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Carbide and nitride precipitation during laser cladding of Inconel 718 alloy
coatings

Article  in  Optics & Laser Technology · January 2013

DOI: 10.1016/j.optlastec.2013.03.023

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 Optics & Laser Technology 52 (2013) 30–36

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Optics & Laser Technology

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

Carbide and nitride precipitation during laser cladding of Inconel 718

alloy coatings
Yaocheng Zhang a, Zhuguo Li a,n, Pulin Nie a, Yixiong Wu a,b
a
Shanghai Key Laboratory of Materials Laser Processing and Modification, School of Materials Science and Engineering, Shanghai Jiao Tong University,
Shanghai 200240, China
b
State Key Laboratory of Metal Matrix Composites, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China

art ic l e i nf o a b s t r a c t

Article history: The microstructure of the laser clad Inconel 718 alloy coating was observed by scanning electron
Received 11 January 2013 microscope (SEM). The chemical composition of precipitation phases was investigated by energy
Received in revised form dispersive spectrometer (EDS) and solid phase microextraction (SPME). The crystal structure and lattice
13 March 2013
constants of precipitation are determined by transmission electron microscope (TEM). Vickers hardness
Accepted 29 March 2013
of the coatings and the nanohardness of the interstitial phases were measured. The insular carbide (MC)
Available online 3 May 2013
and the tetragonal nitride (MN) with face-centered cubic (FCC) structure are rich in Ti and Nb but
Keywords: depleted in Ni, Fe and Cr due to the interdiffusion and redistribution of alloying elements between MC
Inconel 718 and MN and supersaturated matrix. MC and MN were precipitated in the forms of (Nb0.12Ti0.88)C1.5 and
Laser clad
Precipitation (Nb0.88Ti0.12)N1.5, and the Gibbs free energies of formation can be expressed as ΔG0½ðNb0:12 Ti0:88 ÞC1:5  ¼
−122:654–3:1332 TðkJ=molÞ and ΔG0½ðNb0:88 Ti0:12 ÞN1:5  ¼ −157:814–3:0251 TðkJ=molÞ. The nanohardness and
Young's modulus of the MC and MN were much higher than the matrix, and the plastic deformation
energy of interstitial phases was lower than the matrix. The precipitation of MC and MN is beneficial to
the mechanical properties of coating.
Crown Copyright & 2013 Published by Elsevier Ltd. All rights reserved.

1. Introduction composition, precipitation forms and formation of Gibbs free

IN718 is a nickel-based superalloy widely used in high-
temperature applications including turbine engines and power
generation because of its excellent mechanical properties (yield
strength up to 650–700 1C, impact strength and fracture toughness
down to −40 1C) and corrosion resistance. The precipitation phases
in the laser clad IN718 alloy coating include Laves, δ and MC.
However, a small amount of MN [1,2] is found in the clad IN718
coating and weld. The brittle phase MC and MN [3,4] are formed
during solidification of Ni-based superalloy to strengthen grain
boundaries and improve the high-temperature mechanical proper-
ties. The previous literatures [5–10] have found that the MC was
rich in Ti and Nb, and revealed that the MC was a eutectic product
of L-(γ+NbC) at about 1245 1C. Hajmrle et al [6] had identified the
chemical composition of a MN-type phase precipitated at about
1265 1C in heat-treated IN718 as 61Nb–18Ti–17Fe–3Ni–1Cr (wt%).
The investigation on precipitation forms and the mechanical
properties of MC and MN in the laser clad IN718 alloy coating is
seldom reported. This paper not only investigates the chemical
n
Corresponding author. Tel.: +86 21 54748940/8018; fax: +86 21 34203024.
E-mail address: lizg@sjtu.edu.cn (Z. Li).
energies of the MC and MN, and also measures the hardness and
deformation energy of the MC and MN.
2. Experimental
The coatings were prepared with a 3.5 kW high power diode
laser (Rofin DL-035Q) cladding system. The substrate used for the
laser cladding is 6 mm thick IN718 alloy plate. The dimension of
IN718 alloy powder for laser cladding is about 150 μm. Pure argon
was used to prevent the molten pool from oxidation and contam-
ination, and deliver the alloying powder to the molten pool. The
clad coating was fabricated with different scanning speeds and the
processing parameters were listed in Table 1. The energy distribu-
tion of the slow axis and fast axis is Gaussian distribution and top-
hat distribution, respectively. The laser cladding processes along
the fast axis. The energy density for the fabrication is about 182 W/
mm2. The chemical composition of the clad coating was 19.20 Cr,
18.1 Fe, 4.92 Nb, 0.54 Al, 0.97 Ti, 3.19 Mo, 0.20 Si, 0.04 Mn, 0.09 C,
0.11 N, and balance Ni in weight percent.
The microstructure of the coatings was observed with JSM-
7600F field emission SEM equipped with EDS after etching with a
Kalling's reagent (20 ml HCl, 20 ml C2H5OH and 1 g CuCl2). The

0030-3992/$ - see front matter Crown Copyright & 2013 Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.optlastec.2013.03.023
 Y. Zhang et al. / Optics & Laser Technology 52 (2013) 30–36
Table 1
Processing parameters for laser cladding.
Laser power (W) 1200
Scanning speed (mm/s) 8–50
Powder feed rate (g/min) 18
Shield gas flow (l/min) 15
Laterally shield gas flow (l/min) 8
chemical composition of precipitation phases was investigated by
EDS and SPME. The cladded coating was pelt off the substrate and
electrolyzed for SPME in the electrolyte solution of 7.5% KCl+0.5%
citric acid diluted with distilled water at the temperature about
−20 1C. The concentration of each element of the extractant is
determined by inductively coupled plasma (ICP). The crystal
structure and lattice constants of MC and MN were characterized
by JSM-2100F field emission TEM. Vickers hardness of the coatings
was measured on HVS-10 Vickers hardness tester at a load of 4.9 N
for 15 s. The nanohardness and Young's modulus of the precipita-
tion phases were investigated by nanoindentation with CMS 06-
0140 nanoindentor. In the nanoindentation test, 3 locations of
each phase were chosen. For each location, fifteen indentations
were conducted in a 3  5 array with constant intervals. The
applied load increased linearly to the peak load 5 mN in 30 s
during the loading stage, and then the load was released in 30 s.
The nanohardness and Young's modulus of the materials can be
derived through analysis of the loading–displacement data during
the loading–unloading nanoindentation cycle using the method of
Oliver and Pharr [11,12]. The nanohardness is given by Eq. (1) as:
F max
H¼
Ac
where, Fmax is the maximum applied load and Ac is the area
function of contact depth hc.
Similarly, using the method of Oliver and Pharr, the calculation
of elastic modulus of the material Es is given by following Eqs. as:
rffiffiffiffiffiffiffiffiffiffiffiffiffi
1 π dF
Er ¼ ð2Þ
2 Ac ðhc Þ dh
1 1−ν2s 1−ν2i
¼ þ
Er Es Ei
where, Es and νs are Young's modulus and Poisson's ratio of the
specimen material, and Ei and νi are Young's modulus and
Poisson's ratio of the indenter material, respectively. Er is the
effective Young's modulus of the contact pair indenter–specimen,
Er is obtained by nanoindentation. For the diamond indenter, Ei
and νi are taken as 1141 GPa and 0.07, respectively.
3. Results and discussion
3.1. Microstructure
Fig. 1 depicts a typical cross section of single laser track obtained
with the scanning speed of 8 mm/s. Good metallurgical bonding
exists between the laser clad IN718 coating and the substrate. A
large dilution region is formed under the high energy density, while
the chemical composition of the coating is basically steady due to
the similar chemical composition of the powder and the substrate.
Fig. 2 shows the microstructure of the laser clad IN718 coatings
fabricated with different scanning speeds. As shown in Fig. 2, the
tetragonal and the insular precipitation phases appear in the coat-
ings. The white dendritic Laves phase is refined and its concentra-
tion is decreased, and the concentration of the tetragonal and the
insular phases increase slightly with increasing the scanning speed.
31
Fig. 1. Cross section of the cladded coating with scanning speed of 8 mm/s.
The white dendritic precipitation is Laves, the insular phase is MC-
type carbide and the tetragonal phase is MN-type nitride [13,14].
The morphology of MC and MN varies from dendritic to petaline,
and then tetragonal with increasing solidification rate. The grain
growth rate is dependent on the difference between the atom
deposition rate of solution atom depositing on the solid–liquid
interface and the withdrawal rate of atoms escaping from the
growth steps to the liquid alloy. The grain growth is dominated
ð1Þ by the latent heat of fusion of the alloy, and the higher melting
entropy is inclined to form finer and more homogeneous micro-
structure. Nevertheless, the supercooling of the molten pool
increases with increasing the scanning speed and the cooling rate,
and the large supercooling promotes the atom interface coarsening
and forms the insular and/or tetragonal phases.
3.2. Precipitation form of phase
The EDS analysis was carried out to investigate the chemical
ð3Þ composition of the MC and MN, as shown in Fig. 3 and Table 2. The
results reveal that the tetragonal phase is rich in N, Ti and Nb,
while the insular phase is rich in C, Ti and Nb. The precipitation
phases contain large amounts of strong interstitial phase forma-
tion alloying elements (Nb and Ti), but without weak interstitial
phase formation alloying elements (Fe and Ni) [15,16]. The con-
centrations of Ti and Nb in insular phase are (6.2–9) times and
(16.7–18.4) times higher than the nominal concentration, respec-
tively. The concentrations of Ti and Nb in tetragonal phase are (72–
80) times and (2.8–4.5) times higher than the nominal concentra-
tion, respectively.
The forms of MC and MN are defined as (NbαTi(1−α))Cβ and
(NbxTi(1−x))Ny [17], α and x are the Nb atomic numbers, β and y are
the non-metal atomic numbers in the sublattices of (NbTi)C and
(NbTi)N, respectively. The calculational results according to Avoga-
dro's principle show that α≈0.12, β≈1.5, x≈0.88, and y≈1.5, respec-
tively. However, the C concentration cannot be determined
accurately by EDS. SPME for concentration of alloying elements in
MC and MN is carried out. The coating mass for SPME is 12.31 g, and
reclaimed mass of each element of MC and MN in the coating is
presented in Table 3. The determination results of SPME agree well
with the above calculation results when measurement error about
8% was taken into account. The measurement error is taken on the
basis of the mass difference of each element between clad coating
and the electrolyte solution. It is indicated that the formation of MC
and MN is (Nb0.12Ti0.88)C1.5 and (Nb0.88Ti0.12)N1.5, respectively.
32 Y. Zhang et al. / Optics & Laser Technology 52 (2013) 30–36

Fig. 2. Microstructure of the clad coatings with different scanning speeds: (a) 8 mm/s, (b) 17 mm/s, (c) 33 mm/s and (d) 50 mm/s.

Fig. 3. EDS analysis on the MC and MN in the clad coating with different scanning speed of 50 mm/s: (a) SEM interesting area, (b) energy spectrum of tetragonal phase, and
(c) energy spectrum of insular phase.

The TEM results show that the MC and MN are both FCC
structure, as shown in Fig. 4. The lattice constants of MC and MN
are aMC ¼0.4315 nm and aMN ¼0.4407 nm, respectively. The lattice
constants of (Nb0.12Ti0.88)C1.5 and (Nb0.88Ti0.12)N1.5 are approxi-
mately equal to that of TiC and NbN, and the lattice constants are
changed owing to Nb and Ti replacing the Ti atomic position in TiC
and Nb atomic position in NbN, respectively. The concentrations of
C and N in the interstitial phases are higher than TiC and NbN,
indicating that the interstitial phases (Nb0.12Ti0.88)C1.5 and
(Nb0.88Ti0.12)N1.5 in the coating are compound phases due to the
 Y. Zhang et al. / Optics & Laser Technology 52 (2013) 30–36 33

rapid cooling (105–106 K/s) of the laser cladding with fast scanning Fig. 5(b). The nanohardness and Young's modulus of MC and MN
speed. The MC and MN have a coherent relationship with FCC are both higher than the matrix.
austenite, and can dissolve in the high-temperature austenite During the nanoindentation deformation, the total absorbed
region or precipitate in the low-temperature austenite region of deformation energy (W0) of the material can be represented by the
the phase diagram. area between the loading curve and the X-axis [18]. It can be
The concentration of (Nb, Ti) in the MC and MN is the primary expressed as
factor on its mechanical properties and the effect of MC and MN on
Z hmax
the improvement of mechanical properties of the coating. There-
W0 ¼ F load dh ð4Þ
fore, the nanohardness of MC and MN as well as the Vickers 0
hardness of the coatings are investigated.
where, Fload is the load during loading stage of nanoindentation
(nN), h is the penetration depth (nm).
3.3. Hardness test

Fig. 5(a) depicts the loading–unloading curves of nanoindenta-

tion of MC and MN with the maximum normal load of 5 mN. The
penetration depth of MN is much deeper than MC due to the
different nanohardness. The average nanohardness is 2017.4 HV0.5
of MC and 1375.2 HV0.5 of MN, the average Young's modulus is
371.8 GPa of MC and 328.8 GPa of MN, respectively, as shown in

Table 2
EDS results of MC and MN of clad coating with different scanning speeds.

Speed MN (NbxTi(1−x))Ny MC (NbαTi(1−α))Cβ

(mm/s)
N Ti Nb x y C Ti Nb α β
(wt%) (wt%) (wt%) (wt%) (wt%) (wt%)

17 27.82 57.19 14.99 0.881 1.464 18.50 5.84 75.66 0.130 1.410
28.90 55.25 12.35 0.897 1.603 20.91 5.20 73.89 0.120 1.651
25.32 59.44 15.23 0.883 1.286 18.40 6.37 75.23 0.141 1.393

33 27.38 56.50 16.12 0.872 1.444 20.18 4.87 74.96 0.112 1.585
31.87 54.06 14.08 0.882 1.776 19.12 6.70 74.18 0.149 1.454
26.97 57.15 15.88 0.875 1.411 20.51 5.22 74.27 0.120 1.612

50 30.15 57.89 11.96 0.904 1.608 20.79 4.86 74.34 0.113 1.646
25.22 59.50 15.28 0.883 1.279 12.54 5.97 81.48 0.125 1.394
24.79 55.64 19.57 0.847 1.289 18.84 4.64 76.52 0.105 1.461

Table 3
Determination results by solid phase microextraction (μg).

Element C N Ti Nb

Mass 6.4 19.1 82.2 38.4 Fig. 5. Loading and unloading curves of MC and MN (a) and the nanohardness and
Young's modulus of MC and MN (b).

Fig. 4. TEM bright field images of (a) MC and (b) MN in the clad coating with scanning speed of 50 mm/s.
34 Y. Zhang et al. / Optics & Laser Technology 52 (2013) 30–36

Similarly, the elastic strain energy (W1) can be given by the area alloy because the strengthening phase precipitates during the
between unloading curve and X-axis. W1 is the recovered energy standard heat treatment. Our previous TEM analysis [10] on the
during the unloading. It can be expressed as: single track of laser cladded coating shows that there is no strength-
Z hmax ening phase precipitation without heat treatment. The variation in
W1 ¼ F unload dh ð5Þ hardness was influenced by the Laves morphology and the volume
hp fraction of MC and MN. With increasing scanning speed, Laves is
where, Funload is the load during unloading stage of nano- refined and its concentration is decreased, the concentration and the
indentation (nN). size of MC and MN are increased. The change of Laves morphology
The plastic deformation energy W2 can be expressed as: and concentration leads to decrease in hardness, while the hardness
Z hmax Z hmax of the clad coating increases with increasing scanning speed. It is
W 2 ¼ W 0 −W 1 ¼ F load dh− F unload dh ð6Þ indicated that the eutectic products MC and MN form as the hard
0 hp particles to hinder the grain boundary sliding and dislocation motion,
According to Eqs.(4)–(6), the results of W0, W1 and W2 of MC, and is beneficial for increasing Vickers hardness. MC and MN cannot
MN and matrix are carried out and listed in Table 4. Defining η as be dissolved in the standard heat treatment, indicating that effect
efficiency of deformation energy provided by the material during of MC and MN on the mechanical properties sustains after heat
the loading and unloading curves, η reflects the recovery ability of treatment. The clad coating obtained at higher scanning speed
materials during the deformation, and the materials with higher η contains more MC and MN with larger size, and exhibit higher
can absorb more impact energy. hardness.

η ¼ W 1 =W 0
The average values of the total deformation energy (W0), elastic
deformation energy (W1), and η of interstitial phases are presented
in Table 4. The value of hp is the unrecoverable penetration depth
during the unloading step of the nanoindentation. η is the
parameter to characterize the deformation resistance of material.
It can be concluded that the lower value of hp, the higher value of η
and hardness.
The hardness of MC and MN is higher than the matrix, and the
hard inclusions MC and MN can improve the deformation resis-
tance. Moreover, the plastic deformation energy of MC and MN is
much lower than matrix. Therefore, the mechanical properties of
the coating can be enhanced by appropriate amounts of the MC
and MN.
The Vickers hardness of the clad coatings is investigated (Fig. 6),
and the result shows that Vickers hardness of the coatings increases
from 256 HV0.5 to 287.6 HV0.5 as the scanning speed increases from
8 mm/s to 50 mm/s. The IN718 alloy is a precipitation strengthening
Table 4
Average values of the total deformation energy (W0), elastic deformation energy
(W1), plastic deformation energy (W2) and η of MC and MN and matrix.
ð7Þ
3.4. Gibbs free energies of formation MC and MN
In MC and MN, the metal and non-metal atoms form a
complete close-packed crystal structure while other atoms can
replace the interstitial sites of the sublattices. The simplified
sublattice can be represented by (M1, M2)x(N1, N2)y, x and y are
the atomic numbers of the metal atom and non-metal atom in the
sublattice, respectively. The Gibbs free energies of formation of the
phases can be evaluated by the solution model of Hillert and
Staffansson [19,20]. In this model, M1 and M2 represent the metal
elements on one sublattice and N1 and N2 are the non-metal
elements. The Gibbs free energy is assessed by using thermody-
namic models for the Gibbs energy of individual phases, and is
expressed as
ΔG0½ðM1 ;M2 Þx ðN1 ;N2 Þy  ¼ Z M1 Z N1 Δf G0½M1 N1 
þZ M1 Z N2 Δf G0½M1 N2  þ Z M2 Z N1 Δf G0½M2 N1 
þZ M2 Z N2 Δf G0½M2 N2  −TSideal þ GEm ð8Þ
Z M1 ¼ nM1 =ðnM1 þ nM2 Þ ð9  1Þ

W0 (nJ) W1 (nJ) W2 (nJ) η Z M2 ¼ nM2 =ðnM1 þ nM2 Þ ð9  2Þ

MC 191.09 90.78 100.30 0.475 Z N1 ¼ nN1 =ðnN1 þ nN2 Þ ð9  3Þ

MN 410.38 58.75 351.63 0.141
Matrix 731.55 60.59 670.96 0.083
Z N2 ¼ nN2 =ðnN1 þ nN2 Þ ð9  4Þ

where, Δf G0½Mi Nj  is the standard Gibbs energy of formation of the

reference phase MiNj; nM1 , nM2 , nN1 and nN2 are the mole fractions
for the metal and non-metal atoms on its sublattice separately;
Sideal is the entropy of ideal mixing and GEm is the excess molar
Gibbs energy.

−Sideal =R ¼ nM1 lnZ M1 þ nM2 lnZ M2 þ nN1 lnZ N1 þ nN2 lnZ N2 ð10Þ

GEm ¼ Z M1 Z M2 Z N1 LN N2 M1
M1 M2 þ Z M1 Z M2 Z N2 LM1 M2 þ Z N1 Z N2 Z M1 LN1 N2
1

þZ N1 Z N2 Z M2 LM 2
N1 N2 ð11Þ

where, LN N2 M1 M2
M1 M2 , LM1 M2 , LN1 N2 and LN1 N2 are interaction parameters
1

among atoms on the same sublattice and different sublattices,

Fig. 6. Vickers hardness and dendritic space of the clad coatings with different
scanning speeds.
respectively. The parameters L are zero for an ideal solid solution.
The L values of precipitation phases (TiN, NbN, TiC and NbC) are
approximately equal to zone.
Simplified the size of sublattices as x+y¼1 for convenient
calculation at the basis of atomic number of each element and
its atomic ratio in the sublattice, the standard Gibbs energy of the
 Y. Zhang et al. / Optics & Laser Technology 52 (2013) 30–36
Fig. 7. Comparison between the Gibbs energies of formation of MC and MN.
MC and MN is obtained from the previous works [20,21]:
Δf G0½TiC ¼ −0:0939 T−135:08 kJ=mol TiC
Δf G0½TiN ¼ −0:1027 T−286:89 kJ=mol TiN
Δf G0½NbN ¼ −0:0428 T−140:21 kJ=mol NbN
Δf G0½NbC ¼ −0:000995 T−31:5 kJ=mol NbC
The Gibbs free energies of formation of (Nb0.12Ti0.88)C1.5 and
(Nb0.88Ti0.12)N1.5 are obtained as:
ΔG0½ðNb0:12 Ti0:88 ÞC 1:5  ¼ −122:654−3:1332 TðkJ=molÞ
ΔG0½ðNb0:88 Ti0:12 ÞN1:5  ¼ −157:814−3:0251 TðkJ=molÞ
The Gibbs free energies of formation of (Nb0.12Ti0.88)C1.5 and
(Nb0.88Ti0.12)N1.5 during the temperature range of phase transition
[10] are presented in Fig. 7. It is found that Gibbs free energies of
formation of (Nb0.12Ti0.88)C1.5 and (Nb0.88Ti0.12)N1.5 are lower than
MC and MN with simple structure. The Gibbs free energies of
(Nb0.12Ti0.88)C1.5 and (Nb0.88Ti0.12)N1.5 are negative and are lower
than the sums of TiC and NbC, TiN and NbN, respectively. It is
indicated that the chemical reaction of formation of (Nb0.12Ti0.88)
C1.5 and (Nb0.88Ti0.12)N1.5 could occur with proper conditions.
During the solidification process, Nb element is segregated in
the liquid due to lower diffusion coefficient, and Ti, C and N are
rejected into the reaction due to the less distribution coefficients
than unity of other alloying elements in the early stage of the
solidification [22,23]. The concentration of these alloying elements
increases with the solidification process, then MN and MC form
simultaneously when the concentration of the alloying elements
exceeds the maximum solubility in the austenite matrix. There-
fore, the supersaturated alloying elements remain in the inter-
stitial phase and Laves phase at the termination of solidification.
Meanwhile, the alloying elements show a positive Soret coefficient
in the solidification process due to a large temperature gradient
[24]. The alloying elements interdiffuse and redistribute between
MC/MN and supersaturated Laves [25,26]. Thus, MC and MN
containing high concentration of Ti and Nb are apt to form in
the clad coating due to rapid solidification cooling rate that
facilitates the sufficient diffusion of strong interstitial phase
formation alloying elements [27,28].
35
4. Conclusions
(1) The microstructure of the clad coating is refined with increas-
ing the scanning speed of the laser cladding. The size and
amounts of MC and MN are related to the scanning speed due
to the large supercooling.
(2) The insular MC and the tetragonal MN are rich in Ti and Nb as
the results of the interdiffusion and redistribution of the
alloying elements between interstitial phases and supersatu-
rated matrix during the rapid solidification cooling process.
MC and MN are precipitated in the forms of (Nb0.12Ti0.88)C1.5
and (Nb0.88Ti0.12)N1.5.
(3) The nanohardness and Young's modulus of MC and MN are
higher than matrix, while the plastic deformation energy of
MC and MN is much lower than matrix. Vickers hardness of
the coatings is related to the precipitation of MC and MN.
(4) The Gibbs free energies of formation of (Nb 0.12 Ti 0.88 )C 1.5
and (Nb0.88 Ti 0.12)N 1.5 can be expressed as ΔG0½ðNb0:12 Ti0:88 ÞC 1:5  ¼
−122:654 −3:1332 TðkJ=molÞ and ΔG0½ðNb0:88 Ti0:12 ÞN1:5  ¼ −157:814
−3:0251 TðkJ=molÞ.
ð12  1Þ
Acknowledgments
ð12  2Þ This research was financially supported by the funding of
Ministry of Science and Technology of the People's Republic of
China (Grant no. 2009DFB50350) and the National Natural Science
ð12  3Þ
Foundation of China (Grant no. 50971091).
ð12  4Þ
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