained approximately constant [74], as shown in Fig. 10.
It is particularly important that not to ignore the effect of spatter and
5.3. The influence of the reused powder on the parts microstructure oxide particles on the microstructure of the fabricated parts. Since
spatter ejection occurs on the surface of the melt pool, the floating ox­
In the PBF process, the effects of the reused powder on the micro­ ides are picked up. They then stay on the surface of the liquefied droplet
structure of parts are firstly reflected by the thermal property variations and solidify, forming significantly thicker oxide layers [14,31]. Soun­
of the powder bed, where heat absorption and heat conduction deter­ darapandiyan [75] reported that when spatter and oxides particles
mine the geometrical characteristics and the solidification behavior of participate in the PBF-Ti6Al4V parts, oxygen could first dissolve into the
the melt pool, ultimately having an impact on the microstructure of the Ti matrix wherein the oxygen can occupy the octahedral interstitial and
product. On the other hand, as previously mentioned, the reused powder cause strain in the c-axis of the hexagonal close-packed crystal lattice.
covers a certain amount of heat-affected zone powder, spatter and Furthermore, oxygen is also an alpha phase stabilizing element in
condensate particles. The dissimilar thermal histories that individual Ti6Al4V, and it tends to randomly segregate at the grain boundaries,
particles experienced during production render deviations in the acting as a solid solution strengthener, hindering the gliding of dislo­
microstructure and chemistry, which can also potentially affect the cations, leading to an intense hardening.
microstructure of the products.
The particle size and PSD of the reused powder have a certain effect 5.4. The influence of the reused powder on the parts defects
on the grain size and phase structure of the products. It has been
confirmed that a broader PSD with fine particles can obtain higher heat Previous mentioned that the degradation of the reused powder can

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J. Li et al. Powder Technology 441 (2024) 119815

Fig. 10. Microstructure of the PBF-EB/M/Ti6Al4V samples. Exemplar beta ribs were noted with arrows [74].
(a) for the virgin powder, (b) for the reused powder.

potentially impact the manufacturing process parameters, as well as the types and sizes of defects increased. Tiny and smooth pores gradually
melting of powder particles, the formation, spread and solidification of developed into the enlarged pores defects due to the interconnection of
the melt pool, thereby possibly leading to the emergence of defects in the micro-voids. Meanwhile, the size and number of irregular voids obvi­
final products. The defects can be summarized as follows: gas pores, ously emerged and increased in the sample, and some of unmelted
lack-of-fusion, balling phenomenon, delamination, spatter, inclusion, particles also began to appear gradually with reuse. In addition, also
and microcracks [76]. notes that owing to the presence of moisture and other gaseous con­
As the further understanding of the relationship between defects and stituents on the reused powder surface, the ionization during operation
the characteristics of powder gradually strengthens, researchers and can cause them to deliver a significant amount of gas. As a result, the gas
manufacturers have recognized that the formation of various defects is content was supersaturated in the melt, and the porosity in the final
mainly controlled by the behavior of the melt pool, with the charac­ products such as lack of fusion and gas pores increased from 1 vol% to 3
teristics of the powder and powder bed being important factors [77–79]. vol% [35].
Moreover, the degradation of the characteristics of reused powder has a Currently, voids defects such as gas pores and lack-of-fusion are
detrimental influence on the interaction between the energy beam, recognized as one of the common defects in PBF parts. Researchers
powder and melt pool, especially for the stability of the melt pool outlined that the formation of voids defects is mainly controlled by the
[80,81]. Thus, the types of defects and the probability of defect occur­ behavior of molten pool, and the characteristics of powder and powder
rence increase correspondingly with the amount of the reused powder bed are one of the important factors [76–78]. The first is related to the
and the building cycles [82–84]. Wang [85] studied the influence of gas content of powder and the packing density of powder bed. Higher
powder reuse times on the defect types and sizes in PBF-LB/M/CoCrW gas content and the lower packing density of the degraded powder tend
alloy samples (see Fig. 11). As the reuse times increased to sixth, the to resulting in higher gas present between powder particles, which may
be further dissolved in the molten pool. Because of the supercoiling rate
during the solidification process, some dissolved gas cannot escape from
the molten pool before solidification, thus forming the entrapped gas
pores in the fabricated parts. The second reason attributes to the powder
granulometry and PSD. It suggested that higher tendency for finer par­
ticles as well as narrow PSD at high energy density easily induced higher
temperature molten pool and higher gas solubility in the liquid metal
which likely initiated keyhole melting and porosity upon solidification
[4]. On the contrary, larger particles would require longer periods to
achieve complete melting which reduced the probability of vaporization
and gas pores [54]. Spatter and oxidized particles contribute to the third
forming mechanism of the porosities. One is that the enhancement of the
melting point by the oxides leads to unmelted particles at the insufficient
energy density, causing pores defect. Especially, if there exists unmelt
particles between scan tracks, defects of insufficient overlap, delami­
nation or lack-of-fusion will be formed and remained in the final parts
[84]. In addition, the high melting point of the oxide means high vis­
cosity and lower temperature liquid melt, thus having the poor flow­
ability and the spreading ability of the molten pool. As a result, defects of
poor bonding or lack-of-fusion can be generated in the final parts
[35,75]. Another detrimental influence is that the increase of oxygen
content in the melt liquid changed the kinetics and solidification
behavior of the molten pool. The wetting ability of the molten pool
would be considerably limited due to the appearance of the surface
oxidation and the consequent variation of the surface tension gradient.
As a result, the melt convection behavior was seriously changed,
restricting the efficient densification rate and resulting in the formation
of the interconnected and irregular pores defect [85].
Balling phenomenon is another common defect in PBF products. As
Fig. 11. The influence of powder reuse times on the defect types and sizes in
the temperature distribution throughout the depth causes the generation
PBF-LB/M/CoCrW alloy [85]. (a) first, (b) second, (c) third, (d) fourth, (e) fifth,
and (f) sixth.
of flotation forces, while the surface temperature distribution leads to

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turbulent flows. Flow instability can lead to Rayleigh instabilities, which lip systems. However, α lath thickness will increase with the rising of the
is sufficient to alter the temperature coefficient of surface tension from oxygen content in the reused powder, thus weakening the strengthening
negative to positive thereby changing the Marangoni convection from effect [74]. Therefore, the solid solution strengthening of the oxygen is
centrifugal to centripetal, causing the melt pools to break into droplets stronger than that of the microstructure with reuse times. Nevertheless,
known as the balling phenomenon [80]. Zhou [81] classified the balling it should be noted that the critical value of oxygen content in the reused
formation mechanism as the competition between the melt spreading powder shout be set around 0.33 wt%. Below the critical level, the in­
and solidification. The characteristics of the powder and powder bed fluence of oxygen on ductility is insignificant; while, beyond this value,
play an important role in the balling phenomenon. On the one hand, the the ductility drops sharply [23]. In addition, with powder reuse, the
increase of oxygen content in the reused powder and the formation of variation of mechanical properties also has a great relationship with the
surface oxides changed the surface tension of the molten pool, resulting building direction, especially the elongation shows a strong anisotropy,
in centripetal Marangoni convection in the molten pool and resulting in while the strength, elastic modulus and work hardening rate are less
balling defects. On the other hand, the prolonged utilization of powder affected [62,74]. Schur [62] confirmed that the elongation reduction in
increased the proportion of the non-spherical and irregular particles in the horizontal direction was 1.5 times than in the vertical direction;
the reuse powder, which reduced the packing density and heat transfer while, the elastic modulus and strength difference between horizontal
so as to form the small size melt pool, thus easily solidifying into balling and vertical directions fluctuated only around 2–3%.
particles [82]. Compared with Ti6Al4V powder, Inconel 718 powder is less affected
In general, PBF technology typically leads to the formation of a high by the thermal histories because of its slow sintering behavior and
temperature gradient and rapid cooling rate. Furthermore, the influence resistance to picking up oxygen [47,91,92]. Hence, the effect of reused
of non-uniform thermal expansions and contractions in the vicinity of powder on mechanical properties is relatively slight. This has been
the energy irradiation region can contribute to the formation of residual confirmed by Ardila [93] and Paccou [94], which showed that even
stresses in the finished part [83]. The formation of residual stress is long-term recycling (up to 50 cycles), the mechanical properties of
related to the temperature field and stress field in the forming process, Inconel 718 did not significantly increase or decrease due to the little
and is greatly affected by the characteristics of the reused powder. Some change in the characteristics of the reused powder. In addition, Kim [95]
of the undissolved oxide compounds could substantially raise absorp­ investigated the environment-assisted fracture (EAF) behavior of
tivity and increase melt pool temperature, possibly creating larger gra­ Inconel 718 specimens made from reused powder by the PBF-LB process.
dients that may further lead to higher residual stresses accumulated in Powder recycling six times did not affect the EAF sensitivity. Yi [96]
the solidified part [48]. Similarly, excessive fine particles may have analyzed the effect of usage times on mechanical properties from the
induced quicker melting and higher melt pool temperature, which can relationship between defects and mechanical properties. Although the
prolong melt pool life and generate the steep temperature gradient at the defects of spherical small pores increased with reuse, these defects were
edge of the molten pool, thus inducing huge thermal stress, residual beneficial to promote a more homogeneous deformation and reduce
stresses and eventually causing the generation of micro-cracks [76]. stress concentration during the plastic deformation process, thus coun­
teracting the adverse effects of the rising porosity and having little effect
5.5. The influence of the reused powder on the parts mechanical on the room-temperature tensile properties of PBF-LB/M/Inconel 718
properties parts. Hann [97] suggested that the increased oxygen content in the
reused powder can be released by the interaction of the laser heating
The changes in the characteristics of reused powder not only have an during preparation, and not all of it is trapped in the sample due to rapid
impact on the product’s performance in terms of microstructure, defects, solidification. In other words, as long as the increase in oxygen associ­
and surface roughness, but also affect the mechanical properties of the ated with reused powder is not realized in the final product, no signif­
final parts [86,87]. Table 1 summarized recent literatures on the icant change in mechanical properties can be observed. However, when
comprehensive effects of powder reuse on the powder characteristics residual oxygen in the final product is present in high levels, another
and mechanical properties of various materials in the PBF process. view arises. LPW Technology analyzed the effect of PBF-LB/M/Inconel
Nevertheless, due to the multiple complex influences of PBF process 718 powder degradation on mechanical properties, due to an increase
parameters and the intrinsic properties of materials on the characteris­ in oxygen with each reuse, there was a significant increase in the ulti­
tics of the reused powder, the quantitative and qualitative relationship mate tensile strength (UTS) and a reduction in ductility from 20% to
between powder degradation and the microstructure of the product has 13% after 25 builds [98]. Bhowmik [99] attributed the higher strength
not been established at present. Hence, the same is true for mechanical and lower ductility to the higher dislocation density and more effective
properties, which cannot also be described by the same definition. dispersion hardening, including some oxygen-rich inclusions/disper­
In recent years, many researchers have investigated the influence of soids originated from reused powder through multiple heating cycles. In
powder degradation on the mechanical properties of the Ti6Al4V alloy. addition, Lee [100] found that due to the presence of oxides, the
As mentioned earlier, due to the unique intrinsic properties, most of the strength and elongation of Inconel 718 at room temperature and high
reused powder of Ti6Al4V either in PBF-LB or PBF-EB processes retained temperature were enhanced simultaneously with iteration numbers. The
the initial spherical morphology with the reduction of fine particles, increase of mechanical properties at room temperature was owing to the
showing good flowability and high packing density of the powder bed, enhanced work hardening rate and the hindrance of dislocation motion
except that the oxygen content in the reused powder increased linearly. by alumina dispersion hardening. At high temperature, with the increase
Correspondingly, there was an increase in strength and a decrease in of diffusion rate, the retardation effect of alumina on dislocation motion
ductility, such as elongation, impact toughness, and fatigue life with decreased, resulting in an almost constant elongation value.
powder reuse [23,24,37,42,56,63,76,88–90]. As for the reason, many Owing to the low melting point, high active chemistry, and low
researchers suggested that the rising oxygen content in the reused surface hardness, aluminum alloy powder appears to be the most sen­
powder and the variations in the microstructure of the final products are sitive to reuse, with changes in particle size, PSD, morphology, and an
the root causes for this change in mechanical properties. Furthermore, in increase in oxygen content during the PBF-LB process [41,101].
comparison, the strengthening effect of oxygen solid solution caused by Particularly, due to the high affinity with oxygen, spatter particles easily
the rising oxygen content in powder is higher than the effect of micro­ formed during the PBF-LB process, which can impair the high cycle
structure evolution. In the typical PBF-Ti6Al4V alloy, the microstructure strength since the higher concentration of Al2O3 particles can act as
consists of elongated prior β grains oriented along the build direction crack initiators during dynamic stress [102,103]. Fiegl [35] revealed
and a basket structure matrix composed of α and β phases, where α phase that due to the formation of hydroxides and oxides during the PBF-LB
has better strengthening effect than that of β phase owing to the limited process, after 30 months of long-term reuse, a decline of about 15% in

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Table 1
Effect of cycle times on the characteristics of the powder and the mechanical properties of the parts.
Process Materials Build Characteristics changes of the powder Typical variation in mechanical properties Ref.
cycles

PBF-EB Ti6Al4V 21 Oxygen increased from 0.08 wt% to 0.19 wt%. The powder YS and UTS increased from 834 MPa and 920 MPa to 960 MPa [23]
became less spherical and the PSD became narrower. The and 1039 MPa, respectively. Elongation slightly decreased
flowability of the powder improved. from 16% to 15.5%.
30 Oxygen increased from 0.142 wt% to 0.356 wt%. For the horizontal build direction, elastic Modulus increased [42,62,74]
Microstructures ranged from near-virgin martensitic alpha to from 98.9 GPa to 109.4 GPa. YS and UTS increased from 739
heavily coarsened alpha platelets with intergranular beta. MPa and 888 MPa to 1050 MPa and 1122 MPa, respectively.
Fines decreased and PSD narrowed. Deformed with surface Elongation decreased from 11.7% to 3.5%.
dimples and irregular shape increased. Alpha case surrounded
the powder.
10 Powder morphological degradation such as hard-sintering, A marginal increase of 10 MPa in YS and UTS. Elongation [88]
partial melting and agglomerations. PSD shifted slightly showed a negligible difference. The fatigue life decreased from
inwards at the finer side and outwards at the coarser side. 121,384 ± 14,128 cycles to 99,759 ± 8287 cycles.
Oxygen increased from 0.0 wt. 8% to 0.10 wt%. Recycled
powder particles was with α lath coarsening, β precipitation
and reduction of randomness in crystal orientations.
PBF-LB Ti6Al4V 31 Oxygen increased from 0.09 wt% to 0.13 wt%. Powder surface A slight increase in the tensile strength, elongation was from [29]
exhibited coarsening. A minor of elongated/irregular particles 13.8 ± 0.6% to 14.4 ± 0.5%.
were observed. Flowability improved, and tap density slightly
declined.
12 No provided data YS and UTS changed from 993.2 MPa and 1047 MPa to 1003.7 [63]
MPa and 1057.1 MPa. Elongation decreased from 11.6% to
7.7%. The fatigue strength declined.
9 Spatters and condensate particles increased. Slightly finer Recycling had a slightly increase on YS and UTS, did not [84]
powder created after each recycling, and PSD slightly widened. reduce the elongation. However, the impact strength values
Oxygen and nitrogen increased from 0.16 wt% and 0.028 wt% decreased by over 50% from 9.4 ± 0.5 J/cm2 to 4.0 ± 0.1 J/
to 0.18 wt% and 0.035 wt%. cm2.
18 Oxygen increased from 0.099 wt% to 0.126 wt%. PSD The mean hardness and tensile strength increased from 367.8 [89]
remained relatively stable. Flowability improved. Larger HV to 381.9 HV and from 947.6 Mpa to 1030.7 Mpa,
agglomerated spatter particles were present. Fine particles respectively, whereas the ductility reduced from 10% to 3%.
reduced. No change in shape.
18 Oxygen content increased by 14% from 0.14 wt% to 0.16 wt%. No modification to the tensile properties, but with a decrement [90]
Oxide layer with a thickness of up to 20 nm formed on the in the impact strength of 30% for vertical- and 12% for
powder surface. A small shift in PSD, no change in the horizontal stress-relieved specimens and 19% and 16% for
morphology. Flowability increased. furnace-annealed specimens, respectively
PBF-EB Inconel 30 Oxygen increased from 146 ppm to 312 ppm. Powder surface is Defect density, both oxide inclusions and lack of fusion [40]
718 covered by a relatively thin and homogeneous oxide layer. increased, which was detrimental to the mechanical
properties.
PBF-LB Inconel 14 The variation with respect to the particles size, PSD and shape Similar in terms of equivalent microstructure, porosity, and [93]
718 was <10%. Chemicals remained stable except for Ni and Nb. toughness.
50 Oxygen increased by about 85% from 0.054% to 0.1%. Little effect on the monotonous tensile behavior. In fatigue, no [94]
Average particle size increased slightly due to the presence of difference for higher stress, and a slight reduction for lower
spatters and satellites, and an increase in flowability. stress.
6 No data provided Decrease in electrochemical stability and the electrochemical [95]
resistance. The marginal increase in EAF sensitivity, and no
effect on EAFCP resistance.
14 Increase in apparent density and flowability, and no change in Little effect on the mechanical properties. UTS and YS are [96]
chemicals even the impurities. Larger than 45 μm particles around 1025 MPa and 750 MPa, respectively. Elongation
increased by 6 vol%. PSD shifted to the right side. ranges from 27% to 30%.
10 No apparent change in particle morphology, particles size and No apparent effects on the UTS, YS, elongation and Low cycle [97]
PSD. A gradual increase in oxygen from 151 ppm to 172 ppm. fatigue.
25 A little increase in oxygen with each reuse. Tensile strength increased, elongation decreased from 20% to [98]
13%.
12 No changes for composition of the major alloying elements. Tensile, compressive and creep strength is not substantial [99]
Oxygen content slightly increased and exceeded the change.
specification limit of 0.02%.
10 The average particle size increased by 5 μm. Agglomerated Creep tests showed that samples made of virgin powder last [100]
non-spherical powders were visible frequently. PSD shifted longer at 550 ◦ C and 600 ◦ C, while the samples of reused
towards left. The increased amounts of O ranged from 81 ppm powder last longer at 700 ◦ C. At 25 ◦ Cand 650 ◦ C, both the
to 200 ppm. Oxide spots on the powder surface by the thickness strength and elongation were enhanced simultaneously.
of f 470–780 nm.
PBF-LB AlSi10Mg 8 Tap density and the apparent density slightly increased. PSD YS and UTS decreased of 10 MPa. Elongation at break [27]
exhibited a slight leftward. Average particle size decreased, oscillated ~18%. High cycle fatigue decreased from 160 to
and chemicals remained stable. 145 MPa.
AlSi10Mg 30 Spatters increased by 3vol.%. The thickness of oxide layer Tensile and yield strength reduced by 15%. Elongation [35,36]
Mos. increased from 4 nm to 38 nm. Oxygen and hydrogen increased decreased from 3.3% to 2.9%.Vickers hardness decreased from
from 500 ppm to 1250 ppm and 80 ppm to 130 ppm, 108 HV to 96 HV.
respectively. A similar PSD and apparent density.
AlMgScZr 4 A rejuvenation step mixing 40% of virgin powder, no large UTS and elongation with virgin and reused powder are 565 [66]
differences in composition and morphology, only coarser PSD MPa, 13% and 537 MPa, 11%, respectively.
presented.
AlSi10Mg 96 h No change on the mean particle size. Notable shift to coarsen A significant deterioration of the mechanical properties, YS [102]
particles of PSD. No significant change of powder shape and and UTS in vertical direction decreased from 171.7 MPa and
packing densities. Oxygen increased from 0.067% to 0.257%.
(continued on next page)

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J. Li et al. Powder Technology 441 (2024) 119815

Table 1 (continued )
Process Materials Build Characteristics changes of the powder Typical variation in mechanical properties Ref.
cycles

Ejected spattered emerged, and oxide layer formed on the 269.7 MPa to 150.3 MPa and 229.3 MPa respectively,
powder. elongation decreased from 7.1% to 3.4%.
AlSi10Mg 1 Fine particles decreased. PSD widened and flowability Comparable mechanical properties, no notable influence of the [103]
improved. exposure to corrosive environment on the mechanical
performance.
PBF-LB 316 L 12 No significant change in particles size and shape. Fine particles No consistent trend in strength and ductility. [6]
decreased with an increase of larger particles. No change in
flowability and density. Ejected particles increased. No
statistical trends in the chemicals.
316 L 30 Minor changes to PSD, bulk composition, and hardness, but Minor changed in UTS and YS, slight increase in ductility. [21]
significant changes to particle morphology, microstructure,
magnetic properties, surface composition, and oxide thickness.
316 L 6 PSD widened, and large particle size increased. A reduction in the UTS and Young’s modulus. [64]
304 L 5 Fines decreased, particles coarsened, and PSD slightly narrow. Tensile properties did not change. The impact toughness [105]
No discernible changes in the chemicals except the increase of showed a steady decline.
oxygen content from 0.026% to 0.032%. Condensate and
spatter increased.
316 L 15 More agglomerates and irregularly shaped particles increased. Similar tensile properties and micro-hardness because of grain [106]
PSD shifted towards larger. No significant difference in refinement, more numerous and finer grains coming from the
chemicals, but oxygen increased from 475 ppm to 675 ppm. oxide spatters acting as nucleation sites.
Larger oxidized spatters increased, δ-ferrite (4 wt%) appeared
in the reused powder.
No significant changes in particle size, PSD, and particle shape. Similar mechanical properties include tensile properties,
17–4PH 11 [32]
Apparent density and powder bed density increased elongation, the elastic modulus and hardness.
PSD narrowed. Particles size decreased from 30.8 μm to 28.4 No significant variation in tensile properties including yield
17–4 PH 15 μm. Fine particles decreased from 9 vol% to 6 vol%. No and ultimate tensile strengths. Elongation slightly increased. [107]
apparent change in shape. Bulk and tapped densities increased. Fatigue behavior was insensitive to powder reuse.

tensile strength and yield strength was observed as well as the reduction Another is to intensify the recycled powder separation process to ensure
of 12% in the elongation. Del Re [27], reusing AlSi10Mg throughout any detrimental impurities be removed before each building. For
eight build cycles, revealed a decrease of 10 MPa in the yield strength example, Pinto [18] advised that heat treatment above the Curie tem­
(YS) and UTS, and a decrease of 15 MPa in the high cycle fatigue. perature could eliminate the magnetic behavior of the reused powder,
Nevertheless, when the number of powder cycles is fewer or a rejuve­ thus decreasing the propensity to defect formation and damage to the
nation procedure is carried out, the detrimental effect of the reused mechanical properties. By employing a sieving process to remove the
powder on mechanical properties can be mitigated. Barile [104] majority of degraded powder, Sartin [6] found that there was no
confirmed that with only one cycling time, the slight degradation of the consistent trend in mechanical strength and ductility relative to powder
reused powder did not significantly affect the mechanical properties of reuse for up to twelve cycles in PBF-LB/M/316 L products. Recycled
the PBF-LB/M/AlSi10Mg samples. Even when the samples were exposed powder sieving processes were also used by Delacroix [106], and no
to the corrosive environment of dense saltwater fog for up to 1000 h, significant difference was shown in the microhardness and tensile
there was no considerable effects of the powders reuse on the corrosion properties of the PBF-LB/M/316 L components after 15 cycles. The same
behavior of the specimens. Additionally, after Al-Mg-Sc-Zr reused effect of reused powder is observed for 17–4PH steels. Because no sig­
powder treated by sieving procedure and a rejuvenation step mixing 40 nificant changes in reused power characteristics after recycled 11 times,
vol% of virgin powder, the mechanical properties remained unchanged the mechanical properties of the samples manufactured with the virgin
after four successive cycles [66]. and reused powders are similar [32]. Furthermore, in the PBF-LB/M/
Normally, the microstructure of stainless steel is composed of more 17–4 PH process, after removing all spatters and breaking down ag­
complex phases. Moreover, there are not only liquid phase trans­ glomerates in the reused powder, specimens fabricated from powder
formations but also solid phase transformations during the PBF forming reused 14 times had better fatigue strength in the high cycle regime than
process. Hence, the investigations of stainless steel sometimes provide those of virgin powder [107].
conflicting results with other materials [44]. It is stated that PBF-LB/M/
316 L and 304 L stainless steel reused powders show a shift towards a 6. The determination method of the reuse times and powder
higher percentage of larger particles with a wide PSD, thus having a reusability strategies
significant negative effect on the mechanical properties of the produced
component due to the increased porosity creating weak points. Testing 6.1. The determination method of the reuse times
conducted by McGeehan [64] showed a reduction in the UTS and
Young’s modulus in 316 L stainless steel as the powder was reused 6 It has been reached the consensus that the variation of main char­
times. Sutton [105] revealed that after recycling 304 L stainless steel acteristics such as morphologies, particle size, PSD, and chemical
powder for 5 times, tensile properties did not change, while the impact composition is inevitable during PBF successive operations. However,
toughness showed a steady decline. Heiden [21] investigated the me­ even for the experienced powder feedstock, such as Inconel 718 or
chanical properties of 316 L stainless steel with degradation of powder Ti6Al4V, how many times the reused powder can be built, even stan­
during the PBF-LB process. After thirty powder reuses, the mechanical dards in ASTM F3055 (2014) for AM in PBF do not offer official
properties decreased reasonably with the degradation of reused powder. guidelines [32]. To avoid manufacturing interruption and quality
In practice, two practical approaches can be carried out to mitigate the degradation, it is necessary to take measures to evaluate or grade the
adverse effects of reused powder on the mechanical properties of the reused powder before the next building, rather than at the end of
final product. The first method is to adjust and optimize the process production.
parameters in time according to the reused powder characteristics, Cordova [22] proposed a relatively practical decision to determine
thereby stabilizing melt pool and reducing the generation of defects. whether the reused powder can continue to be used, which is shown in

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J. Li et al. Powder Technology 441 (2024) 119815

6.2. Strategies for enhancing the powder reusability

Up to now, a so-called regeneration or reconditioning technology

enhancing powder reusability has been offered in AM fields, meaning
that the reused powder can be rejuvenated or brought back to its initial
characteristics [108]. However, the treatment effect of powder reus­
ability is affected by numerous factors such as the intrinsic properties of
powder feedstock, degradation degree of the reused powder, process
parameters, and handling techniques. Therefore, the premise of the
reusability treatment effect is that the reused powder can ensure smooth
operation in the next building and no continuous degradation in product
quality. Based on this, the strategies for enhancing powder reusability
can be summarized as follows.
The first strategy is implemented for the batch powder that was run
out of in several buildings. The process includes recycling, sieving,
testing, and grading. After each cycle, all the unmelted powder is
recycled and sieved to remove these particles that are not within the
specified scope of the process. Subsequently, the chemical composition,
roundness, flowability, and other characteristics of the sieved powders
are tested and ensured to be within the specified range. This process can
be repeated until the amount of the reused powder within the specifi­
cation is not sufficient for the next manufacturing. Furthermore, in order
to minimize the adverse effects of oxygen heterogeneity in reused
powder, Nicholas [109] advised that all the powder feedstock should be
used up until it passes through the machine once, and then mixed all the
recycled powder to carry out subsequent steps. In this method, the
overflow, sintered, and spatter powder generated during each operation
are separated and not allowed to continue reuse. After that, the recycled
powder is mixed and sieved before being reintroduced into the process
flow, thus becoming a new initial powder batch.
The second strategy, known as the virgin powder supplement
method, involves mixing the reused powder (sieved treatment) with a
certain amount of virgin powder after a defined number of buildings or
in between each cycle, also known as the frequent refreshing (or Top Up)
strategy [41]. The amount of virgin powder can be fed according to the
actual powder consumption in the previous manufacturing or the
experienced values. Ryan [34] used the top-up recycling strategy and
found that the oxygen content in the sieved and blended powder was
only 0.131 wt% and 0.127 wt%, respectively. Compared with the PBF-
LB/M/Ti6Al4V recycled powder (0.40 wt% and 0.43 wt% after 7 cy­
cles), the effect is very obvious. Meanwhile, the nitrogen and hydrogen
content decreased from 0.234 wt% and 0.03 wt% to lower than 0.03 wt
% and 0.012 wt%, respectively. Nevertheless, this strategy can also in­
crease the number of powder reuse, but only partially solves the in­
homogeneity of the powder if the appropriate supplement is not carried
out. Additionally, there is a possibility that a small fraction of the
powder can reach a very high degradation level due to prolonged usage
Fig. 12. Reusability decision diagram based on powder properties [22]. time. The potential disadvantage is that some unforeseeable damages to
operation and product quality gradually become uncontrollable. In
Fig. 12. Depending on the values obtained for certain parameters, five practice, this method is mostly used to produce non-high-end compo­
steps testing including the PSD, the circularity, the chemical composi­ nents [108].
tion, the flowability and the tap density need to be completed. The The third strategy is the powder deoxygenation process. Recently, in
starting point is to determine the PSD. The PSD of the reused powder order to reduce the oxygen content in the titanium alloys recycled
must be in the correct range for the PBF process. The particle shape (fs) powder, Xia [110] developed a low-temperature molten salt calcium
and circularity (fc) parameters should be between 0.7 and 1.0, and deoxygenation process using calcium as the deoxygenating agent. The
bigger number is better. The critical value of gas content and contami­ calcium halide bearing eutectic molten salt was used to facilitate the
nation in the reused powder should be as low as possible. Attentively, dissolution of the deoxygenation agent Ca and the formation of Ca+ ions
the significant decrease in fluidity (> 25%) must be avoided from reuse. in the molten salt. They then reacted on the surface of the oxide parti­
Otherwise, the reused powder must be further treated with effective cles, causing the deoxygenation reaction. This process can remove ox­
measures before being reused. In addition, in order to ensure a homo­ ygen content in titanium powder from >20,000 ppm to <1000 ppm. In
geneous and compact powder bed, the packing ratio (η) is at least 0.6 addition, the de-oxidation in solid state process, hydrogen-assisted
(ρtap/ρtrue). The practice has confirmed that this method can assist end- deoxygenation process, the Ca vacuum process, and the electrolysis
users effectively improve the reuse times of the reused powder. process are also beneficial for deoxygenation [111].
The fourth strategy is the powder reconditioning technology. In
general, the degraded recycled powder and powder prepared by the
water atomization method have disadvantages such as irregular shape,

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J. Li et al. Powder Technology 441 (2024) 119815

more satellite powders, and high oxygen content, which limit the usage Table 2
amount and cycling times of reuse. Plasma spheroidization technology Chemical compositions of raw powder and spheroidized powder. /wt% [115].
can be regarded as a plausible technique to recondition powder, Si Mn Ni Cr Mo O Fe
contributing to improve powder characteristics such as increase powder
Row powder 0.97 0.53 13.0 17.2 2.29 0.30 Bal.
purity, roundness, and flowability, as well as decrease internal porosity Spheroidized Powder 0.77 0.51 12.8 16.5 1.67 0.16 Bal.
and oxygen content.
General Electric Co (GE) has developed a plasma spheroidization
equipment [112]. By melting the outermost layers of the particle, the in both apparent and packing density. Owing to not sensitive to the
size of particles decreased to within acceptable parameters for use in change in particle shape, Hall flow results did not change. The oxygen
PBF, while the particles became more spherical. Meanwhile, the oxygen, content reduced to 0.016 wt% after post-ICP. The spheroidization effect
nitrogen, and hydrogen content reduced significantly. Further to this, indicates that the ICP process is successful in restoring the morphology
GE stated that alloying elements can be added into the powder feedstock of the recycled powder, and the characteristics meet the requirements of
to alter the chemical composition of the output powder, so that the PBF process.
output powder is chemically altered to meet the specification. As a Up to now, the spheroidization process is gradually used to modify
result, the oxygen content can be reduced by 97%; meanwhile, the the non-spherical powders produced from water atomization, chemical
flowability, packing density, particle porosity, surface morphology and reactions, mechanical processes, especially the waste powder produced
powder purity can be improved. These claims are supported by Powell in the building process. With up to a third of the production cost of AM
[4], Moghimian [41], LPW Technology Ltd. [113] and Matthes [114] component being the cost of the powder used, commercial viability
et al. depends on establishing a robust supply chain and an effective powder
The National Institute of Advanced Industrial Science and Technol­ recycling strategy [117,118]. If a sufficient quantity of the irregular
ogy (AIST) uses DC arc plasma as a thermal source to obtain the high- particles can be collected and spheroidized, the spheroidization process
grade powder from the irregularly shaped powder [115]. The plasma will further improve the service life of the metal powder and lower the
spheroidization system consisted of a plasma spray gun, a processing cost of the PBF technology. The enhancement in the build cycles and the
chamber, a powder feeder, and a powder and gas supplying system. On reduction in costs of the metal powder will benefit to the promotion and
the one hand, high temperature molten metal droplets can be formed by the potential applications of PBF in high-end fields such as aerospace,
DC technology, which can be rapidly cooled to generate spherical fine new energy resources and medical devices [119–121]. In addition, this
metal particles. Furthermore, the nanoparticles and spherical particles technology can also be applied to the preparation of high-quality
can be simultaneously produced in the short processing time. By uti­ conductive materials in the fields of electronics, energy storage and
lizing this technique, water-atomized powders of 316 L stainless steel electromagnetic wave absorption [122,123].
were recondition to spherical shape. Fig. 13 exhibited the reconditioned
effect. It can be found from SEM images, this process successfully 7. Conclusion and outlook
spheroidized the irregular shaped powder of SUS316 L with an average
particle diameter of 38 μm. Table 2 shows the changers of the chemical In summary, understanding the interaction between the energy
compositions. The chemical compositions of spheroidized particles did beam, powder and melt pool in the PBF process is crucial for achieving
not change significantly compared with the raw powder. In contrast, the stable and high-quality AM products. The complex physical phenomena
oxygen content decreased significantly. involved in this interaction can generate side-effects and lead the
Garboczi [116] introduced the inductively coupled plasma (ICP) changes in the characteristics of the recycled powder, such as particle
spheroidization process to recondition the degraded powders. The morphology, microstructure, magnetic properties, surface composition,
powders to be repaired were injected axially into the plasma using argon and oxide thickness, correspondingly affect the flowability, packing
as the carrier gas. As individual particles were heated and melted in the density, and thermal properties of the powder bed. The characteristics
plasma, surface tension caused them to form a dense molten metal degradation of the reused powder can affect the AM process parameters,
droplet. Subsequently molten droplet cooled, solidified and fell to the final product microstructure, and mechanical properties. As the recy­
bottom of the reactor, and then collected in the container. Owing to cling of powder continues, the type, size, number and the potential
being converted into gaseous condensate of the alloy during the plasma defects increase correspondingly, leading to mechanical properties and
transitioning, a lot of fines were accompanied with the process, which surface performance issues in the final products.
must be subsequently washed. Figs. 14 showed the morphologies of the To maintain the quality of the AM products and extend the life of the
Inconel 718 powder and the Ti6Al4V powder before and after the ICP reused powder, it is important to accurately assess the powder’s char­
process, including the effect of washing. Flowability, density, and acteristics before each operation and adjust the process parameters
chemical characteristics of the pre and post-ICP for Inconel 718 powders accordingly. Additionally, regeneration and reconditioning technologies
are shown in Table 3. Due to the reduction of irregular particles and an can help rejuvenate the reused powder, restoring it to its original
increase in spherical particles, the post-ICP powder showed an increase characteristics and reducing waste in the AM industry. By employing a

Fig. 13. Reconditioned effect on the morphologies of 316 L powder particles [115]. (a) raw powder, (b) spheroidized powders.

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J. Li et al. Powder Technology 441 (2024) 119815

Fig. 14. The spheroidization effect of ICP process. Above is Inconel 718 powders, below is Ti6Al4V powders [116]. (a) and (d) used powder, (b) unwashed
reconditioned powder, (c) and (e) reconditioned powder after washed.

the performance life of metal powders will be significantly improved,

Table 3
promoting the growth and adoption of additive manufacturing across a
Pre and Post-ICP Inconel 718 powder characteristics [116].
wide range of industries.
Pre-ICP Post-ICP

Hall flow 12.7 s/50 g 12.6 s/50 g CRediT authorship contribution statement
Apparent density 4.3 g/cm3 4.6 g/cm3
Packing density 4.4 g/cm3 4.8 g/cm3
Jiwen Li: Writing – review & editing, Writing – original draft,
Oxygen content 0.02 wt% 0.016 wt/ %
Conceptualization. Wei Liu: Writing – original draft. Jie Shen: Writing
– original draft. Xin Zhang: Data curation. Shunjie Li: Data curation.
comprehensive understanding of the interaction between the energy Zhenshuai Wang: Data curation.
beam, powder and melt pool, optimizing process parameters, and uti­
lizing regeneration and reconditioning technologies, it is possible to Declaration of competing interest
enhance powder reusability, maintain the quality of the final products,
and reduce costs in the additive manufacturing industry. The authors declare that they have no known competing financial
As the PBF process continues to evolve and become more widely interests or personal relationships that could have appeared to influence
adopted in various industries, research and development efforts should the work reported in this paper.
focus on addressing current challenges and enhancing the performance
life of metal powders. Some key areas of focus for the future include: Data availability

(1) Developing simple, effective testing devices for online detection The data that has been used is confidential.
and rapid identification of key powder characteristics, as well as
establishing standards for evaluating the reusability of powders. Acknowledgement
These advancements will contribute to improved process
parameter optimization, product quality, and cost reduction. This research has been supported by Program for Changjiang
(2) Deepening the understanding of the interaction between the en­ Scholars and Innovative Research Team in University of Ministry of
ergy beam, powder and melt and its effects on the characteristics Education of China (Grant No. IRT_1234) and the Non-ferrous Metal
of recycled powder. This knowledge will facilitate more accurate Generic Technology Collaborative Innovation Center of Henan Province.
predictions, descriptions, and control of the manufacturing pro­
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