metals

Article
Research on Selective Laser Melting of Ti6Al4V:
Surface Morphologies, Optimized Processing Zone,
and Ductility Improvement Mechanism
Di Wang 1,2 ID
, Wenhao Dou 1 and Yongqiang Yang 1, *
1 School of Mechanical and Automotive Engineering, South China University of Technology,
Guangzhou 510640, China; mewdlaser@scut.edu.cn (D.W.); dwh68@outlook.com (W.D.)
2 School of Metallurgy and Materials, The University of Birmingham, Birmingham B152TT, UK
* Correspondence: meyqyang@scut.edu.cn; Tel./Fax: +86-020-8711-1036




Received: 24 May 2018; Accepted: 15 June 2018; Published: 21 June 2018


Abstract: The quality and mechanical properties of titanium alloy fabricated using selective laser
melting (SLM) are critical to the adoption of the process which has long been impeded by the lack of
uniformity in SLM-fabrication parameter optimization. In order to address this problem, laser power
and scanning speed were combined into linear energy density as an independent variable, while
surface morphology was defined as a metric. Based on full-factor experiments, the surface quality of
SLM-fabricated titanium alloy was classified into five zones: severe over-melting zone, high-energy
density nodulizing zone, smooth forming zone, low-energy density nodulizing zone, and sintering
zone. The mechanism resulting in the creation of each zone was analyzed. Parameter uniformity was
achieved by establishing a parameter window for each zone, and it also revealed that under smooth
forming conditions, the relationship of linear energy density to the quality of the formed surface is
not linear. It was also found that fabrication efficiency could be improved in the condition of the
formation of a smooth surface by increasing laser power and scanning speed. In addition, maximum
elongation of the SLM-fabricated titanium alloy increased when the densified parts were processed
using an appropriate heat treatment, from a low value of 5.79% to 10.28%. The mechanisms of change
in ductility of the alloy were thoroughly analyzed from the perspectives of surface microstructure
and fracture morphology. Results indicate that after heat treatment, the microcosmic structure of the
alloy was converted from acicular martensite α’ phase to a layered α+β double-phase structure, the
fracture type also changed from quasi-cleavage to ductile fracture.

Keywords: selective laser melting; optimized parameter zone; surface morphology; ductility
improvement mechanism; energy density

1. Introduction
Ti6Al4V (TC4) is the most common α+β dual-phase, high-temperature titanium alloy, and is
studied more thoroughly than any other titanium alloy [1]. Due to its low density, excellent specific
strength, and desirable mechanical properties, it has found widespread uses in military, aviation,
space [2], and auto industries. Compared with stainless steel and CoCr alloy, Ti6Al4V is characterized
by outstanding biological compatibility, corrosion resistance, and an elastic modulus more similar to
bone tissues than other alloys. Hence, it is usually used for medical purpose and is of great value to
biomedical research and applications [3–6]. Titanium alloy is manufactured using casting or forging
traditionally. However, titanium’s strength and hardness are rather high, leading to a machining
process that is rather complex and expensive, making it hard to produce complicated structures.
As a result, Ti6Al4V possesses a unique combination of strength, toughness, corrosion resistance,

Metals 2018, 8, 471 ; doi:10.3390/met8070471 www.mdpi.com/journal/metals

Metals 2018, 8, 471 2 of 17

low specific weight, and biocompatibility, making it very suitable for high-performance engineering
solutions [7].
Selective laser melting (SLM) is a metal additive manufacturing technology which can directly
fabricate parts following the design or acquisition of complex 3D models using computer techniques.
This is done by directly melting metal or alloy powders using a high-energy laser beam, depending
on the information of each slice of the model, and each part is manufactured in a stacked manner [8].
The density of SLM-fabricated parts has reached over 99% due to continuous development of the
manufacturing technique, and a dimensional error could be controlled within 0.05 mm. Because of
its ability to directly fabricate complex curved surfaces and porous structures [9,10], SLM-fabricated
Ti6Al4V alloys find widespread use in the direct manufacturing of auto and aviation components [11],
in addition to medical implants [12–14]. Study of the fabrication of Ti6Al4V around the world using
SLM is still focused on process control and parameter optimization, but using different optimization
metrics. Wang et al. [15] investigated the influence of laser scanning speed on the density and
mechanical properties of SLM-fabricated titanium alloy. Experimental results demonstrated that a
density of 99.57%, hardness of 407 HV, and tensile strength of 1225 MPa could be achieved, which
was explained briefly after studying its microscopic structure. Thijs et al. [16] discussed the influence
of parameter and scanning strategy on microscopic structure during the manufacturing process,
demonstrating that rapid cooling led to the presence of martensite, a columnar crystal generated
during the re-melting process of the previous layer, and that the direction of its growth was determined
by the local transmission of heat. Song et al. [17] explored the influence of laser power and scanning
speed on the microcosmic structure of SLM-fabricated titanium alloy using a 3D finite element model
in the analysis. Their results indicated that a laser power of 110 W and scanning speed of 0.2 m/s led
to an appropriate gradient of temperature within the powder bed which maximized depth of melting.
The influence of laser power and scanning speed was comprehensively evaluated under the metrics of
mechanical properties (e.g., density and coarseness) and microcosmic properties (e.g., hardness and
structure). It was determined from these observations that optimization parameters for the fabrication
of titanium alloy by SLM vary considerably and are dependent on optimization metrics. In this context,
the lack of uniformity in parameter optimization is a big challenge that must be addressed for further
adoption of SLM when fabricating titanium alloy.
Another common challenge that impedes the SLM fabrication of titanium alloy is the low
elongation that is achieved [18,19]. Vrancken et al. [20] studied the influence of heat treatment
temperature, time, and cooling speed on microcosmic structure and mechanical properties of
SLM-fabricated Ti6Al4V. The experimental results revealed that the maximum temperature of heat
treatment had more influence on mechanical properties of the fabricated parts than any other factor,
then a new heat treatment process was proposed to improve maximum elongation of titanium alloy.
In this paper, the influence of linear energy density on surface morphology is discussed.
A full-factor experiment was performed to classify the quality of the SLM-fabricated titanium alloy into
several zones, and the principles behind each zone were analyzed. A fabricating parameter window for
optimization of SLM fabrication of Ti6Al4V alloy powder was established. Based on this, tensile testing
was performed and the morphology of the microcosmic structure observed. The mechanism regarding
improvement in ductility of the SLM-fabricated titanium alloy after thermal treatment is discussed.

2. Experimental Methods

2.1. Equipment and Material

The experiments were carried out using a self-developed selective laser melting (SLM) machine,
a DiMetal-100 (SCUT, Guangzhou, China). Figure 1a (reproduced from reference [21]) displays the
principles of the DiMetal-100 SLM manufacturing equipment. The setup consisted of a fiber laser,
optical-path transmission unit, sealing chamber (including powder recoating device), mechanical drive,
control systems, and processing software. The laser was directed using a scanning galvanometer, which
which focused it through an F-θ lens for selectively melting the metallic powder on the plane,
followed by layer-wise stacking into a metal part. The machine had a scanning speed in the range
10–5000 mm/s, thickness of processing layer in the range 20–100 µm, and a laser focusing spot
diameter of 70 µm. The largest size of parts produced was 100 mm × 100 mm × 100 mm. Since
Metals 2018, 8, 471
the
3 of 17
powder was fully melted during the process, protection of the SLM-processed parts from oxidation
was essential, and achieved by completing the process in an atmosphere of argon or nitrogen with
focused
less thanit0.15%
through O2. an F-θ lens for selectively melting the metallic powder on the plane, followed by
layer-wise stacking
Ti6Al4V powder intofrom
a metal part.
Falcon The machine
Aerotech hadofa scanning
Limited speedsatisfied
China, which in the range 10–5000 mm/s,
the requirements of
thickness
ASTM of processing
F2924, was used for layer
SLMin fabrication.
the range 20–100 µm, and
The Ti6Al4V a laserviewed
powder focusing
at aspot diameter ofof70
magnification µm.
1500×
The
usinglargest
scanningsizeelectron
of parts microscopy
produced was (SEM, mm ×
100Nova 100 mm ×
NanoSEM 100
430, FEImm. Since the
company, powderOR,
Hillsboro, wasUSA)
fully
melted during the process, protection of the SLM-processed parts from oxidation was essential,
is shown in Figure 1b. It can be seen that the powder particles are almost entirely spherical and mostly and
achieved
not adheredby completing the process
to one another; the mean inparticle
an atmosphere ofof
diameter argon or nitrogen
the powder was with less than 0.15% O2 .
36 µm.

Figure
Figure 1.
1. Principles,
Principles, devices,
devices, and
and materials
materials for
for selective
selective laser
laser melting
melting (SLM)-based
(SLM)-based 3D
3D metal
metal printing:
printing:
(a) illustration of SLM fabrication (reproduced from [21], with permission from Elsevier, 2018);
(a) illustration of SLM fabrication (reproduced from [21], with permission from Elsevier, 2018);
(b) Ti-6Al-4V
(b) Ti-6Al-4V powder
powder viewed
viewed byby scanning
scanning electron
electron microscopy
microscopy (SEM).
(SEM).

2.2. Experimental Methods

Ti6Al4V powder (the composition of Ti6Al4V powder can be found in Table S1 in the
Supplementary
2.2.1. Determination Material) fromfor
of Range Falcon Aerotech Limited
the Fabricating of China, which satisfied the requirements of
Parameters
ASTM F2924, was used for SLM fabrication. The Ti6Al4V powder viewed at a magnification of 1500×
usingAscanning
full-factor experiment
electron microscopywas (SEM,
performed
Nova to obtain the
NanoSEM 430,optimal combination
FEI company, Hillsboro,of OR,
parameters
USA) is
including laser power, scanning speed, layer thickness, scanning spacing,
shown in Figure 1b. It can be seen that the powder particles are almost entirely spherical and and laser spot size.
mostly
Modifiability
not adhered toofone these parameters
another; the meanwasparticle
considered jointly,
diameter andpowder
of the the influence of each factor on SLM
was 36 µm.
fabrication quality analyzed. Laser power “P” and scanning speed “V” were selected for studying
2.2. influence
the Experimental Methods
of the process parameters on the surface quality of the SLM-fabricated titanium alloy.
Experimentation on the fabrication process consisted of an early stage (I) of large-range exploration
2.2.1.aDetermination
and late stage (II) of of Range for the Fabricating
range refinement. Parameters
In the early stage (I), the range was 150–400 W for laser
power A and 600–1600
full-factor mm/s for scanning
experiment speed, astoshown
was performed obtainin the
Figure 2a. According
optimal to theof
combination forming effect
parameters
during
including stage (I),power,
laser we refined and speed,
scanning optimizedlayerthethickness,
selection scanning
of parameters
spacing,in order
and laserto reduce the
spot size.
complexity of the experiment. The narrow scanning speed range was more sustainable
Modifiability of these parameters was considered jointly, and the influence of each factor on SLM for optimizing
parameters, and weanalyzed.
fabrication quality got stage (II) building
Laser powerparameters. The late speed
“P” and scanning stage (II)
“V” ofwere
rangeselected
refinement is shown
for studying
in Figure 2b. In the experiment, the block size was 10 mm × 10 mm × 10 mm, 25
the influence of the process parameters on the surface quality of the SLM-fabricated titanium alloy.µm for layer thickness,
0.08 mm for hatch
Experimentation onspacing, and scanning
the fabrication process mode wasofS-shaped
consisted orthogonal
an early stage scanning. In
(I) of large-range addition,
exploration
following the layer
and a late stage thickness
(II) of of 25 µm, In
range refinement. layer thicknesses
the early of the
stage (I), 30 µm,
range35was
µm,150–400
40 µm,W and for45 µmpower
laser were
also used to get an optimized processing window. The principles of the fabrication
and 600–1600 mm/s for scanning speed, as shown in Figure 2a. According to the forming effect during are presented in
Figure 2c.we refined and optimized the selection of parameters in order to reduce the complexity of the
stage (I),
experiment. The narrow scanning speed range was more sustainable for optimizing parameters, and
we got stage (II) building parameters. The late stage (II) of range refinement is shown in Figure 2b.
In the experiment, the block size was 10 mm × 10 mm × 10 mm, 25 µm for layer thickness, 0.08 mm
for hatch spacing, and scanning mode was S-shaped orthogonal scanning. In addition, following the
layer thickness of 25 µm, layer thicknesses of 30 µm, 35 µm, 40 µm, and 45 µm were also used to get
an optimized processing window. The principles of the fabrication are presented in Figure 2c.
Metals 2018, 8, 471 4 of 17
Metals 2018, 8, x FOR PEER REVIEW 4 of 17

Figure2.2.Setting
Figure Settingparameters
parameters for
for SLM
SLM fabrication of of Ti6Al4V:
Ti6Al4V: (a)
(a) Fabricating
Fabricatingparameters
parametersfor
forstage
stage(I);
(I);
(b) fabricating parameters for stage (II); (c) principles of S-shaped
(b) fabricating parameters for stage (II); (c) principles of S-shaped normal scanning.
scanning.

2.2.2.Testing
2.2.2. TestingMethods
Methods
Surfacemorphology
Surface morphology of of the
the titanium
titanium alloy
alloy parts
parts fabricated
fabricated byby SLM
SLM using
using different
different parameters
parameters
neededto
needed tobe
beinvestigated
investigated in in this
this study,
study, with
with features
features such
such as
as track
track overlap
overlap and
and track
track fabrication
fabrication
quality analyzed. To this end, the 3D super depth-of-field microscope VHX-5000
quality analyzed. To this end, the 3D super depth-of-field microscope VHX-5000 (KEYENCE company, (KEYENCE
company,
Osaka, Osaka,
Japan) was Japan)
adopted wasforadopted
observingfor surface
observing surface morphology
morphology and quality and
of quality of the fabricated
the fabricated parts, and
parts, and the roughness was measured by 3D optical Profilometer from Rtec
the roughness was measured by 3D optical Profilometer from Rtec Instruments company (San Jose, Instruments company
(SanUSA).
CA, Jose, CA, USA).
Then,
Then, in in order
order totostudy
studythe theinfluence
influenceof heat treatment
of heat on the
treatment onductility performance
the ductility of the SLM-
performance of the
fabricated TC4 alloy, the heat treatment steps of our experiment were defined based
SLM-fabricated TC4 alloy, the heat treatment steps of our experiment were defined based on the phase on the phase
diagramof
diagram ofTC4
TC4andandrelevant
relevant investigations
investigations [22,23].
[22,23]. Vacuum
Vacuum heat
heat treatment
treatment was
wasperformed
performedusing
usinganan
N41/H Muffle furnace from Nabertherm company, Lilienthal, Germany. The heat treatmentprocess
N41/H Muffle furnace from Nabertherm company, Lilienthal, Germany. The heat treatment process
required elevation of the temperature to 840 °C over 3 h, the temperature maintained for 2 h, then the
required elevation of the temperature to 840 ◦ C over 3 h, the temperature maintained for 2 h, then the
furnace cooled until the temperature reduced to 450 °C and subsequently cooled by air.
furnace cooled until the temperature reduced to 450 ◦ C and subsequently cooled by air.
The tensile strength of the SLM-fabricated TC4 alloy was tested. The experiment was designed
The tensile strength of the SLM-fabricated TC4 alloy was tested. The experiment was designed to
to be compliant with ISO 6892-1:2016, a standard for experimentation in tensile strength of metal
be compliant with ISO 6892-1:2016, a standard for experimentation in tensile strength of metal materials
materials at room temperature. Other parameters of performance were also tested and analyzed in
at room temperature. Other parameters of performance were also tested and analyzed in accordance
accordance with this standard. Samples with a diameter of 5 mm and scale distance of 40 mm were
with this standard. Samples with a diameter of 5 mm and scale distance of 40 mm were selected for
selected for the tensile experiment. Two groups of SLM-fabricated Ti6Al4V titanium (i.e., those with
the tensile experiment. Two groups of SLM-fabricated Ti6Al4V titanium (i.e., those with and without
and without heat treatment) underwent the tensile experimentation using the electronic universal
heat treatment) underwent the tensile experimentation using the electronic universal testing machine
testing machine CMT5105 (MTS company, Eden Prairie, MN, USA), at a rate of 0.2 mm/min.
CMT5105 (MTS company, Eden Prairie, MN, USA), at a rate of 0.2 mm/min. The stress-strain curves
The stress-strain curves were obtained from a software calculation of experimental data on stress and
were obtained from a software calculation of experimental data on stress and distortion. Subsequently,
distortion. Subsequently, tensile strength, yield strength, and elongation were computed. Tensile
fracture was observed using a NanoSEM 430 (FEI company, Hillsboro, OR, USA).
Metals 2018, 8, 471 5 of 17

tensile strength, yield strength, and elongation were computed. Tensile fracture was observed using a
NanoSEM 430 (FEI company, Hillsboro, OR, USA).
Except for tensile property, micro-hardness is taken into discussion as well. The micro-hardness
test strictly complied with ISO 6507-1:2018 on micro-hardness tester HVS-3.0 (Jinan Fangyuan Testing
Machine company, Jinan, China). In this article, only the upper surface micro-hardness was considered.
The imposed loading was 1 kg, and the holding time was 15 s. Similarly, both the as-built samples and
heat-treated samples were considered.
In order to study the influence of heat treatment on the ductility and micro-hardness of the
SLM-fabricated Ti6Al4V alloy from the perspective of microcosmic structure, samples of the Ti6Al4V
alloy were manufactured using SLM in compliance with ISO 4499:2011. Here, the same smooth
forming parameters were adopted using a block size of 10 mm × 10 mm × 10 mm. Some samples
were thermally treated using the method descried above. Finish grinding and mechanical polishing
were performed on the thermally-treated and as-built samples using abrasive paper of 600, 800, 1000,
and 1500 mesh in addition to a polishing cloth. The upper surface of each sample was corroded using
aqua regia for approximately 60 s. The microcosmic structure of each samples’ surface metallography
was observed using a Leica DMI 5000 (Leica Microsystems company, Buffalo Grove, IL, USA) at a
magnification of 50–500×.

3. Results and Discussions

3.1. Classification of Surface Morphology

A macroscopic view of fabricated square parts was performed and summarized. Note that for
some samples, the required energy was too great to proceed with the fabrication process and the
process had to be halted by human intervention via the controlling software. From the experimental
results, it is clear that for a given laser power, the quality of fabricated parts varies considerably with
increased scanning speed. Meanwhile, a parameter is needed as a metric to classify the fabricated
regions. Surface quality of the SLM-fabricated parts strongly correlated with the parts’ density and
properties. In this paper, surface quality was defined as the principal metric to observe track quality
and overlapping effectiveness. Based on the definitions put forward in References [24–28], the linear
energy input model in Reference [28] was used to investigate the influence of energy input on surface
morphology and melting status.
P
ψ= , (1)
V
The surface morphology of parts fabricated under different parameters was observed using the
VHX-5000. The observed results can be classified into five categories (i.e., severe over-melting zone,
high energy density nodulizing zone, smooth forming zone, low energy density nodulizing zone
and sintering zone, which can be found in Figures S1–S5 in the Supplementary Material), as shown
in Figure 3. It can be seen that these regions are very distinct. The serious over-melting zone is
characterized by serious distortion, roughness, and some nodulizing at the surface of the parts, as
seen in Figure 3a. Its typical parameters are P = 150 W for laser power and V = 600 mm/s for scanning
speed. For the high-energy density nodulizing region, the surface of the parts become smooth with
slight nodulizing, but there were still irregular bulges and concaves, as seen in Figure 3b. Its typical
parameters were P = 150 W for laser power and V = 700 mm/s for scanning speed. For the smooth
forming zone, the surface was smooth with continuous tracks, ideal overlapping, and elimination of
nodulizing, as shown in Figure 3c. Its typical parameters were P = 150 W for laser power and V = 800
mm/s for scanning speed. For the low-energy density nodulizing zone, the track at the surface of the
parts was not continuous, and melting status was poor, leading to the presence of some holes between
tracks. Moreover, some powders were not melted at the surface, some ball-shaped bulges were present,
and the upper surface of the parts was coarse and void of metallic lustre, as shown in Figure 3d.
Its typical parameters were P = 150 W for laser power and V = 1000 mm/s for scanning speed. For
Metals 2018, 8, 471 6 of 17

the sintering zone, the surface of the parts lacked metallic lustre, the track was not continuous, and
most of the powder was sintered, as seen in Figure 3e. Note the surface appears sandy with weak
bonding strength between tracks. Its typical parameters were P = 150 W for laser power and V = 1100
Metals 2018, 8, x FOR PEER REVIEW 6 of 17
mm/s for scanning speed. Visual results indicate that nodulizing was present in both the high-energy
(Figure 3b) and low-energy density nodulizing zones (Figure 3e), this result confirms the conclusions
both the high-energy (Figure 3b) and low-energy density nodulizing zones (Figure 3e), this result
in confirms
References [29,30]. In addition, close observation of the results reveal that spatter particles were
the conclusions in References [29,30]. In addition, close observation of the results reveal that
inserted
spatter particlestrack-overlapped
into the were inserted intosurface of all samples.surface of all samples.
the track-overlapped

Figure 3. Surface morphologies of parts fabricated with parameters in different ranges: (a) serious
Figure 3. Surface morphologies of parts fabricated with parameters in different ranges: (a) serious
over-melting zone; (b) high-energy density nodulizing zone; (c) smooth forming zone; (d) low-energy
over-melting zone; (b) high-energy density nodulizing zone; (c) smooth forming zone; (d) low-energy
density nodulizing zone; (e) sintering zone.
density nodulizing zone; (e) sintering zone.
Furthermore, in order to fully show and distinguish the five categories of surface, the roughness
Furthermore,
and in order to fully
3D surface morphologies are show
shownand distinguish
in Figure 4. Note the five
that forcategories of surface,
software reasons, the roughness
in Figure 4, the
and 3D of
peak surface morphologies
the parts is the bottom areofshown
the 3D in Figuremorphology,
surface 4. Note that andforvice
software
versa. Inreasons, in Figure
addition, on the 4,
theZ-axis,
peak ofthethe
origin
partsbegins
is thefrom
bottomthe of
bottom
the 3Dof surface
the 3D surface morphology.
morphology, In figure
and vice versa.4a,b, it can clearly
In addition, on the
be observed
Z-axis, the originthat the from
begins proportion of smooth
the bottom of the 3Dformed
surface tracks increasedIn first
morphology. Figureand then
4a,b, decreased.
it can clearly be
As mentioned
observed that theabove, the bulges
proportion including
of smooth formedballings
tracksand concaves
increased which
first weredecreased.
and then generated due to high-
As mentioned
energy density, led to the broken scanning track. The key difference between the
above, the bulges including ballings and concaves which were generated due to high-energy density,serious over-melting
zone and high-energy density nodulizing zone is the area of normal forming plane and the depth or
height of defect. Except for the height as shown in Figure 4a,b, the average roughness values Ra of
multi-group samples were 20.91 µm and 16.82 µm. More smooth tracks would reduce the roughness.
But in the parameter window, the roughness could not be a sufficient condition for strictly classifying
Metals 2018, 8, 471 7 of 17

led to the broken scanning track. The key difference between the serious over-melting zone and
high-energy density nodulizing zone is the area of normal forming plane and the depth or height of
defect. Except for the height as shown in Figure 4a,b, the average roughness values Ra of multi-group
samples were 20.91 µm and 16.82 µm. More smooth tracks would reduce the roughness. But in the
parameter
Metals 2018,window, the REVIEW
8, x FOR PEER roughness could not be a sufficient condition for strictly classifying the forming
7 of 17
zones. Because of some unmeasurable defects, the reliability of roughness was weakened. In the actual
the formingofzones.
exploration Because
processing of some unmeasurable
parameters, defects, the
the comprehensive reliability
evaluation of roughness
method was weakened.
is necessary. Similarly,
In the actual exploration of processing parameters, the comprehensive evaluation
the incomplete melting causes the holes and breaks in the track. There is little regular big concaves method is
necessary. Similarly, the incomplete melting causes the holes and breaks in the track. There
or bulges in the low-energy density nodulizing surface and sintering surface, which is significantly is little
regular big
different from concaves or bulges
the serious in the low-energy
over-melting density nodulizing
zone or high-energy surface and zone.
density nodulizing sintering surface,
Considering
which is significantly different from the serious over-melting zone or high-energy density nodulizing
surface roughness, the average measured values of Ra in the low-energy density nodulizing zone
zone. Considering surface roughness, the average measured values of Ra in the low-energy density
and sintering zone were 20.37 µm and 14.51 µm, respectively. It seems that the normal forming plane
nodulizing zone and sintering zone were 20.37 µm and 14.51 µm, respectively. It seems that the
would increase the surface roughness. But in fact, the area of normal forming surface in the low-energy
normal forming plane would increase the surface roughness. But in fact, the area of normal forming
density nodulizing zone was bigger than that in the sintering zone. The sintered state of breaking
surface in the low-energy density nodulizing zone was bigger than that in the sintering zone.
tracks with a small thickness decreased the surface roughness. The accumulation of holes and breaking
The sintered state of breaking tracks with a small thickness decreased the surface roughness.
tracks exacerbated the quality of the surface.
The accumulation of holes and breaking tracks exacerbated the quality of the surface.

Figure 4. 3D surface morphologies of five forming zones: (a) serious over-melting zone; (b) high-
Figure 4. 3D surface morphologies of five forming zones: (a) serious over-melting zone; (b) high-energy
energy density nodulizing zone; (c) smooth forming zone; (d) low-energy density nodulizing zone;
density nodulizing zone; (c) smooth forming zone; (d) low-energy density nodulizing zone;
(e) sintering zone.
(e) sintering zone.

3.2. Fabricating Parameter Optimization Window

After inspecting and summarizing the surface morphology of all square parts obtained from the
full-factor experiment, the SLM-fabricated titanium alloy’s surface was classified into five zones (i.e.,
severe over-melting zone, high-energy density nodulizing zone, smooth forming zone, low-energy
density nodulizing zone, and the sintering zone). Based on Equation (1), the fabricating parameters
Metals 2018, 8, 471 8 of 17

3.2. Fabricating Parameter Optimization Window

After inspecting and summarizing the surface morphology of all square parts obtained from the
full-factor experiment, the SLM-fabricated titanium alloy’s surface was classified into five zones (i.e.,
Metals
severe 2018, 8, x FOR PEERzone,
over-melting REVIEW 8 of 17
high-energy density nodulizing zone, smooth forming zone, low-energy
density nodulizing zone, and the sintering zone). Based on Equation (1), the fabricating parameters
morphology, all fabricating parameters were allocated to a corresponding zone. Statistical data from
in the experiment were converted into linear energy density. According to their respective surface
the experiment was utilized to compute the linear energy density of each zone, with laser power “P”
morphology, all fabricating parameters were allocated to a corresponding zone. Statistical data from
as the abscissa and linear energy density “ψ” as the vertical coordinate. Given a layer thickness of 25
the experiment was utilized to compute the linear energy density of each zone, with laser power “P” as
µm, the results and the relationship between the energy input and the forming zone is plotted in
the abscissa and linear energy density “ψ” as the vertical coordinate. Given a layer thickness of 25 µm,
Figure 5. From this figure, it can be deduced that for SLM-fabricated titanium alloy, the range of
the results and the relationship between the energy input and the forming zone is plotted in Figure 5.
linear energy density is not constant. Rather, it varies with laser power (scanning speed). For the
From this figure, it can be deduced that for SLM-fabricated titanium alloy, the range of linear energy
smooth forming zone, the range of linear energy density varied from 0.17 to 0.22 J/mm at low laser
density is not constant. Rather, it varies with laser power (scanning speed). For the smooth forming
power (150~200 W), 0.23~0.26 J/mm at P = 300 W, and 0.27~0.29 J/mm at P = 400W. Therefore, the
zone, the range of linear energy density varied from 0.17 to 0.22 J/mm at low laser power (150~200 W),
linear energy density was not linearly related to the quality of the formed surface. The traditional
0.23~0.26 J/mm at P = 300 W, and 0.27~0.29 J/mm at P = 400W. Therefore, the linear energy density
belief that setting the linear energy density appropriately can necessarily guarantee surface quality is
was not linearly related to the quality of the formed surface. The traditional belief that setting the
incorrect. It is also incorrect to establish direct correspondence between energy input and quality of
linear energy density appropriately can necessarily guarantee surface quality is incorrect. It is also
surface formation. On the evidence of Figure 5, after limiting the fabricating parameters to the smooth
incorrect to establish direct correspondence between energy input and quality of surface formation.
forming zone, the efficiency of laser forming can be improved by increasing laser power or scanning
On the evidence of Figure 5, after limiting the fabricating parameters to the smooth forming zone, the
rate.
efficiency of laser forming can be improved by increasing laser power or scanning rate.

Figure
Figure 5.
5. Formation
Formation zones
zones in
in energy
energy density
density vs.
vs. energy
energy input.
input.

Samples obtained at a layer thickness of 30 µm, 35 µm, 40 µm, and 45 µm were similarly
Samples obtained at a layer thickness of 30 µm, 35 µm, 40 µm, and 45 µm were similarly analyzed.
analyzed. The relationship with varying layer thickness between laser energy input and parameter is
The relationship with varying layer thickness between laser energy input and parameter is plotted in
plotted in Figure 6. Given a layer thickness of 25 µm, 30 µm, 35 µm, 40 µm, and 45 µm, the fabricating
Figure 6. Given a layer thickness of 25 µm, 30 µm, 35 µm, 40 µm, and 45 µm, the fabricating parameter
parameter windows of the smooth forming zone are shown in Figure 6. It can be seen that for a given
windows of the smooth forming zone are shown in Figure 6. It can be seen that for a given layer
layer thickness, the linear energy density of the smooth forming zone varies in the same way with
thickness, the linear energy density of the smooth forming zone varies in the same way with increasing
increasing the laser power P. That is, the upper and lower limits of the linear energy density of the
smooth forming zone increased by a large margin. Moreover, the two limits of the smooth forming
zone also increased considerably with layer thickness. This can be attributed to the fact that if the
quantity of powder in a layer increases, greater energy input density is required to melt the powder
in order to obtain a satisfactory track and quality of formation. Therefore, the quality of SLM-
Metals 2018, 8, 471 9 of 17

the laser power P. That is, the upper and lower limits of the linear energy density of the smooth
forming zone increased by a large margin. Moreover, the two limits of the smooth forming zone also
increased considerably with layer thickness. This can be attributed to the fact that if the quantity of
powder in a layer increases, greater energy input density is required to melt the powder in order to
obtain a satisfactory track and quality of formation. Therefore, the quality of SLM-fabricated titanium
alloy can be guaranteed by limiting the fabricating parameters to the range of the smooth forming
zone, or choosing
Metals 2018, the fabricating
8, x FOR PEER REVIEW parameters based on the windows in Figure 6. 9 of 17

Figure 6.
Figure 6. Energy
Energy input
input vs.
vs. parameter
parameter ranges
ranges under
under varying
varying thicknesses.
thicknesses.

3.3. Analysis
3.3. Analysis of
of Mechanical
Mechanical Properties
Properties

3.3.1. Tensile
3.3.1. Tensile Properties
Properties
According to
According to the
the parameter
parameter windowwindow in in Figure
Figure 6,6, the
the tensile
tensile pieces
pieces were
were carried
carried out
out with
with the
the
optimal parameters, 200 W for laser power (P), 1000 mm/s for scanning
optimal parameters, 200 W for laser power (P), 1000 mm/s for scanning speed (V), 30 µm for layerspeed (V), 30 µm for layer
thickness, 0.08
thickness, 0.08 mm
mm forfor hatch
hatch space
space and
and S-shaped
S-shaped orthogonal
orthogonal scanning
scanning strategy.
strategy. The
The orientation
orientation of of the
the
tensile pieces
tensile pieces was
was parallel
parallel toto the
the substrate.
substrate.
Figure 7 and Table 1 showthe
Figure 7 and Table 1 show thestress-strain
stress-straincurvecurveandand mechanical
mechanical properties,
properties, respectively,
respectively,of
SLM-fabricated
of SLM-fabricated Ti6Al4V
Ti6Al4V alloy withwith
alloy andandwithout heat heat
without treatment. Each set
treatment. Eachof data
set ofisdata
the mean
is theofmean
tests
ontests
of threeonsamples. It can be
three samples. It seen
can be that stress
seen thatsoars
stressdramatically with the
soars dramatically increasing
with of tensile
the increasing strain.
of tensile
Regardless
strain. of process
Regardless conditions,
of process the stress–strain
conditions, curve of
the stress–strain the SLM-fabricated
curve Ti6Al4V
of the SLM-fabricated alloy can
Ti6Al4V be
alloy
divided
can into three
be divided intostages: those ofthose
three stages: elastic
ofdeformation, yield, and
elastic deformation, dramatic
yield, decreasedecrease
and dramatic in stress.inPrior to
stress.
heat treatment, the stress–strain curve soared and decreased considerably
Prior to heat treatment, the stress–strain curve soared and decreased considerably during elongation during elongation of
Ti6Al4V, and clear necking was not observed. Elongation of the parts reached
of Ti6Al4V, and clear necking was not observed. Elongation of the parts reached 5.79% ± 0.29% prior 5.79% ± 0.29% prior to
failure,
to asas
failure, detailed
detailed ininTable
Table1,1,andandthethefracture
fracturetype
typewas
wasbrittle
brittle fracture
fracture by
by inference.
inference. ItIt can also be
can also be
determined from Table 1 that after heat treatment, the SLM-fabricated Ti6Al4V
determined from Table 1 that after heat treatment, the SLM-fabricated Ti6Al4V decreased in tensile and decreased in tensile
and yield
yield strength,
strength, butmet
but still still the
metASTM
the ASTMF136 F136 criteria
criteria of titanium
of titanium alloy alloy for medical
for medical purposes.
purposes. AfterAfter
heat
heat treatment,
treatment, its elongation
its elongation increased
increased to 10.28%
to 10.28% ± 0.20%.
± 0.20%.
Metals 2018, 8, 471 10 of 17
Metals 2018, 8, x FOR PEER REVIEW 10 of 17

Figure 7. Testing
Figure 7. Testingofoftensile
tensileproperties:
properties:(a)(a)tensile
tensile bars
bars with
with no no heat
heat treatment;
treatment; (b) tensile
(b) tensile bars bars
withwith
heat
heat treatment; (c) strain–stress curves of Ti6Al4V
treatment; (c) strain–stress curves of Ti6Al4V alloy. alloy.

Table
Table 1.
1. Tensile
Tensile properties
properties of
of Ti6Al4V before and
Ti6Al4V before and after
after heat
heat treatment.
treatment.

Manufacturing Method Tensile Strength/MPa Elongation/% Notes

Manufacturing Method Tensile Strength/MPa Elongation/% Notes
SLM 1240.5 ± 7.7 5.79 ± 0.29 -
SLM
SLM (Reference) 1267.0±±7.7
1240.5 5 5.79± ±
7.28 0.29
1.12 [20] -
SLM (Reference) 1267.0 ± 5 7.28 ± 1.12 840 °C for 3 h [20]+ tempering
SLM + Heat Treatment 1068.3 ± 26.7 10.28 ± 0.20 h +◦ C
for 2840 furnace
for 3 h cooling to
+ tempering
SLM + Heat Treatment 1068.3 ± 26.7 10.28 ± 0.20 4502 °C
for h ++air cooling
furnace cooling to
◦
SLM + Heat Treatment 705 °C 450
for 3Ch +air
+ aircooling
cooling
1082.0 ± 34.0 9.04 ± 2.03 ◦
(Reference
SLM one)
+ Heat Treatment 705 C for [20]
3 h + air cooling
1082.0 ± 34.0 9.04 ± 2.03
(Reference one) 940 °C for 1 h [20]+ tempering
SLM + Heat Treatment
948.0 ± 27.0 13.59 ± 0.32 h at◦ 650
for 2 940 C for°C1 h+ +
airtempering
cooling
SLM + Heat Treatment
(Reference two) 948.0 ± 27.0 13.59 ± 0.32 at 650 ◦ C + air
for 2 h[20]
(Reference two)
cooling [20]
Ti6Al4V Alloy Forgings ≥895.0 ≥10.00 ASTM B381-05
Ti6Al4VAlloy
Ti6Al4V Alloyfor
Forgings
Surgical ≥895.0 ≥10.00 ASTM B381-05
≥860.0 ≥10.00 ASTM F136-12
Implant
Ti6Al4V Application
Alloy for Surgical
≥860.0 ≥10.00 ASTM F136-12
Implant Application

Furthermore, after annealing at about 700–950 °C, UTS (ultimate tensile strength) decreased by
aboutFurthermore,
200 Mpa, and theannealing
after elongation at improved
about 700–950with◦ C,
increasing temperature
UTS (ultimate and was enhanced
tensile strength) decreased by
nearly 4–9%.
about 200 Theand
Mpa, results
the show that after
elongation heat treatment,
improved the titanium
with increasing alloy hadand
temperature better
wasductility
enhanced while
by
reducing the The
nearly 4–9%. strength,
resultswhich
show is in after
that line with Zhang’s research
heat treatment, [10]. alloy
the titanium From hadTable 1, compared
better with
ductility while
published
reducing theliteratures, there
strength, is still
which some
is in linework
withfor improvement
Zhang’s researchin[10].
our heat
From treatment
Table 1,results,
comparedalthough
with
the influence
published of different
literatures, therescanning
is still somestrategies
work forshould be considered.
improvement According
in our heat to results,
treatment the principle
althoughof
maximum
the influence temperature
of differentand cooling
scanning rates [20,31],
strategies shouldabegroup of moreAccording
considered. refined experiments could
to the principle of
contribute to a detailedand
maximum temperature description
cooling ratesin the microstructure
[20,31], evolution.
a group of more refinedInexperiments
fact, the balance of tensile
could contribute
strength and description
to a detailed elongation through heat treatmentevolution.
in the microstructure is more determined
In fact, theby an actual
balance application’s
of tensile strength need.
and
elongation through heat treatment is more determined by an actual application’s need.
Metals 2018, 8, 471 11 of 17

Metals 2018, 8, x FOR PEER REVIEW 11 of 17

3.3.2. Micro-Hardness
3.3.2. Micro-Hardness
The three groups of micro-hardness samples were formed by the same optimal parameters of
The three
tensile pieces, andgroups of micro-hardness
the heat treatment parameter sampleswas were
alsoformed by the
the same. Fivesame optimal
testing points parameters
were taken ofon
tensile pieces, and the heat treatment parameter was also the same. Five testing points
the surface of each sample for micro-hardness testing. The spacing of the test points was 2 mm, and were taken on
thethe surface
results of of each sample for
micro-hardness micro-hardness
are shown in Figure testing. The spacing
8. Figure of sample
8a is the the test points
without was 2 mm,
heat and
treatment,
the results of micro-hardness are shown in Figure 8. Figure 8a is the sample without heat treatment,
and Figure 8b is the sample after heat treatment. The comparison found that the surface indentation
and Figure 8b is the sample after heat treatment. The comparison found that the surface indentation
side length (D1 ≈ D2 = 72.8 µm) of the no heat treatment’s sample surface was slightly smaller
side length (D1 ≈ D2 = 72.8 µm) of the no heat treatment’s sample surface was slightly smaller than
than that of the surface indentation of the sample surface after heat treatment (D1 ≈ D2 = 73.5 µm).
that of the surface indentation of the sample surface after heat treatment (D1 ≈ D2 = 73.5 µm).
The average micro-hardness value of the upper surface of the SLM directly-made Ti6Al4V alloy was
The average micro-hardness value of the upper surface of the SLM directly-made Ti6Al4V alloy was
373.67 ± 5.33 HV1. After the heat treatment, the average micro-hardness value was measured at
373.67 ± 5.33 HV1. After the heat treatment, the average micro-hardness value was measured at
367.67 ± ±7.33
367.67 7.33HV1.
HV1.Wang
Wangetetal.al.[31]
[31]chose
chose aa 1000
1000 mm/s scanningspeed
mm/s scanning speedtotobuild
builda aspecimen
specimen with
with a a
hardness ofofabout ◦
hardness about400
400HV.
HV.Vilaro
Vilaroetetal.
al.[32]
[32]found
found that
that the samplewas
the sample wasannealed
annealedatat800–850
800–850 °C, C,
andand
thethe
hardness decreased by about 20 HV after cooling, which was closely related to
hardness decreased by about 20 HV after cooling, which was closely related to the precipitation the precipitation
of of
α phase. ◦ C [31],
α phase.Moreover,
Moreover,thethehardness
hardness cancan be
be reduced
reduced by by about
about35 35HV
HVwhenwhenannealing
annealing at at
875875°C [31],
although
althoughthethe
hardness
hardnessofofthe
thesample
samplewas wasslightly
slightly reduced after heat
reduced after heattreatment.
treatment.

Figure
Figure 8. 8.Measurement
Measurementpoints
points and
and results
results of
of micro-hardness
micro-hardnesstesting
testingfor
forthe
theSLM
SLMTi6Al4V sample:
Ti6Al4V sample:
(a) before heat treatment; (b) after heat treatment.
(a) before heat treatment; (b) after heat treatment.

3.4. Mechanical Evolution Mechanism

3.4. Mechanical Evolution Mechanism
Pederson et al. clarified the mechanism for the change in properties of SLM-fabricated titanium
Pederson et al. clarified the mechanism for the change in properties of SLM-fabricated titanium
alloy following heat treatment, and they summarized the alloy phase diagram [33]. The β phase
alloy following temperature
transforming heat treatment, and they
for Ti6Al4V is summarized
990 ± 5 °C. If the the alloy phase diagram
temperature heats up [33].
more The
than βthephase
β
transforming temperature for Ti6Al4V is 990 ± 5 ◦ C. If the temperature heats up more than the
phase transforming temperature, then β phase would grow quickly and become a coarse structure, β
phase transforming
leading temperature,
to the increase then
in plasticity andβaphase
decreasewould grow quickly
in strength. The heatand becomeprocess
treatment a coarsewasstructure,
set as
leading to the increase in plasticity and a decrease in strength. The heat treatment
follow: temperature was heated up to 840 °C over 3 h, the temperature was maintained for 2 h, then process was set as
follow: temperature was heated ◦
up to 840reduced
C overto3 450
h, the
the furnace cooled until the temperature °C temperature was maintained
and subsequently cooled by air.for 2 h, then
the furnace cooled until structures
the temperature reduced to 450titanium◦ C and subsequently cooled by air.
The microcosmic of the SLM-fabricated alloy following heat treatment were
The microcosmic
inspected, as shown in structures
Figure 9. of the SLM-fabricated
Morphology of the alloy’stitanium alloy following
microcosmic heat treatment
structure along the directionwere
of laser scanning
inspected, as shown inin
theFigure
X–Y plane without heat
9. Morphology oftreatment
the alloy’s is presented
microcosmicin Figure 9a. Italong
structure can bethe
observed
direction
of that
laserprior to heat
scanning intreatment,
the X–Y planeit consisted
without mainly of acicularismartensite
heat treatment presentedα’inand β phases.
Figure 9a. It The
can reason for
be observed
this is that during rapid cooling of Ti6Al4V, and new columnar β crystals formed.
that prior to heat treatment, it consisted mainly of acicular martensite α’ and β phases. The reason for Before diffusion
can
this is occur, the alloy
that during elements
rapid coolingareofconverted
Ti6Al4V,intoandan newoversaturated
columnar βsolid solution
crystals whichBefore
formed. has the same
diffusion
cancomposition of theelements
occur, the alloy parental are
phase but withinto
converted a different crystal structure
an oversaturated (i.e., α’ phase
solid solution whichmartensite).
has the same
It can be seen from Figure 9a that the acicular martensite α’ phase exists in abundance. Note that
Metals 2018, 8, 471 12 of 17

Metals 2018, 8, x FOR PEER REVIEW 12 of 17

composition of the parental phase but with a different crystal structure (i.e., α’ phase martensite). It can
be seen from
martensite is Figure 9a that
principally the acicular martensite
characterized α’ phase
by high strength and exists in abundance.
hardness. Its ductilityNoteandthattenacity
martensite
are
is
dependent on the substructure of martensite (lath martensite is superior to acicular martensite on
principally characterized by high strength and hardness. Its ductility and tenacity are dependent in
the substructure
tenacity). of martensite
Therefore, (lath martensite
SLM-fabricated is superior
Ti6Al4V features to acicular
high strengthmartensite in tenacity).
and low elongation Therefore,
prior to heat
SLM-fabricated
treatment. As shown Ti6Al4V features9b,
in Figure high
thestrength
α’ phaseand lowtremendously
grows elongation prior andtoisheat treatment.
dispersed in theAsβshown
phase
in Figure 9b, the α’ phase grows tremendously and is dispersed in the
after recrystallization and annealing. The reason is that when the heat treatment temperature β phase after recrystallization
and annealing.toThe
approximates thereason
β phase is conversion
that when the heat treatment
temperature, β phasetemperature
nucleation approximates
occurs alongto the
the β phase
boundary
conversion temperature,
of the α’ phase. The closer phase
β the nucleationisoccurs
temperature to the along
phasethechangeboundary of the α’the
temperature, phase.
higherThethe
closer the
content
temperature is to the phase change temperature, the higher the content
of the β phase. As the acicular martensite α’ phase converts into the layered α+β double-phase of the β phase. As the acicular
martensite
structure, theα’ phase converts
material’s into theimproves
elongation layered α+β double-phase
accordingly. The structure,
above results the material’s elongation
can also explain the
improves accordingly. The above results can also explain the reason why
reason why micro-hardness of SLM-ed Ti6Al4V alloy had a slight decline after heat treatment; it is micro-hardness of SLM-ed
Ti6Al4V
due to thealloy had SLM-ed
fact that a slight Ti6Al4V
decline after heat treatment;
microstructures were itcomposed
is due toofthe thefact thatand
brittle SLM-ed
toughTi6Al4V
acicular
microstructures were composed of the brittle and tough acicular α’ phase
α’ phase martensite. However, the α’ phase martensite would change to a layered α+β double-phase martensite. However, the α’
phase
and it martensite
leads to thewould change to adecline.
micro-hardness layeredSallica-Leva
α+β double-phase
et al. [34]andalso
it leads to the
studied themicro-hardness
malleability of
decline. Sallica-Leva et al. [34] also studied the malleability of
SLM-fabricated titanium alloys using different heat treatments and concluded that theSLM-fabricated titanium alloys using
α’ phase
different heat treatments
decomposition and
is critical toconcluded
improvements that theinα’malleability,
phase decomposition is critical
which proves ourto improvements
findings in this in
malleability, which proves our findings in this experiment. After analyzing
experiment. After analyzing fracture morphology of the SLM-fabricated titanium alloy Ti6Al4V, it is fracture morphology of the
SLM-fabricated
revealed that due titanium
to heatalloy Ti6Al4V,
treatment, it is deeper
many revealed that due
dimples to heat
were treatment,
uniformly many deeper
distributed acrossdimples
a large
were uniformly distributed across a large area within tensile fractures of the parts.
area within tensile fractures of the parts. It further confirms the conversion of the fabricated titanium It further confirms
the
alloyconversion of the fabricated
from quasi-cleavage fracture titanium alloy
to ductile from quasi-cleavage fracture to ductile fracture.
fracture.

Figure 9. Surface micro-structure of Ti6Al4V alloy: (a) before heat treatment; (b) after heat treatment
Figure 9. Surface micro-structure of Ti6Al4V alloy: (a) before heat treatment; (b) after heat treatment
(α phase is bright, β phase is dark).
(α phase is bright, β phase is dark).

In order to further analyze the mechanisms of tensile property variation in the SLM-fabricated
Ti6Al4V alloy after heat treatment, the morphologies of tensile fractures were inspected. Figure 10
presents tensile fractures of SLM-fabricated Ti6Al4V alloy. Figure 10b shows the fractured parts after
heat treatment. It can be seen that the morphology of the tensile fracture resembles honeycombs with
Metals 2018, 8, 471 13 of 17

In order to further analyze the mechanisms of tensile property variation in the SLM-fabricated
Ti6Al4V alloy after heat treatment, the morphologies of tensile fractures were inspected. Figure 10
Metals 2018, 8, x FOR PEER REVIEW 13 of 17
presents tensile fractures of SLM-fabricated Ti6Al4V alloy. Figure 10b shows the fractured parts after
aheat treatment.
number It can
of small be seen
holes that at
present thethe
morphology
fracture. Thisof the is tensile
the most fracture resembles
fundamental honeycombs
criterion with
for fragile
a number of small holes present at the fracture. This is the most fundamental
fracture or ductile fracture. In addition, the size and depth of the dimples are related to the material’s criterion for fragile
fracture orItductile
ductility. can be fracture.
deduced Infromaddition,
Figurethe10b,size and depth
following heatoftreatment,
the dimples arethe
that related
dimplesto the material’s
in the tensile
ductility. It can be deduced from Figure 10b, following heat treatment, that
fracture are large and deep, creating a ductile fracture. Figure 10c,d show fractures of parts withoutthe dimples in the tensile
fracture
heat are large
treatment. and deep,
Many creating
cleavage planes a ductile
and torn fracture.
edges with Figure 10c,d
local showdeformation
plastic fractures of areparts without
present in
heat treatment. Many cleavage planes and torn edges with local plastic deformation
this fracture, in addition to a small number of dimples. Figure 10d shows that clear cleavage bands are present in this
fracture,
are in addition
present to a small number
at the microcosmic surface of dimples. Figure
morphology of the10d shows
tensile that clear
fracture. Some cleavage
dimplesbands are
are also
present
present at at the
themicrocosmic
edges, whichsurface morphology
are small and shallow.of theIttensile
indicates fracture. Some dimples
that although are also
the parts havepresent
tenacity,at
the edges, which are small and shallow. It indicates that although the parts
the ductility is limited. Therefore, the fracture of the Ti6Al4V sample without heat treatment is a have tenacity, the ductility
is limited. Therefore,
quasi-cleavage the In
fracture. fracture
fact, itofisthe Ti6Al4V sample
meaningful to discuss without heat
failure treatment isfrom
mechanisms a quasi-cleavage
the view of
fracture. In fact, it is meaningful to discuss failure mechanisms from the
macroscopic fracture morphology. In recent work published in [35,36], even in a smooth forming view of macroscopic fracture
surface, roughness might lead to the origination of fatigue crack which would further evolve might
morphology. In recent work published in [35,36], even in a smooth forming surface, roughness into a
lead toinitiation
crack the origination
point. of fatigue crack which would further evolve into a crack initiation point.

Figure 10. SEM images of fracture morphology of tensile testing: (a) thermally treated sample (500×);
Figure 10. SEM images of fracture morphology of tensile testing: (a) thermally treated sample (500×);
(b) thermally treated sample (5000×); (c) as built sample (500×); (d) as built sample (2000×).
(b) thermally treated sample (5000×); (c) as built sample (500×); (d) as built sample (2000×).

3.5. Discussion
3.5. Discussion
Figures 3 and 4 show that, except for the smooth forming zone, the surface morphology of the
Figures 3 and 4 show that, except for the smooth forming zone, the surface morphology of the
other zones all had defects. Track deformation and concavity occurred within the over-melting zone.
other zones all had defects. Track deformation and concavity occurred within the over-melting zone.
The reason is that the high density of linear energy input lengthens the cooling and solidification
The reason is that the high density of linear energy input lengthens the cooling and solidification
process of the track. As a result, the melting pool absorbs the powder at both sides more easily, leading
process of the track. As a result, the melting pool absorbs the powder at both sides more easily, leading
to convexity. The convexity at the initial layer will not cause defects or other adverse influence on the
to convexity. The convexity at the initial layer will not cause defects or other adverse influence on the
fabrication of parts. But it does affect powder coating at the next layer. This problem deteriorates in
fabrication of parts. But it does affect powder coating at the next layer. This problem deteriorates in
subsequent layers and may well cause failure of the fabrication process. Spattering happens throughout
subsequent layers and may well cause failure of the fabrication process. Spattering happens throughout
the process, and its generated principle can be depicted, as Figure 11 shows, where one can see several
types of spatter which formed during laser interaction with powder. As discussed in [21], particle
spattering was mostly attributed to recoil pressure caused by instantaneous melting or even steaming
of laser and powder. Another reason is that gas in the powder that is rapidly heated results in instantly
swelling volume, propelling the powder to the solidification layer. Spattered particles are inserted at
Metals 2018, 8, 471 14 of 17

the process, and its generated principle can be depicted, as Figure 11 shows, where one can see several
types of spatter which formed during laser interaction with powder. As discussed in [21], particle
spattering was mostly attributed to recoil pressure caused by instantaneous melting or even steaming
of laser
Metals and
2018, 8, powder.
x FOR PEER Another
REVIEWreason is that gas in the powder that is rapidly heated results in instantly14 of 17
swelling volume, propelling the powder to the solidification layer. Spattered particles are inserted
thethe
at surface
surface or orinterior of of
interior thethe
SLM-fabricated
SLM-fabricated parts, reducing
parts, reducingthethe
quality of of
quality thethe
powder
powder coating
coatingin
addition
in addition to tothethedensity
densityandandperformance
performanceofofthethe fabricated
fabricated parts.
parts. As
As for
for the low-energy
low-energy density
density
nodulizing zone, there are both both non-melted
non-melted powder
powder andand ball-shaped
ball-shaped bulges
bulges at
at the
the surface.
surface. The reason
for this is that the linear energy density is so low that some powder does not have enough time to melt,
wettability of the liquid track is insufficient
and wettability insufficient for the
the already
already solidified
solidified zone. At the surface of thethe
sintering zone, almost no track is formed and the powder is mostly sintered.
almost no track is formed and the powder is mostly sintered.

Figure 11. Spatter generation mechanism when laser interact with powder
powder in
in SLM
SLM process.
process.

Based on
Based on the
the research
research in in this
this study
study andand the
the experience
experience we we have
have obtained
obtained fromfrom years
years of
of
experimentation, it is clear that the surface quality of fabricated parts strongly
experimentation, it is clear that the surface quality of fabricated parts strongly correlates with such correlates with such
critical metrics
critical metrics asas density
density and and hardness
hardness of of the
the parts.
parts. High-quality
High-quality fabrication
fabrication of of parts
parts can
can be
be ensured
ensured
by observing surface quality during the fabrication process and then flexibly
by observing surface quality during the fabrication process and then flexibly adjusting the energy adjusting the energy
input (i.e., laser power and scanning speed). A major bottleneck for SLM
input (i.e., laser power and scanning speed). A major bottleneck for SLM is the negative feedback in is the negative feedback in
the fabrication
the fabricationprocess
process [37].
[37]. ThereThere are dozens
are dozens of factors
of factors having enormous
having enormous influence influence on SLM
on SLM fabrication
fabrication quality. It is thus of great significance to flexibly adjust parameters
quality. It is thus of great significance to flexibly adjust parameters based on observations of one metricbased on observations
of one The
alone. metricSLM alone. The SLMand
solidification solidification
melting pool andismelting pool(typically
very small is very small100 mm (typically 100 mm
in diameter), in
and
diameter), speed
processing and processing
is usually speed
in the is usually
range in themaking
1–3 m/s, range it1–3 m/s, making
extremely it extremely
difficult to performdifficult to
real-time
perform real-time monitoring and feedback control on SLM. In this paper,
monitoring and feedback control on SLM. In this paper, surface morphology of SLM-fabricated titanium surface morphology of
SLM-fabricated
alloy is classifiedtitanium
into five alloy is classified
categories. A CCDinto five categories.
(central A CCDoptical
composite design) (centralvision
composite
devicedesign)
can be
optical vision device can be adapted to capture the layer-wise surface of
adapted to capture the layer-wise surface of the SLM-fabricated parts at certain frequencies, and the SLM-fabricated parts at
then
certain frequencies, and then measure the surface status of each layer. Subsequently,
measure the surface status of each layer. Subsequently, defects in the fabricated layers can be detected defects in the
fabricated
using layersimage
real-time can beprocessing
detected using real-time
techniques andimage processing
the reasons for the techniques
defects can andbethe reasons In
analyzed. forthis
the
defects can be analyzed. In this way, robustness and repeatability of
way, robustness and repeatability of SLM-fabricated parts can be improved significantly. Figure 12SLM-fabricated parts can be
improved significantly. Figure 12 shows the surface morphology, sparking
shows the surface morphology, sparking comparisons between two typical fabrication processes. comparisons between two
typical
It can befabrication
seen fromprocesses.
Figure 12aItthat can the
be parts
seen from
have Figure
a rough12a that the
surface, parts have
irregular a rough
sparking and surface,
spatter.
In Figure 12b, the parts have a smooth melting surface, while the melting layer has regularwhile
irregular sparking and spatter. In Figure 12b, the parts have a smooth melting surface, the
sparking
melting layer has regular sparking but no spatter. Without observing its microcosmic
but no spatter. Without observing its microcosmic structure, the fabricated parts in Figure 12b have a structure, the
fabricated
denser parts in structure
microcosmic Figure 12b andhavestrongera denser microcosmic
mechanical structure and stronger mechanical
properties.
properties.
Another important benefit arising from the research on parameters associated with the
fabrication of titanium alloy is improvement to SLM fabrication efficiency. The traditional method
for greater efficiency is to adjust the parameters based on relationships with energy input. But these
relationships are impossible to be clarified without considerable efforts. Our experiment reveals that
given the smooth forming conditions, the energy density ratio P/V is not fixed, and that the value of
Metals 2018, 8, 471 15 of 17

Another important benefit arising from the research on parameters associated with the fabrication
of titanium alloy is improvement to SLM fabrication efficiency. The traditional method for greater
efficiency is to adjust the parameters based on relationships with energy input. But these relationships
are impossible to be clarified without considerable efforts. Our experiment reveals that given the
smooth forming conditions, the energy density ratio P/V is not fixed, and that the value of P/V is not
Metals 2018, 8, x FOR PEER REVIEW 15 of 17
linearly correlated with the range of optimized parameters. Therefore, in order to improve fabrication
efficiency
fabricationwithout compromising
efficiency part quality,part
without compromising the optimal
quality, values of thevalues
the optimal speed need
of thetospeed
be chosen from
need to be
Figure
chosen6from
based on layer
Figure thickness
6 based andthickness
on layer power. and power.

Figure 12. Surface morphology and sparking of two typical SLM fabrication processes: (a) rough
Figure 12. Surface morphology and sparking of two typical SLM fabrication processes: (a) rough
surface without regular sparking and spatter formed; (b) fine surface with regular sparking and no
surface without regular sparking and spatter formed; (b) fine surface with regular sparking and no
spatter formed.
spatter formed.

4. Conclusions
4. Conclusions
A full-factor experiment was performed in this study to optimize the parameters for SLM
A full-factor experiment was performed in this study to optimize the parameters for SLM
fabrication of titanium alloy. The SLM-fabricated parts were classified into different categories. The
fabrication of titanium alloy. The SLM-fabricated parts were classified into different categories.
parameter windows of the smooth forming zone were explored. The mechanisms concerning the
The parameter windows of the smooth forming zone were explored. The mechanisms concerning
improvement of ductility of the SLM-fabricated titanium alloy were investigated. The major
the improvement of ductility of the SLM-fabricated titanium alloy were investigated. The major
conclusions were as follows:
conclusions were as follows:
1. From the perspective of surface morphology, a full-factor experiment was performed to classify
1. the
From the perspective
SLM-fabricated of surface
titanium alloymorphology, a full-factor
into five zones: experiment zone,
severe over-melting was performed
high-energy to density
classify
the SLM-fabricated titanium alloy into five zones: severe over-melting zone,
nodulizing zone, smooth forming zone, low-energy density nodulizing zone, and sintering high-energy density
zone.
2. An optimal parameter window was established for the smooth forming zone. It was foundzone.
nodulizing zone, smooth forming zone, low-energy density nodulizing zone, and sintering that
2. for
Antheoptimal
linearparameter window
energy density was
of the established
smooth formingfor zone,
the smooth forming
the upper zone. limits
and lower It wasincrease
found that by
for the linear energy density of the smooth forming zone, the upper and lower limits
a large margin. Moreover, the two limits also increase considerably with a rise in layer thickness. increase by
a large margin. Moreover, the two limits also increase considerably with a rise in layer
It refutes the conclusion in some studies that there is a linear relationship between energy input thickness.
It refutes
and qualitytheofconclusion
fabricated in some studies that there is a linear relationship between energy input
parts.
and SLM-fabricated
3. The quality of fabricated parts.
titanium alloy was annealed using an appropriate heat treatment. After heat
3. treatment,
The SLM-fabricated
the structure of thealloy
titanium alloywas
wasannealed
convertedusing
froman appropriate
acicular heat treatment.
martensite α’ phase toAfter heat
a layered
treatment,
α+β the structure
double-phase of theFracture
structure. alloy wastype
converted
was alsofrom acicular from
converted martensite α’ phase tofracture
quasi-cleavage a layered
to
α+β double-phase structure. Fracture type was also converted from quasi-cleavage
ductile fracture. This is the reason for improvement in ductility of SLM-fabricated titanium alloy. fracture to
ductile fracture. This is the reason for improvement in ductility of SLM-fabricated titanium alloy.
Author Contributions: Conceptualization, D.W., Y.Y.; Data curation, D.W., W.D.; Form analysis, D.W., W.D.;
Supplementary Materials:
Funding acquisition, The following
D.W., Y.Y.; are available
Investigation, online
D.W., W.D.; at www.mdpi.com/xxx/s1,
Methodology, D.W., W.D.; ProjectFigure S1. Severe
administration,
over-melting zone, D.W.,
Y.Y.; Supervision, Figure Y.Y.;
S2. High energy density
Visualization, W.D.;nodulizing zone, Figure
Writing—original S3. D.W.,
draft, Smooth forming
W.D.; zone, Figure S4.
Writing—review &
Low energy density nodulizing zone, Figure S5. Sintering zone; Table S1: Composition of Ti6Al4V powder.
editing, D.W., W.D., Y.Y. The authors would also want to express thanks to Master Hui Lin for his help on the
Author Contributions:
microstructure Conceptualization,
characterization D.W.,
and mechanical Y.Y.; Data
testing in thiscuration, D.W., W.D.; Form analysis, D.W., W.D.;
experiment.
Funding acquisition, D.W., Y.Y.; Investigation, D.W., W.D.; Methodology, D.W., W.D.; Project administration, Y.Y.;
Funding: This
Supervision, research
D.W., Y.Y.; was funded byW.D.;
Visualization, the National Natural Science
Writing—original draft, Foundation
D.W., W.D.; of China, grant number
Writing—review 51775196;
& editing, D.W.,
the Guangdong Province Science and Technology Project, grant numbers 2017B090912003, 2017A050501058,
2016B090914002, 2014B010131002, and 2015B090920002; the High-level Personnel Special Support Plan of
Guangdong Province, grant number 2016TQ03X289; the Guangzhou Pearl River New Talent Project, grant
number 201710010064; the Guangzhou Major Science and Technology Research for People’s livelihood through
CEEUSRO Collaborative Innovation, grant number 20150802005. Di Wang thanks the China Scholarship Council
for the award to study for one year at the University of Birmingham, grant number 201706155082.
Metals 2018, 8, 471 16 of 17

W.D., Y.Y. The authors would also want to express thanks to Master Hui Lin for his help on the microstructure
characterization and mechanical testing in this experiment.
Funding: This research was funded by the National Natural Science Foundation of China, grant number 51775196;
the Guangdong Province Science and Technology Project, grant numbers 2017B090912003, 2017A050501058,
2016B090914002, 2014B010131002, and 2015B090920002; the High-level Personnel Special Support Plan of
Guangdong Province, grant number 2016TQ03X289; the Guangzhou Pearl River New Talent Project, grant
number 201710010064; the Guangzhou Major Science and Technology Research for People’s livelihood through
CEEUSRO Collaborative Innovation, grant number 20150802005. Di Wang thanks the China Scholarship Council
for the award to study for one year at the University of Birmingham, grant number 201706155082.
Conflicts of Interest: The authors declare no conflict of interest.

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