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JOURNAL OF IRON AND STEEL RESEARCH, INfERNATIONAL. 2009,16(1),07-11

Segregation of Niobium During Electroslag Remelting Process

DONG Yan-wu", JIANG Zhou-hua", LI Zheng-bang"
O. School of Materials and Metallurgy, Northeastern University, Shenyang 110004, Liaoning, China,
2. Central Iron and Steel Research Institute, Beijing 100081, China)

Abstract, Experiment was carried out after the process parameters were calculated by the model previously estab-
lished. The relationship between interdendritic spacing and local solidification time (LST) mainly determined by
process parameters was exposed. Furthermore, the extent of segregation was studied. The results indicate that LST
and interdendritic spacing are the largest and the amount of Laves phase as a result of the niobium segregation is the
highest in the center of the ingot, whereas the opposite results are obtained at the edge of ingot. The extent of ele-
ment segregation and the amount of Laves phase can be reduced when appropriate parameters are used. Therefore,
the duration of subsequent homogenization treatments for 718 is shortened and the alloy quality is improved.
Key words; electroslag remelting; Inconel 718; segregation; local solidification time; interdendritic spacing

Inconel 718 is a Ni-Fe-based alloy strengthened dendritic spacing) is controlled by LST.

by r' and i' phases. The alloy is widely used in avi-
ation, space navigation, and shipping industries at
high temperatures up to approximately 700 'C owing
to its excellent properties, high fabricability, and
relatively low cost. It is about 35% of all superalloy
production in recent years[l]. However, Laves phase
is precipitated owing to niobium segregation during
the production of the alloy, which is a brittle phase
and influences the mechanical properties and decrea-
ses the niobium content needed by forming the r'
and i' phases. Long time homogenization treatment
is, thus, needed to eliminate or decrease the segre-
gation of niobium-'", However, it is usually difficult
to eliminate segregation in the center of large ingot.
It is known that solidification structure is deter-
mined by local solidification time (LST) during vari-
ous casting processes. Experiments were carried out
in this study on the basis of a model established pre-
viously[3] for electroslag remelting (ESR) to investi-
gate whether or not solidification structure (inter-
1 Experimental
1.1 Preparation of electrode
Scrap with proper composition was used to pro-
duce the as-cast ingot by a vacuum induction melting
furnace. Argon was injected into the melting cham-
ber to prevent metal loss with burningl'", To com-
pensate the loss, carbon, aluminum, and titanium
were added into the chamber. The ingot after cast-
ing is forged into electrode with 1. 7 m in length and
70 mm in diameter, and subsequently used for elec-
troslag remelting. Table 1 shows the composition of
the electrode.
1.2 ESR experiment
ESR is the final melting process for many spe-
cial steels and alloy steels, including Inconel 718
when duplex technique is used because of high quali-
ty of the products obtained from this route. The pa-
rameters of power supply are very important for the

Table 1 Chemical composition in mass percent of consumable electrode %

Element C Cr Mo Ti Al Nb P S
Content 0.066 17.78 2.79 1. 04 0.35 5.21 0.006 0.002

Foundation Item, Item Sponsored by Weaponry Pre-Research Fund (51412020304QT090l)

Blography,OONG Yan-wu(l978-) , Male, Doctor; E-mail.yanw~dong@163.com; Revised Date; January 19,2008
 • 8 • Journal of Iron and Steel Research, International Vol. 16

quality of the ingot. Too fast or too slow melting
rates would have a negative impact on solidification
structure-'v .
ESR is a very complex physicochemical process,
including the interactions of electromagnetic field,
velocity field, and temperature field, etc. A model
has been established on the basis of the Maxwell's
equations, turbulent Navier-Stokes equations, and
thermal transfer equations. The relationship be-
tween the interdendritic spacing and the local solidi-
fication time[6] during the ingot solidification
process, which has been regarded as a criterion for
controlling the quality of crystallization'f' , is further
defined. Table 2 shows the parameters of power
supply calculated for Inconel 718 by using an estab-
lished model.
The mold used is 130 mm in diameter and 800 mm
in height. The components of remelting slag are CaFz-
Al z0 3-MgO-TiOz containing .no, of 4%. Table 3
shows the parameters to be executed on the basis of
the parameters calculated with the model and the la-
boratory conditions. The voltage determined by the
transformer is fixed at 44 V. The difference of LST
for the similar voltage and current is produced owing
to the characteristics of ESR. At the beginning of
ESR, shallow molten pool and better cooling condi-
tion bring short LST. With the increase in the ingot
height, the cooling condition becomes weak, making
the molten pool deeper and the LST increase.
Table 2 Calculated process parameters for ESR by model
No. 2 3 4 5
99. 1
Power/kW 103.7 95.1 90. 1 83. 7

Table 3 Operating parameters for producing Inconel 718 by ESR

No. Melting length/ mm Voltage/V Current/kA LST' in the center Is d i in the center/ f-lm d IT in the center/ f-lm
1 409.4 44 2.45 90 128.4 35. 7
2 372. 7 44 2. 35 394 140.6 58. 5
3 336.0 44 2. 25 379 142.2 57. 7
4 299.3 44 2.2 416 141. 0 59.5
5 262.6 44 2.0 421 141. 2 59.8
Note: d I ' d II are the primary and secondary interdendritic spacing, respectively; * means the values calculated with the model.

2. 1.2 Macroscopic examination

2 Results and Discussion
The ingot was cut along the transversal and
2. 1 Investigation of ingot produced by ESR longitudinal directions. No defects such as voids, white
2. 1. 1 Composition and inclusions in the ingot spots, and freckles were observed in the ingot (Fig. 2).
The voltage and current were relatively stable
during remelting. The surface of ingot is rather
smooth (Fig. 1). The chemical composition at the
top and bottom of the ingot is very close, e. g. the
difference of titanium content is only o. 08% (Table 4).
However, the chromium and molybdenum contents in-
crease owing to the oxidation of titanium and niobium.
Specimens were taken from the near surface,
half radius, and center of the ingot. The specimens
were characterized by SEM equipped with EDX after
grinding and polishing. The results indicate that
both Al, 0 3 and TiN inclusions are fine and disper-
sive. Sometimes Al, 0 3 and TiO z , and TiN and NbC
coexist in a single particle of inclusion. Fig. 1 Appearance of Inconel 718 ingot produced by ESR

Table 4 Chemical composition in mass percent of Inconel 718 at the top and bottom of ingot %
Element C Cr Mo Ti Al P S Nb
Top of ingot 0.067 17.93 2. 92 0.89 0.30 0.006 0.001 5 5.00
Bottom of ingot 0.065 17.86 2. 93 0.81 0.29 0.006 O. 001 5 4.81
Issue 1 Segregation of Niobium During Electroslag Remelting Process ·9·

The columnar crystals are well orientated at an angle

of 60° - 70° to the radial direction, indicating that the
melt bath is very flat during remelting.
2. 1. 3 Characterization of precipitation in ingot
A type of phase in white particles was observed
in the as-cast ingot during the analysis. The phase is
considered as Laves phase according to its appear-
ance and position. The composition of the Laves
phase analyzed with EMP-BIO (Shimadzu) is listed
in Table 5.
Niobium content is quite high, and silicon, molyb-
denum, and titanium contents are also high CTable 5).
However, chromium content in Laves phase is lower
Fig. 2 Macrostructure of ingot in longitudinal direction in comparison to that in the base metal. It indicates

Table 5 Composition in mass percent of Laves phase %

Position Fe Ni Cr Si Nb Mo Ti
Center 15.96 45.40 11. 31 1. 27 20.48 4.03 1. 54
18.07 42. 10 13.47 1. 20 19.32 3.57 2.27
Half radius 17.45 40.36 13. 10 1. 54 21. 04 5.17 1. 33
16.95 41. 04 12.53 1. 61 20.96 5.34 1. 57
Near surface 17.77 42.20 13.49 1. 20 19.91 4.04 1. 39
16.90 39.13 13.25 1. 56 22.44 5.66 1. 07
Average 17.18 41. 71 12.86 1. 40 20.69 4.64 1. 53
Radhakrishnan et al 11.60 45.20 13.00 22.40 4.90 1. 10
Knorovsky et al 11.60 45.80 13.30 1. 40 22.30 4.60 1. 20
YNAG Ai-min 12.825 32.31 13.445 34.56 6.86 0.785

that the formation of Laves phase is closely related
to element segregation. The extent of element segre-
gation observed, especially niobium segregation, is less
significant than that reported by YANG Ai-min[7] and
very close to the achievement of Radhakrishnan et
al[S] and Knorovsky et al[9].
Specimens at the near surface, half radius, and
center were used to examine the density, quantity,
and dimensions of Laves phase. Metallographic char-
acterization was carried out and ten areas were cho-
sen on every specimen. The results are list in Table
6. It seems that the precipitation of Laves phase is
more than that reported in published works. How-
ever, it is noteworthy that the ingot used in the pub-
lished works was only I - 2 kg, which is casted by
vacuum induction furnace with a crucible of 5 kg
holding capacity[7,lO]. And that, relatively small in-
got is less prone to segregation. Fig. 3 shows that
more Laves phase is precipitated at a longer LST,
which is in accordance with the results calculated on
the basis of the model. The longest LST in the cen-
ter of the ingot results in the highest amount of
Laves phase precipitation.
Fig. 4 shows the effect of LST on interdendritic
spacing, where the solid lines are the calculated re-
sults. The relation shown is very coincidental. Fig. 5
shows the dendritic appearance. Another type of
phase precipitated in the alloy is MCC, N), which is
present either as strips, as particles, or in cellular
shape (Fig, 6). The MCC, N) phase is enriched in nio-

Table 6 Results of quantitative metallographic analysis of Laves phase

Experiment Item Center Half radius Near surface
This work Density/mm- z 663 356 103
Amount/% 2.2.7 1. 30 0.66
.Equivalent diameter/urn 5.28 5.13 5.01
YANG Ai-min Amount/% 1. 89-2. 11
 • 10 • Journal of Iron and Steel Research. International Vol. 16

2.2 • Measured value

~
- Calculated value
~ 1.8
.<::
.::>.
'"
~.... 1.4
0
l:: 1.0
='
0

~
0.6 L.L~~_~_~_~_~_~----l

100 150 200 250 300 350 400 450

Timels

Fig. 3 Relationship between Laves phase precipitation and LST

Fig. 6 SEM micrograph of MC phase in alloy
160 r - - - - - - - - - - - - - - -
Table 7 Chemical composition in mass percent of
= 120
rr»>:- ...
1
M (C. N) carbides analyzed by EDS %
~ Calculated POS Element Nb Ti C N
5 - - - Calculated SOS
.~ • Measured POS Content 65.50 16.57 10.33 7. 60
u 80 • Measured SOS 72.75 7.09 9.06 11. 10
'.;:3
.>:
'tl
e
1:
~
40 420 F=====-------------,
.s
410
o 200 400 600
Time/s
.!!! 400
POS-Primary interdendritic spacing; ~
SOS-Second interdendritic spacing 390
Fig. 4 Relationship between interdendritic spacing and LST
380

45 50 55 60 65 70
Melting rate/(kg-h")

Fig. 7 Relationship between melting rate and LST for ESR

alloy IN718 (diameter of crucible = 130 mm)

crucible in diameter, the melting rate should be con-

trolled at approximately 66 kg/h, and the lowest
LST can be obtained.

Fig. 5 Relationship between interdendritic spacing and LST
bium and titanium according to SEM-EDX analysis
(Table 7). In general, carbon is rich in interdendrit-
ic , and thus, M(C, N) phase often exists in inter-
dendritic or next to Laves phase.
Fig. 7 shows the relationship between melting
rate and LST for ESR alloy Inconel 718. Too high or
too low melting rate will increase the LST, which
affects the solidification quality. Thus, for the 130 mm
2. 2 Microsegregation of alloy
Segregation, as one of the major defects, is very
hazardous to the properties of ingots or castings.
The heterogeneity results in different structures in
matrix and in sequence deteriorate the mechanical
property, machining property, and heat cracking re-
sistance, etc.
Segregation ratio (SR )[7 J is the ratio of the
highest or lowest solute concentration of interden-
dritic to the highest or lowest solute concentration of
dendritic arm. For a positive segregation element,
Issue 1 Segregation of Niobium During Electroslag Remelting Process • 11 •

SR= (The highest solute concentration of
interdendritic) / (The lowest solute
concentration of dendritic arm)
and for a negative segregation element,
SR= (The lowest solute concentration of
interdendritic) / (The highest solute
concentration of dendritic arm)
SR approaches unity for an element, irrespective of
the condition that it is positive or negative. The
(1) lighter is the element, the more homogeneous it dis-
tributes. Table 8 shows the chemical composition of
interdendritic and dendritic arm analyzed by EMP.
The SR of every element is within the range for cast
(2) alloy K4169 (Inconel 718), except that the SR obta-

Table 8 Composition and segregation ratio in dendritic arm and interdendritic region
Element Fe Cr Nb Mo Ti Si
Dendritic arm! % 28.66 20.94 2. 38 2.34 0.65 0.22
Interdendritic region! % 23.11 17.32 8.12 2.82 1. 17 0.47
Segregation ratio 0.806 0.827 3.412 1. 205 1. 80 2. 136
YANG Ai-min[7] 0.775-0.941 0.831-0.919 2.042-3.91 1. 194-2. 2 1. 55-3. 571

ined in this study is a little lower.
3 Conclusions
Electroslag remelting experiment of Inconel 718
was carried out by using process parameters deter-
mined by the built model. Characterization indicates
that longer LST results in larger segregation tenden-
cy. As a result, more Laves phase is precipitated and
more extended homogenization treatments are nee-
ded at high temperatures. Any decrease in the amount of
Laves phase can thus reduce the duration of the homoge-
neous treatments. Therefore, the amount of Laves
phase, further the segregation of elements, can be
reduced by controlling the process parameters during
electroslag remelting.
References ,
[IJ Liu Xingbo , Kang B, Carpenter W, et al. Investigation of the
Crack Growth Behavior of Inconel 718 by High Temperature
Moire Interferometry [n.Journal of Materials Science. 2004.
39(6), 1967.
[2J Radavich John F. The Physical Metallurgy of Cast and Wrought
Alloy718 [AJ. Loria E A. eds, Superalloy 718-Metallurgy and
Applications [CJ. Warrendale, TMS. 1989. 229.
[3J DONG Yan-wu , JIANG Zhou-hua, Ll-Zheng-bang. Mathemat-
ical Model for Electroslag Remelting Process [n. Journal of
Iron and Steel Research. International. 2007. 14(5). 7.
[4J Alok Choudhury. State of the Art of Superalloy Production for
Aerospace and Other Application Using VIM!VAR Or VIM!
ESR [n ISU International. 1992, 32(5). 563.
[5J Petit P. Fesland J P, Aubert. et al. Manufacturing of Large in
706 and in 718 Forging Parts [AJ. Loria E A. ed. Superalloys
718.625.706 and Various Derivatives [CJ. Warrendale.
TMS. 1997. 153.
[6J Fleming M C. Solidification Processing [MJ. New York.
McGraw Hill Book Company. 1974.
[7J YANG Ai-rnin. Study of Structure Refinement and Optimiza-
tion of Mechanical Proprieties for Superalloy K4169 [DJ. Xi'
an, Northwestern Polytechnical University. 2002 (in Chinese).
[8J Radhakrishnan B. Thompson R G. A Phase Diagram Approach
to Study Liquation Cracking in Alloy 718 [JJ. Met Trans.
1991. 22A(4), 887.
[9J Knorovsky G A. Cieslak M J. Headley T J. et al. INCONEL
718. A Solidification Diagram [n. Met Trans. 1989. 20A
(0), 2149.
[10J XIONG Yu-hua , LIU Wei, YANG Ai-min , et al, Effects of
Ni-Al-Ti Refiner on Grain Structure and Mechanical Properties
of Cast Superalloy K4169 [n. Acta Metallurgica Sinica,
1999. 35(7), 689 (in Chinese).