Scripta Materialia 226 (2023) 115209

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Scripta Materialia
journal homepage: www.journals.elsevier.com/scripta-materialia

Rapid hardening response of ultra-hard Ti-6Al-2Sn-4Zr-6Mo alloy produced

by laser powder bed fusion
Huizhi Peng a, b, Shun Wu a, b, Wen Hao Kan a, b, Samuel Chao Voon Lim a, b, Yuman Zhu a, b, *,
Aijun Huang a, b, *
a
Monash Centre for Additive Manufacturing, Monash University, Notting Hill, VIC 3168, Australia
b
Department of Materials Science and Engineering, Monash University, Clayton, VIC 3800, Australia

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

Keywords: Post heat treatment is essential for additively manufactured alloys to eliminate residual stress and in some cases
Titanium alloy further improve mechanical performance. This study systematically investigated the hardening response of a Ti-
Laser powder bed fusion 6Al-2Sn-4Zr-6Mo alloy processed by laser powder bed fusion (LPBF) to a one-step heat treatment. The results
Isothermal heat treatments
revealed significant hardening at both 500 ◦ C and 650 ◦ C. Most notably, an ultra-high peak-hardness of 563VHN
Martensitic phase transformation
was achieved within 5 mins of heat treatment at 650 ◦ C due to a unique martensite-decomposed α+β micro­
structure consisting of alternating long β laths that are ~5 nm thick and α laths that are ~35 nm thick, and within
the α laths are also short β laths that are ~2 nm thick with an ~11 nm inter-spacing. The influence of both types
of β laths on the α lath thickness was established and related to the ultra-high hardness observed, which provides
new insight for the design of new metastable LPBF-processed Ti alloys.

Ti-6Al-2Sn-4Zr-6Mo (wt.%) (Ti-6246) is a commercial near-β Ti alloy Ti-6246 in the as-built condition had orthorhombic martensite (α′′ )
that possesses excellent corrosion resistance and high strength [1–3]. microstructure, which naturally exhibited a low hardness (~350VHN
Those desired properties make Ti-6246 widely used in aerospace ap­ [13]). Thus, various post heat treatment schemes have been explored to
plications. In addition, Ti-6246 is also used in the oil and gas industries decompose the martensite and thus harden the material [13,15]. While a
as the harsh service environments require excellent corrosion and wear hardness of 365VHN could be achieved after a 600 ◦ C heat treatment for
resistance, with the latter often associated with high hardness. However, 2 h [15], this hardness value is still lower than conventionally-processed
in addition to the naturally poor thermal conductivity of Ti alloys, Ti-6246, where 460VHN can be achieved by ageing for 30 min [16].
wear-resistant and hard materials are difficult to process via conven­ Therefore, a more effective heat treatment strategy is required to
tional “subtractive” manufacturing processes which leads to high pro­ decompose martensite and harden the LPBF Ti-6246 alloy. It should be
cessing costs [4–6]. In recent years, additive manufacturing (AM) noted that the intrinsic heat treatment during additive manufacturing
technology has experienced rapid development due to its ability to has been utilized for Ti alloys to achieve peritectic microstructure [17]
manufacture complex-shaped components with minimal machining or in-situ decomposition of hexagonal martensite (α′ ) to α+β lamellar
required. More importantly, in the oil and gas industry, components are microstructure for better mechanical performance [18–20]. However,
often located at remote sites. AM can enable on-site production and the intrinsic heat treatment was suggested to be less energy-efficient and
improve the efficiency of material supply chains, facilitating rapid it may result in oxidation and influence powder recyclability [21]. On
replacement of worn-out parts thus minimizing the financial losses the other hand, well-designed post-AM heat treatments have shown
associated with production downtime due to part failure [7–10]. Owing their capability in Ti alloys to optimise α and β microstructure [22] via
to these advantages, the Ti-6246 alloy has been recently considered for martensite decomposition in terms of controlled α thickness and volume
AM [11–15]. fraction [23,24], and eventually to achieve much enhanced mechanical
A recent study has shown that a relative density of 99.8% can be properties [25–28]. However, as essential information for microstruc­
achieved in Ti-6246 that has been processed by laser powder bed fusion ture and heat treatment design, the understanding of how the micro­
(LPBF), which is one of the major AM techniques [13]. However, LPBF structure of LPBF-processed Ti-6246 evolves during heat treatment is

* Corresponding authors.
E-mail addresses: [email protected] (Y. Zhu), [email protected] (A. Huang).

https://doi.org/10.1016/j.scriptamat.2022.115209
Received 9 August 2022; Received in revised form 23 November 2022; Accepted 25 November 2022
Available online 1 December 2022
1359-6462/© 2022 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
H. Peng et al. Scripta Materialia 226 (2023) 115209

Fig. 1. (a) Hardness curves of the LPBF-fabricated Ti-6246 samples after being subjected to a one-step post heat treatment at 500 ◦ C or at 650 ◦ C as a function of heat
treatment time; (b) XRD line profiles showing the peaks that resulted from the different phases present in the as-built condition and after being subjected to post heat
treatments at 650 ◦ C for 1 min, 5 mins and 6 h.

currently limited. Thus, this work investigates the microstructure evo­

Table 1
lution and the corresponding hardening response of LPBF-processed
Phases and their lattice parameters determined by the XRD spectra.
Ti-6246 samples that have been subjected to a single-step post-process
heat treatment. Conditions Lattice parameters b/a Phases
The Ti-6246 powder used for the LPBF process was purchased from a (Å) b (Å) c (Å)
Avimetal Powder Metallurgy Technology Co., Ltd, China. All specimens As-built 3.047 4.946 4.661 1.623 α′′
were fabricated using the Concept Laser Xline 2000R system with a laser Under-aged (1 min) 2.960 5.058 4.668 1.709 α′′ lean
power of 270 W, a scanning speed of 1600 mm/s, a layer thickness of 60 3.100 4.647 4.613 1.499 α′′ rich
μm, and a hatch spacing of 90 μm. The subsequent heat treatments were Peak-aged (5 min) 2.944 4.678 α
3.219
conducted in a muffle furnace at 500 ◦ C and 650 ◦ C followed by water
β
Over-aged (6 h) 2.937 4.688 α
quenching. The heat treatment time is counted since the sample entre 3.249 β
the furnace. Micro-hardness tests were carried out using the Struers
Duramin A300 Hardness Tester with the load of 3kgf and the dwell time
of 5 s. Eight indentations were measured for each condition. The aver­ value of ~400 VHN. Under the 500 ◦ C heat treatment, the hardness
aged value of the 8 indentations was used as the final hardness. A Bruker gradually increases to the peak value of 595 ± 10VHN at 66 h. Then, this
D8 Advance X-ray Diffractometer equipped with a Cu Ka X-ray source value decreases until ~540 VHN at 200 h. At 650 ◦ C, in comparison, the
was used for the X-ray diffraction (XRD) line scanning tests. They were ageing hardening is much faster. The peak hardness of 563±7 VHN is
performed at 40 kV and 40 mA with a step size of 0.005◦ and a dwelling achieved quickly within 5 mins. Then, the hardness decreases to
time of 8 s. The scanning electron microscopy (SEM) specimens were 465VHN at 48 h.
prepared by mechanically grinding and polishing. The SEM images were In order to reveal the cause of the exceptional hardening response,
acquired in the FEI Magellan 400 FEG SEM. The specimens for trans­ XRD was first used to evaluate changes in the microstructure due to the
mission electron microscopy (TEM) were cut and grinded into foils with post-process heat treatment at 650 ◦ C, with the XRD profile of each
a thickness of approximately 250 µm and punched into discs with a analysed sample shown in Fig. 1(b) and the calculated lattice parameters
diameter of 3 mm. Then the discs were mechanically thinned to about for each phase present shown in Table 1. According to the XRD line
55 µm and further thinned using the precision ion polishing system profile of the as-built condition, all peaks correspond to an orthorhombic
(PIPS-II). Conventional TEM images, including bright-field (BF) images martensite phase (α′′ ) with the lattice parameters of a = 3.047 Å, b =
and selective area diffraction (SAD) patterns, were obtained on a FEI 4.946 Å and c = 4.661 Å. An as-built fully martensitic microstructure for
Tecnai G2 T20 TWIN TEM at 200 kV and a FEI Tecnai G2 F20 S-TWIN this alloy has been reported in other LPBF studies [13–15]. Further in­
TEM at 200 kV. The scanning transmission electron microscopy (STEM) spection of the XRD data for the over-aged sample revealed the presence
images, including bright-field scanning transmission electron micro­ of the hexagonal α phase and the body-centred cubic β phase. This result
scopy (BF-STEM) images, high-angle annular dark-field scanning indicates that the α′′ phase in the as-built condition eventually de­
transmission electron microscopy (HAADF-STEM) images and corre­ composes into the α and β phases after prolonged heat treatment at
sponding energy dispersive X-ray (EDX) maps, were obtained on a FEI 650 ◦ C. To provide further insight on this decomposition process, XRD
Tecnai G2 F20 S-TWIN TEM at 200 kV. analysis was also conducted on under-aged (1 min) and peak-aged
Fig. 1(a) shows the hardness curves for the LPBF Ti-6246 aged at samples. Close inspection of the resulting XRD profiles revealed shifts
500 ◦ C and 650 ◦ C. In the as-built condition, the sample has a hardness in the peak positions between the under-aged and the peak-aged

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H. Peng et al. Scripta Materialia 226 (2023) 115209

Fig. 2. (a) SEM-BSE image showing elongated prior β grains along the build direction and the high number density of martensite laths existing within the prior β
grains of the LPBF-processed as-built sample; (b) BF-STEM image showing the martensite variants.

Fig. 3. (a) TEM bright-filed image of the peak

aged sample showing its general microstruc­
ture, and on the bottom-left corner shows a
higher magnification image of the selected area
where the morphology and distribution of the β
phase are indicated, as well as the diffraction
pattern inserted on the top-right corner; (b) The
STEM-HAADF image of an individual α lath and
the corresponding EDX maps of (c) Mo, (d) Al,
and (e) Ti, which shows the distribution of so­
lute atoms in the peak aged microstructure; (f)
BF-STEM image of the over-aged sample
(650 ◦ C/6 h) showing the morphology and
distribution of the α and β phases; (g) The
STEM-HAADF image of an individual α lath,
providing information inside the α laths and the
corresponding EDX maps of (h) Mo, (i) Al, and
(j) Ti, showing the distribution of solute atoms
in the over-aged microstructure.

conditions, especially for peaks with a 2θ angle exceeding 50◦ . Similar transition pathway during ageing at 650 ◦ C can be determined as α′′ →
phenomena have been observed in other studies [29–32] where two α′′ lean + α′′ rich→ α + β. More specifically, heat treatment causes solute
distinct martensitic zones have been defined - one rich in β stabilizing partitioning within the α’’ phase to form the α′′ lean and α′′ rich which
elements and the other lean (herein referred to as α′′ rich and α′′ lean, eventually transform into the α and β phases, respectively, that ulti­
respectively). On this basis, the peaks in the under-aged condition can be mately leads to the high peak-aged hardness observed.
well-indexed as α′′ rich or α′′ lean, with their calculated lattice parameters To provide further details on our identified phase transformation, in-
also shown in Table 1. Based on the above XRD analyses, the phase depth microstructural characterization was carried out. Fig. 2(a) is a

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H. Peng et al. Scripta Materialia 226 (2023) 115209

Fig. 4. (a) The relationship between hardness and the α lath thickness of LPBF Ti-6246, as illustrated by the red dashed line, based on the measurements obtained for
the samples that were aged at 650 ◦ C for 5 min, 6 h, 10 h and 12 h. Some hardness values and corresponding α thickness measured from conventionally-manufactured
Ti-6246 with evenly distributed lamella structure are also included for comparison; (b) hardness vs heat treatment time of additively manufactured and conventional
manufactured Ti-6246, showing the comparison between the peak-ageing treatment in our work and previously reported in the conventional [16,35–45] and
additively manufactured [13,15] Ti-6246. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

low-magnification SEM image showing the microstructure of the as-built Hardness is an indicator of resistance to plastic deformation [33].
LPBF-processed Ti-6246. As can be observed, the prior β grains have a High hardness generally indicates good wear resistance. In dual-phase Ti
width of ~ 10 μm and an aspect ratio larger than 10 distributed in the alloys with a lamellar or basket-weave microstructure, the relationship
microstructure. The long axis of the prior β grains is nearly parallel to the between hardness and α thickness has been previously described as
build direction. The inserted image in Fig. 2(a) is a high-magnification HV = HV0 + Kd− 0.5 , where HV is the Vickers hardness, HV0 is the
SEM image for the boxed region, showing numerous fine lamellar fea­ intrinsic hardness of the material, K is the Hall-Petch constant, and d is
tures present inside the prior β grains. These fine lamellae were further the α thickness [15,33,34]. Here, to reveal the cause of ultra-high
imaged using BF-STEM, as shown in Fig. 2(b). At least three α′′ variants hardness, in Fig. 4(a), we investigate the relationship between hard­
with a thickness of about 30 nm and an aspect ratio larger than 5 were ness and α thickness in LPBF Ti-6246. The α thicknesses in the different
found within the imaged area. overaged conditions (650 ◦ C 6 h, 10 h and 12 h) were measured to be
Fig. 3(a) shows the distribution and morphology of α and β phases in ~61 nm, 73 nm, and 82 nm, respectively. And the Hall-Petch equation
the peak-aged condition. From the image, there are two different types was used to fit the overaged conditions, determining intrinsic hardness
of lath features: long laths, as indicated by the blue arrow, aligned along (HV0) and Hall-Petch constant (K) as 424 VHN and 461 VHN*nm− 0.5. If
the vertical direction, and red-arrow-pointed short laths that are aligned this Hall-Petch equation can be extended to the range with hardness up
either along the horizontal or vertical directions. The long laths show a to 570VHN, the estimated α thickness corresponding to the peak-aged
thickness of ~ 5 nm and an aspect ratio exceeding 10. The spacing be­ hardness (563 VHN) is 11 nm. It is much lower than the α laths thick­
tween two neighbouring long laths was measured to be 35 ± 13 nm. In ness (i.e., the spacing between the long β laths) in the peak-aged con­
comparison, the short laths that are distributed between the long laths dition but consistent with the spacing between the short β plates within
have a thickness of ~2 nm and an inter-plate spacing of ~11 nm. Both the α laths. Therefore, in addition to the small thickness of the α laths in
long and short laths show brighter contrast than other areas in the the peak-aged microstructure, the presence of short β laths further re­
STEM-HAADF image, as shown in Fig. 3(b), which indicates the duces the effective α thickness, consequently contributing to the high
enrichment of heavy elements. This can be further evidenced by the hardness. In addition, the hardness and corresponding α thickness
corresponding STEM-EDX maps in Fig. 3(c-e) which show Mo enrich­ measured from conventionally-manufactured Ti-6246 with evenly
ment in both types of laths. Given that Mo is the β stabilizing element distributed α lamellae [35,36] are also included in Fig. 4(a). It appears
[1], these two laths are suggested to be the β phase despite their different they do not follow a simple Hall-Petch relationship. This could be
sizes. On this basis, the dark regions in Fig. 3(b) should correspond to the attributed to the distinct volume fractions of α-precipitates formed from
α-phase. Note, a similar structure was also observed in the 500 ◦ C variable heating temperatures applied in these works since the α volume
peak-aged condition. fraction is also a factor that may apparently affect the hardness.
With the ageing time prolonged to the overaged condition (650 ◦ C/6 Fig. 4(b) compared the hardness and heat treatment time between
h), a dense arrangement of α laths is observed, and the α laths exhibit a the peak-ageing treatment in our work and reported heat treatments for
thickness of about 61 nm, which is much thicker than those appearing in conventionally manufactured [16,35–45] or additively-manufactured
the peak-aged condition. STEM-HAADF and STEM-EDX were applied to [13,15] Ti-6246 alloys. Both the 500 ◦ C and 650 ◦ C peak-aged LPBF
an individual α lath in Fig. 3(g-j). Inside the α lath, no segregation of Ti-6246 alloy possessed hardness values higher than previous works. In
elements, including Mo, was observed. The fine β phase appears to terms of heat treatment strategy, Ti-6246 alloys subjected to martensite
dissolve as the microstructure coarsens. This α/β lamella structure is decomposition heat treatment generally have α/β lamella structure [13,
similar to a typical structure in ageing-hardened near β-Ti alloys [1]. 16,36,40,45–47]. To further harden the material, a typical method is to

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H. Peng et al. Scripta Materialia 226 (2023) 115209

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