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Microstructure and Mechanical Properties Investigation on Nanostructured

Nickel 200 Alloy Using Multi-Axial Forging

Article  in  Materials Science and Engineering A · December 2017

DOI: 10.1016/j.msea.2017.12.042

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 Materials Science & Engineering A 712 (2018) 772–779

Contents lists available at ScienceDirect

Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Microstructure and mechanical properties investigation on nanostructured T

Nickel 200 alloy using multi-axial forging
⁎
Zahid Hussaina, Fahad A. Al-Mufadia, Sivasankaran Subbarayana, , Osama M. Irfana,b
a
Mechanical Engineering Department, Qassim University, Buraidah 51452, Saudi Arabia
b
Mechanical Engineering Department, Beni-Suef University, Beni-Suef, Egypt

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

Keywords: Multiaxial Forging (MAF) is one of the novel severe plastic deformation techniques, which can be used to
Ni alloy produce nanostructured materials in large-scale production. This process is a simple one as it is not necessary to
Severe plastic deformation use special tooling. The present goal of this research work is to manufacture nanostructured Ni 200 alloy using
Multiaxial forging the multiaxial forging process at room temperature. The microstructural examination using various microscopes
Grain refinement
and mechanical properties evolution due to the variation of the number of cycle of forging (4 cycles) was
Mechanical properties
investigated. The observed results explained that the grain size of Ni 200 alloy was decreased significantly due to
Hardness
grain refinement. The rate of shifting of the microstructure to ultrafine and Nano regimes was variable as it was
remarkable after the first cycle of MAF and reduced significantly in subsequent cycles. The average grain size
after the third cycle was 220 nm. The results of uniaxial compression and hardness tests indicated a considerable
increase in strength and hardness.

1. Introduction of materials. The strength of this technique is that it may be used on

Recently, severe plastic deformation (SPD) technique [1–4] can be
used to enhance the mechanical properties of materials. SPD refers to
various metal forming techniques that can impose high strains on me-
tals and alloys in such a way that overall dimensions before and after
forming, are almost same [5–10]. For this, special tool geometries are
required to form materials to the desired shape by preventing them
flowing freely [1]. This method is used to increase the strength of
lightweight materials to an extent, which is not possible with other
thermo-mechanical processing methods [2]. Ultrafine and Nano
grained materials can be produced by this technique and the produced
materials are termed as Nano-SPD materials [2]. Various SPD techni-
ques are available, each has some advantages and some disadvantages.
Zahid et al. [3] reviewed a complete analysis of each technique. Some
of the major established techniques of SPD are equal channel angular
pressing (ECAP), high-pressure torsion (HPT), multiaxial forging
(MAF), accumulative roll bonding (ARB) and twist extrusion (TE). The
processing through all SPD techniques principally involves increasing
dislocation densities by imposing shear stress to the sample, the for-
mation of dislocation walls, which led to the formation of low angle
grain boundaries [4]. Multiaxial forging can be conventionally applied
at room and maximum temperature of one-third of melting temperature
large scale with greater ease as compared to other techniques without
compromising on the quality of microstructure and strength [5]. MAF
can be executed with open channel die or closed channel die. However,
it is the fact that more dimensional accuracy in the SPD samples could
be obtained using closed channel die, which is not attempted by many
researchers [6]. In this method, the sample is pressed to a fixed strain in
a specially designed die, removed and rotated to 90°, reinserted in the
die and the same amount of strain is applied again by pressing and so on
(Fig. 1). MAF is widely used for the production of ultrafine-grained
(UFG) and Nano grains (NG) materials and can be used to process the
copper [7], magnesium [8], aluminum [9], steel alloys [10] and tita-
nium alloys [11]. This technique can refine microstructure into a sub-
microcrystalline structure (SMC) and ultimately improve mechanical
properties such as strength and hardness [12]. Pure Nickel and low
alloying of the Nickel-based material can be used in structural com-
ponents. Further, the mechanical properties of Nickel-based material
can be improved by grain refinement process, which would further
enhance the corrosive resistance [13–15]. In addition, the properties
and characteristics of nickel and nickel-based alloy are well suitable to
manufacture the micro-electromechanical systems (MEMS) applications
[14,15]. Moreover, it is also used in chemical and electrochemical in-
dustry [13]. Some researchers have processed pure nickel and its alloys

⁎
Corresponding author.
E-mail addresses: zahidhussain@qec.edu.sa (Z. Hussain), almufadi@qec.edu.sa (F.A. Al-Mufadi), sivasankarangs1979@gmail.com, s.udayar@qu.edu.sa (S. Subbarayan),
osamaerfan@qec.edu.sa (O.M. Irfan).

https://doi.org/10.1016/j.msea.2017.12.042
Received 24 November 2017; Received in revised form 9 December 2017; Accepted 11 December 2017
Available online 13 December 2017
0921-5093/ © 2017 Elsevier B.V. All rights reserved.
Z. Hussain et al. Materials Science & Engineering A 712 (2018) 772–779

Fig. 1. Schematic illustration of MAF process showing how the

sizes change during process so that overall volume is constant.

through SPD techniques other than MAF [16–23]. However, no pub-

lished data has been found for application of MAF on Ni 200 alloy,
investigation of resultant microstructure evolution and its mechanical
properties. The main objective of the present work is to examine the
microstructural evolution and the mechanical behavior of Ni 200 alloy
subjected to MAF.

2. Materials and methods

The Ni 200 alloy in the form of a square cross-section of 50 ×

50 mm was purchased from Baoding Yuankun Machinery
Manufacturing Co. Ltd, China and it was ensured its purity around 99%.
The chemical composition of Ni 200 alloy taken for the present in-
vestigation is shown in Table 1. A set of samples with the dimensions of
15 × 15 × 30 mm were prepared using a milling machine. The surface Fig. 2. MAF process (a) MAF-Die assembly (b) illustration of MAF execution; (c) MAFed
of the samples was mechanically polished to have a smooth surface. The samples.
prepared samples were annealed in an electric induction furnace under
the nitrogen atmosphere to avoid oxidation and scales. During an- 2
ε eff One cycle = N[ {(ε11)2 + (ε22)2 + (ε33)2}]0.5
nealing, the samples were heated to 750 °C with the heating rate of 9 (1)
40 °C per hour, maintained at this temperature for 60 min (soaking
time) and then put it for furnace cooling. To carry out MAF at room 2 3 ho 2 3 30
= N ln = 3* ln = 2.40
temperature, a closed MAF die (shown in Fig. 2) was designed and 3 h 3 15
fabricated from H13 die steel material so that the samples can be where N is the number of passes carried out in the sample, which needs
multiaxially forged in three orthogonal directions (X, Y, and Z-axes). three passes to complete one cycle of MAF. ε11, ε22 and ε33 are axial
Before forging, the sample height was 30 mm and forged it to 15 mm by strains in three orthogonal directions. ‘h0’ and ‘h’ are initial and final
applying severe mechanical stress at 3 mm per minute (Forging speed heights of the samples. During MAF of each pass, the sample has to be
used here). It is to be noticed here that the width of the sample remains rotated by 90° and then put it into the die for its forging. In the present
constant and 50% normal strain was imposed on the material during investigation, zero cycle (annealed), one cycle, two cycles, three cycles
each pass. The effective strain (εeff) imposed on the material during and four cycles of forging was carried out at room temperature. The
each cycle of MAF under plane strain condition can be determined MAFed samples are shown in Fig. 2(c). The microstructure of all sam-
using the equation [11]. ples was examined after grinding, polishing and etching at room tem-
perature using Marbel's reagent. The microstructural evolutions were

Table 1
Chemical composition of material used in this research.

Element Ni Cu Mn Si C Mg S Fe Pb

Weight (%) 99.5 0.01 0.002 0.01 0.01 < 0.005 < 0.002 0.02 < 0.002

773
Z. Hussain et al.
Fig. 3. Photograph showing the mounting of Nickel 200 alloy for compression test in
MTS.
investigated using the optical microscope (OMAX A35140U) and the
transmission electron microscope (TEM, JEOL JEM 2100). Before TEM
investigations, multiaxially forged samples were cut into small thin
pieces and mechanically polished slowly until the thickness reached to
around 500 nm as thin foils. Ion milling was done on the thin foils up to
around 100 nm and then perforation was made on the thin foils. 10 ×
10 × 5 mm specimen in each multiaxially forged sample was polished,
cleaned using acetone, dried and then it was used for x-ray diffraction
test. Qualitative and quantitative investigations of microstructure after
MAF was made by X-ray diffraction (XRD, Rigaku Corporation, Japan)
analysis.
The variation of mechanical properties due to grain refinement
given by MAF was examined using simple uniaxial compression and
hardness tests. The sample size of 6 × 6 × 9 mm (1.5:1) was prepared
as per ASTM standard of E9-09 for the compression test. Three samples
were used in each condition during compression test and the average
was used for examination. The compression test was carried out using
servo-controlled universal testing machine supplied by MTS, USA
(Model No: 370.25) with a capacity of 250 kN. Fig. 3 shows the
mounting of a sample for compression test by MTS machine. During
compression test, force-displacement data of each sample was extracted
from the machine for further investigation. The mechanical properties
in terms of compressive yield strength and compressive ultimate
strength were calculated using given set height reduction of 40% in all
the samples. Vickers hardness tests were carried out using “ZWICK
universal harness testing” machine (Zwick/ZHU 250) at room tem-
perature. The hardness test was conducted at ten different places along
three orthogonal directions and the average was used for investigation.
Before carrying the hardness test, all samples were mechanically
ground with abrasive papers of progressing grit sizes to minimize the
effects of possible surface cracks developed at high strains as reported
by Kumar [24].
3. Results and discussion
3.1. X-ray diffraction analysis
The X-ray diffraction analysis on as received and MAFed samples
was examined and shown in Fig. 4. The observed values of peak in-
tensity and full-width half maximum from XRD results would help to
examine the grain refinement mechanism occur in the metals/alloys
[25]. The decreasing of peak intensity would indicate more in structural
defects due to increase in dislocation density and twins. It is clearly
observed that the peak intensity at (1 1 1) plane was started to decrease
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Materials Science & Engineering A 712 (2018) 772–779
as a function of the number of cycles of MAF. The peak intensity at (1 1
1) plane of as-received nickel sample was 10,000 cps whereas the in-
tensity of one cycle of MAFed sample was 6000 cps which were de-
creased by 1.7 times when compared to zero cycle Ni 200 alloy. In
addition, the observed peak intensity was around 5000 cps, 4300 cps
and 4150 cps for second, third and fourth cycles of MAFed samples
respectively. Moreover, the peak broadening and slight shifting of peak
towards lower angle were also noticed with increasing the number
MAF. The right side of Fig. 4 shows the magnified view of the most
diffraction peak at (1 1 1) plane for zero and three cycles of multiaxial
forged samples. The three cycle multiaxially forged sample was ex-
hibited the peak shifting towards lower angle when compared to zero
cycle sample. This was attributed to grain refinement occurred in the
structure. It can be noted here that the slight increase of peak intensity
was observed after four cycles of MAF. This was expected because of
dynamic equilibrium between the formation and annihilation of grains
was attained when imposed to high strains [26]. Further, based on full-
width half maximum and diffraction angles, the crystallite size and
lattice strain were determined using Williams-Hall method [27] for
MAFed samples (Table 2). In addition, the dislocation density of each
sample was calculated as below [27] and the same is reported in
Table 2.
16.1 ε 2
ρ =
b2 (2)
where ‘b’ is the burger vector (0.249 for Ni), ‘ε’ is the lattice strain. The
structural analysis in terms of grain size, lattice strain and dislocation
density of multiaxially forged samples from XRD result is illustrated in
Table 2. It was clear that the grain size started to decreases considerably
with the function of the number of cycles of forging up to three cycles.
However, the lattice strain was started to increase with the function of
the number of cycles of forging. These results were expected to struc-
tural modification occurred in the sample which was given by MAF
process. It is to be noted here that the slight increase in grain size and
lattice strain for four cycles of MAF sample was observed which was
attributed to dynamic recrystallization and dislocation annihilation
[28]. The same phenomenon was observed in the dislocation density.
3.2. Microstructural examination
It is well known that the grain morphology orientation can be ex-
amined clearly through an optical microscope. However, the size of
grains cannot be determined exactly using the optical microscope [29].
To find the grain size of any material exactly, it needs TEM investiga-
tion. Therefore, in the present work, the grain morphology reduction
was observed using an optical microscope and to confirm the MAFed
samples under Nano level, TEM investigation was also carried out and
exact grain size was determined. Fig. 5(a)–(e) shows the optical mi-
crostructure of zero, one, two, three and four cycles of MAFed samples
respectively. The observed grain morphology through the optical mi-
croscope of Fig. 5(a)–(e) was clearly shown that the reduction of grain
size occurred drastically as a function of MAF cycles. These results
confirmed that grain refinement occurred in the structure during MAF.
This would help to enhance the mechanical properties of nickel and
nickel alloys.
Fig. 6(a)–(f) show the bright field transmission electron microscope
(TEM) images for zero, one, two, three and four cycles MAFed samples.
The average crystallite size was 805 ± 22 nm, 475 ± 15 nm,
320 ± 13 nm, 220 ± 16 nm, and 275 ± 11 nm for zero, one, two, three
and four cycles of MAFed samples respectively (Table 2). The average
grain size was calculated based on several bright field images and the
average was taken for investigation. In each sample around 400 grains
were counted. These results were demonstrated explicitly that the grain
size after MAF was in sub Nano level. To confirm further, Selective Area
Diffraction (SAD) pattern was taken for the third cycle of MAFed
sample which is shown in Fig. 6(e). The formation of continuous ring
Z. Hussain et al. Materials Science & Engineering A 712 (2018) 772–779

Fig. 4. X-ray diffraction patterns of Nickel 200 alloy with dif-

ferent number of cycles of MAF.

Table 2 process follows an admissible trend. This can be explained by disloca-

Structural analysis of Ni 200 alloy during MAF at different cycles. tion theory equation known as Orowan equation [30].
S. No. Sample By X-ray analysis By TEM γ̇ = ρm bv (3)
condition analysis
Grain size Lattice Dislocation Grain size where γ̇ is the rate of shear strain, ρm is the density of mobile disloca-
(t), nm strain (ε), density (ρ), (t), nm tions, v is the average glide speed of dislocation and b is the magnitude
% m−2
of Berger's vector. Eq. (2) suggests that rate of grain size reduction
1 0 cycle of – – – 805 ± 22 should be constant at a reasonably slow rate of applied shear strain.
ρ
MAF However, the rate of mobile dislocation density (∆mt ) is reduced by other
2 1 cycle of 452 ± 14 0.220 1.256 × 1015 475 ± 15 dislocation processes such as the formation of dislocations of dipoles,
MAF
dislocation locks, and dislocation annihilation. Roters et al. [28] have
3 2 cycle of 305 ± 16 0.260 1.755 × 1015 320 ± 13
MAF
developed a relationship of rate of the reduction of mobile dislocations
4 3 cycle of 212 ± 15 0.310 2.495 × 10 15
220 ± 16 and each of three processes. They proved that rate of dislocation density
MAF reduction is proportional to mobile dislocation. As strain hardening
5 4 cycle of 255 ± 12 0.290 2.183 × 1015 275 ± 11 results into increase in mobile dislocation density, so the rate of re-
MAF
duction also increases proportionally. Therefore, the trend of reduction
in the rate of grain refinement is understandable.
pattern was observed in SAD which indicated that the grain refinement
was under Nano level. Further, more dislocations and twinning were 3.3. Compression stress-strain analysis
observed in three cycles of the forged sample (Fig. 6(d)) when com-
pared to one cycle of forging (Fig. 6(b)). This was attributed to im- The observed mechanical properties with deviation in the form of
posing of more strain and severe shear in the material. However, there error bars are listed in Table 3. The stress-strain curves obtained from
was no dislocation line and or twin observed in zero cycle of MAF compression tests are shown in Fig. 8 for different cycles of forging. The
sample (Fig. 6(a)) due to annealing. In addition, less number of dis- results indicate a significant increase in yield stress for one cycle fol-
location lines and disappearance of twins were observed in four cycle of lowed by a gradual increase for subsequent passes. It can be concluded
MAF sample (Fig. 6(f)) when compared to three cycle of MAF sample from Fig. 8 that nanocrystalline Ni 200 alloy (Fig. 6(a)–(f)) exhibit
(Fig. 6(d)) due to dynamic recovery and dislocation annihilation [28]. superior strength. This can be in part due to high resistance to crack
The measured grain size using XRD was in good agreement with TEM progression by severe plastic deformation [31] and low work hardening
results (Table 2). rate (low value of n in Hoffman's relation) [32]. Therefore, further
For clear understanding, Fig. 7(a)–(c) show the schematic diagram deformation requires high applied stress resulting in higher strength.
representing the arrangement of grains, formation of dislocation lines, The decreased strain hardening due to SPD is probably due to dis-
formation of twins and disappearing of dislocations and twins. In Fig. 7, location tangling which is responsible for faster dislocation spreading
the continuous line indicates the grain boundaries (GBs), the dotted line kinetics [24]. Fig. 9 shows the yield strength and the ultimate strength
indicates the dislocations and the intersection of the dotted line in- values with error bar as a function of applied cycles of forging. Increase
dicates the twins. Fig. 7(a) show the schematic of the arrangement of Ni in strength results from microstructure refinement as evident from Hall-
grain under zero cycle of forging in which there was no dislocation lines Patch relation. The increase in strength was high during the first cycle
and twins. However, the formation of more dislocation lines and twins of forging and then relatively small increase in strength was observed
after three cycles of forging as schematic is shown in Fig. 7(b). Simi- for second and third cycles followed by rather decrease in strength for
larly, the disappearing of twins and the slight increase of grain size due the fourth cycle. This was attributed to grain refinement in the structure
to dynamic recovery and flow softening as schematic is also shown in which was imposed by the process. In general, during SPD by MAF,
Fig. 7(c). dynamic recovery and annihilation would dominate after a certain
Now, it is clear from Figs. 5–7 that the SPD technique of MAF was number of cycles of forging which decrease the rate of increment in the
influenced more to refine the grain size of Ni 200 alloy. It is interesting strength. The strength would reach maximum level when a number of
to note that the grain size was severely reduced to 475 nm after the first dislocations would dominate more in the structure [26]. However, the
cycle and the rate of refinement for subsequent cycles was significantly strength would start to decrease when the dynamic recovery dominates.
reduced. The grain size was reduced to the lowest level of 220 nm after Therefore, after the 4th cycle of MAF, an unusual trend has been ob-
3rd cycle of MAF. The rate of reduction in grain size during MAF served when an increase in cumulative strain causes strength to de-
crease rather increase. The same trend has also been observed by the

775
Z. Hussain et al.
Fig. 5. Optical microstructures of Nickel 200 alloy during MAF (a) zero cycle (b) one cycle (c) two cycles (d) three cycles (e) four cycles.
researcher for other metals during SPD [33–37]. Although this pattern
of strength reduction as the result of further processing needs to be
further explored. Some researchers have attempted to explain this
phenomenon. One of the mechanisms found in the literature is micro-
cracks formation on the surface [24]. However, with the use of proper
lubricant, micro-cracks can be avoided. Another mechanism is “flow
softening” [37] during the final stages that cause the reduction of
strength. When cumulative strain further increases, the strain hard-
ening ability tends to restore due to dislocation annihilation and this
may result in strength reduction as explained by Kumar [38].
3.4. Hardness examination
Fig. 10 shows the results of Vickers hardness tests. A significant
increase in hardness has been observed for the first cycle (Cumulative
strain = 2.40) and then there is a gradual increase in hardness for
second and third cycles of MAF followed by a slight decrease in the
776
Materials Science & Engineering A 712 (2018) 772–779
fourth cycle. The increase in hardness is due to microstructure refine-
ment and strength boosting as explained earlier. The decrease in
hardness at high strains is due to “flow softening” mechanism as it has
been reported by Kumar [35]. Another parameter called inhomogeneity
factor (IF) was calculated that gives an idea about the variation of
hardness within the sample. IF is defined as [11].
i = n (Hi − H)2
∑i = 1 n−1
I. F. = x100
H (4)
where n is the number of measurements taken along the height of each
sample, Hi is the ith measurement and H is average hardness value. Ten
number of measurements were taken along the three orthogonal di-
rections (X, Y and Z axes) to assess the IF. It is well known that lesser
value of IF indicates the material would have more homogeneity con-
sequently it would exhibit improved properties. Fig. 10 shows the re-
sults of IF of Ni 200 alloy after MAF. It can be observed that IF tends to
Z. Hussain et al.
Fig. 6. TEM bright field images of Ni 200 alloy: (a) before MAF; (b) after one cycle of MAF; (c) after two cycle of MAF; (d) after three cycle of MAF; (e) SAD pattern of (d); (f) after four
cycle of MAF.
decrease as the number of cycles of MAF increases. This means that
strain homogeneity was improved and attained after MAF process. In
general, it is expected that the as-received metals/alloys might have
more inhomogeneity due to several processes carried out during its
manufacturing in the Industries (casting, extrusion with different
stages, rolling, cutting, machining etc….). Therefore, the as-received
metals/alloys might have more non-uniform strain homogeneity, re-
sidual stresses, and other defects which resulted in more hardness
variation. However, it can be decreased slightly by annealing process
before plastic deformation applied. The presence of more in-
homogeneity factor (IF) in as-received Ti-6Al-4V alloy and annealed
was also observed, investigated by Behzad et al. [11] before multi-axial
forging and the value of IF had started to decrease with subsequent
MAF cycles. The similar result of IF was observed in the present work.
4. Conclusions
In this research Nickel 200 alloy was multiaxially forged to produce
nanostructured material. The average grain size after three cycles of
forging was 220 nm. The outcomes can be summarized as follows:
● There was severe grain size reduction during the first cycle of MAF
and then the rate of grain refinement was reduced. The trend was
explained using dislocation theory. The grain refinement was also
validated by X-ray diffraction analysis.
● A great increase in yield strength and ultimate strength was
777
Materials Science & Engineering A 712 (2018) 772–779
observed. This can be interpreted with grain size reduction.
● An unusual drop in yield strength and ultimate strength was seen
after application of the fourth cycle of MAF. This was explained by
flow softening mechanism. Annihilation of dislocations occurs when
further strain is imposed thereby causing dynamic recovery and flow
softening of materials to arise.
● The results of hardness measurement show that there was a severe
increase in hardness after the first cycle of MAF and then the rate of
increase was significantly reduced. Also, there was a slight decline
in hardness after the fourth cycle of forging. The trend of variations
in hardness can be correlated with that of variations in micro-
structure refinement.
● Inhomogeneity factor (IF) calculated on the basis of hardness was
observed to decrease with the cycles of MAF. The rate of reduction
in IF was decreased with the applied cycles of MAF. A slight rise in
IF was observed after fourth cycles of MAF.
Acknowledgments
The teamwork of this research wishes to thank Qassim University
for all funding and support required to carry out this research.
Author contributions
Zahid Hussain, Fahad Al-Mufadi, Osama Irfan and Sivasankaran
Subbarayan put the idea of this work, conceived and designed the
Z. Hussain et al. Materials Science & Engineering A 712 (2018) 772–779

Fig. 7. Schematic of microstructure of Ni 200 alloy under MAF (a) 0 cycle of MAF; (b) 3 cycle of MAF; (c) 4 cycle of MAF.

Table 3
Mechanical properties of Ni 200 alloy during MAF at different cycles.

S. No. Sample condition Compressive yield strength (σy) at 0.2% Ultimate compressive strength Vicker's hardness Inhomogeneity factor (IF), %
strain, MPa (σu), MPa (HV30)

1 0 cycle of MAF 345 ± 12 781 ± 13 121.2 ± 17 63.9

2 1 cycle of MAF 615 ± 15 1033 ± 9 260.6 ± 14 48.7
3 2 cycle of MAF 720 ± 8 1100 ± 14 305.9 ± 16 35.8
4 3 cycle of MAF 805 ± 10 1198 ± 12 330.7 ± 13 21.7
5 4 cycle of MAF 765 ± 7 1157 ± 11 315.2 ± 15 29.3

Fig. 8. Compressive engineering stress and strain plots for Ni 200 alloy after MAF with
different cycles of forging. Fig. 9. Compressive properties of Ni 200 alloy during MAF at different cycles.

778
Z. Hussain et al.
Fig. 10. Vicker's hardness and inhomogeneity factor of Ni 200 alloy after MAF with
different number of cycles.
experiments; Zahid Hussain and Osama Irfan performed the experi-
ments; Fahad Al-Mufadi and Sivasankaran Subbarayanan analyzed the
data and interpreted the results; Zahid Hussain, Osama Irfan and
Sivasankaran Subbarayan wrote the paper and Fahad Al-Mufadi re-
viewed it.
Conflicts of interest
The authors declare no conflict of interest.
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