Melting of Superalloy

Paradigm Shift in the Technology Development of Superalloys

 Relevance of Melting of Superalloys
Relevance of Melting of Wrought Superalloys:

 The performance of GTE components (also called the HOT GAS PATH Components) depends on
the performance characteristics in service which is guided by their primary chemical composition in
superalloys.

 Poor quality ingots cannot produce reliable components whatever be the casting or forging process
and/or the heat treatment cycle.

 Most of the superalloys are produced by VIM/VAR or VIM/ESR melting process subsequent to
which the ingots are processed further into components .

 Vacuum Induction Melting (VIM) is the primary melting process of superalloys,

 Vacuum Arc Melting (VAR) or Electro-Slag Refining (ESR) is the secondary melting or refining
process.

 Superalloy ingots must be melted and cast with due regard for the volatility and reactivity of the
elements present. Vacuum melting processes are a necessity for many

 Ni- and Fe-Ni-based alloys  presence of Al and Ti as solutes  .Vacuum melting processes

 Co-base alloys  absence of Al and Ti as solutes Air melting processes.

 Relevance of Melting of Superalloys
Relevance of Melting of Wrought Superalloys:
Melting Process Superalloys Use

VIM B-1900, 731 C Mostly remelt for castings

MAR-M-246 or for powder atomization
Rene 41, Rene 95
IN 718, IN 100

VIM/VAR IN 718, IN 901 Generally used for forging

Rene 41, A 286 for stock and rolled
Waspalloy shapes.
Udimet 500
Udimet 700
VIM/ESR Haynes 188 Primarily cast as slag
Nimonic 155 ingots for flat rolled
L 605, IN 625 products.
A 286
 Melting of Superalloys

Fig.2 Flow diagram of Melting processes used to produce superalloy components

 Vacuum Induction Melting (VIM) of Superalloys
Equipment and Procedures:

 In VIM, an induction furnace is placed

in a vacuum chamber and so operated
that the melting, tapping of the furnace
melt and the casting of the metal are
accomplished without breaking the
vacuum.

 The melting operation is through a high-

frequency induction furnace. The lining
of the furnace should withstand the
vacuum condition.

 For large furnaces, steam ejectors are

used to handle large gas loads followed
by diffusion pump.
Schematic Diagram of VIM Furnace
 Furnace Size: 1 to 60 tonnes

 Vacuum:
Roughing Pump: From 1 atm to 1000 micron
Diffusion Pump: Down to 10 micron
 Vacuum Induction Melting (VIM) of Superalloys
Equipment and Procedures:

 Since all superalloys require complex control of 8 to 20 elements to tighter

ranges or to maxima, hence great care will be required in calculating furnace
charge calculations, weight out and expertise in retention of various elements
in the melt.

 Select proper balance of virgin, scrap and remelt (recycled) materials for
charging that will facilitate melting to the required specifications. Therefore, a
careful control procedure especially in terms of chemical analysis should be
in place to ensure their correct usage and in correct proportions between
virgin, scrap and recycled inputs.

 Virgin materials are in following forms:

Electrolytic Ni, Fe, Nb, Cr, Co and Mn
Armco Fe, Ni pellets, W and Mo roundels
Ferro-Alloys: Fe-Cr, Fe-Mo, Fe-Nb

 Loose powder charges are never used.

Vacuum Induction Melting (VIM) of Superalloys
Melt Practice:

 Pumping down to desired vacuum level and achieving a satisfactory leak rate.

 Power turned and commencement of melting.

 Initial virgin charge will contain non-reactive elements including sufficient C

for de-oxidation during melt down.

 If a mixed heat (virgin/scrap) is to be made, the presence of reactive elements

must be taken into account.

 The virgin charge to be refined first before clean scrap is added, followed by
alloying additions.

 Progress and completion of the de-oxidation and refining reactions can be

assessed through continual leak rate checks.

 The melt is adjusted to pouring temperature and heat is tapped.

 Vacuum Induction Melting (VIM) of Superalloys
Melt Practice: The resultant product can vary from large electrodes to be further remelted by VAR/ESR to
small ingots in a wide variety of investment casting applications.
 Removal of Oxygen:
 De-oxidation is primarily done by the available C to form CO, i. e. removed by the vacuum
process.
 Initially “Carbon Boil” take place vigorously through boiling stage into desorption stage
where CO pressure is insufficient to nucleate bubbles. Hence, CO will form only at the melt
surface where it desorbs into the vacuum.
 The final D.O. level of 20 ppm (0.002wt%) is achieved.
 Oxygen gets introduced into melt from melt reactions with the furnace refractory lining (An
Intrinsic Problem).

 Recombination of Oxygen with reactive elements leads to generation of oxide inclusions.

 Al2O3, MgO, ZrO2 and their mixes are practically used in all VIM furnaces and they
contribute to oxide inclusions in the melt.

 Solution for Oxide inclusions: Minimise contact time with molten metal at high
temperature.
Avoid corrosive slag layers and films.
Use tight brick tolerance.
Select good quality and high density bricks.
Vacuum Induction Melting (VIM) of Superalloys
 Removal of Other Elements:

 Presence of Pb, Se, Cu, Bi, Te are detrimental.

 They have high vapour pressure an therefore can be easily removed under
vacuum.

 Natural stirring of the melt due to induction effects helps in refining process.

 Trace elements like As, Sn, Sb cannot be removed under vacuum and so to be
controlled by raw material selection.
Vacuum Induction Melting (VIM) of Superalloys
Advantages of VIM
 Flexibility due to small batch sizes.

 Low losses of alloying elements by oxidation.

 Achieve very close compositional tolerances.

 Removal of undesirable trace elements with high vapour pressure.

 Removal of dissolved gases O2 and N2.

 Achievement of directional solidification of the ingot from bottom to top,

thus avoiding macro-segregation and reducing micro-segregation.
Benefits of VIM:
•Melting, refining, alloying and casting under vacuum

• Controlled addition of high reactive elements

• Close tolearance achievable for various alloying elements such

as Al, Ti, Nb, Zr, etc.

• Reduction of gas content (H, N, O) and removal of undesirable

trace elements
 Vacuum Arc Remelting (VAR) of Superalloys
Vacuum Arc Remelting:

 Remelting and Refining process.

 Purpose: Produce high quality ingot

by controlling

 Solidification
(macrostructural control)

 Improved Cleanliness
(microstructural control)
 Vacuum Arc Remelting (VAR) of Superalloys
Equipment and Procedures
 Starting material – Cast / Forged electrodes and Copper mould = Water-cooled

 Heat required by the process is supplied by the electrical energy.

 D. C. Power: Voltage: 20 – 30 V and Operating current: 5000 – 30,000 A

 Electrode = –ve pole and Crucible = Grounded (+ve)

 Melting = Under Vacuum
• Roots Pump : Vacuum upto 200 – 500 micron
• Diffusion Pump: Reduces upto 1 – 5 micron at start of melting
 VAR is initiated by striking an arc into a small quantity of metal chips placed on crucible base.

 Power is increased till the progress of melting reaches a pre-determined level based on
desired melt rate.

 In VAR, solidification rate is much slower than conventional ingot static casting because of
desire to control segregation.

 Near the end of the melt, power is gradually reduced in order to hot-top the ingot and
minimise size of shrinkage cavity.

 At the end of melting, the assembly is cooled and removed from the melt station and the
mould is stripped from the ingot.
 Vacuum Arc Remelting (VAR) of Superalloys
Metallurgical Reactions:

 In VAR process, the elements concentration (such as Ni, Cr, Mo, Nb, Al, Ti) remain uniform
throughout the ingot.

 The elements Si, S, P that are carried from VIM ingots cannot be removed .

Advantages of VAR:

 Cleanliness by removing inclusions during remelt cycle.

 Oxide inclusions that float are ultimately taken to the edge of the pool at the mould wall. Hence,
the metal built up there will contain agglomerated inclusions of both oxides and nitrides.

 As VAR does not remove S, hence optimum selection of raw materials during primary VIM process.

 The primary advantage of VAR process is its inert nature w. r. t. reactive elements like Ti, Al and
controlled solidification structure that is obtained in the ingot.

Disadvantage of VAR:

 Inclusions are concentrated at the ingot wall adjacent to the mould and the ingot needs to be removed
by grounding prior to hot working. This leads to loss of costly materials.
 Vacuum Arc Remelting (VAR) of Superalloys
Ingot Defects in VAR Process: “Tree Rings”

 The features “Tree Rings” are chains of fine

equiaxed grains that interrupt a predominantly
columnar dendritic structure.

 Tree Rings can be observed visually on etched

transverse section of VAR ingot as “concentric
circles”.
Fig. Macrograph of "tree-ring" type patterns in IN-718. Pattern is
a result of solidification perturbation of melt pool causing non-
 Tree Rings formation correlate with disturbance uniform dendritic growth and grain size variations
in the thermal fields ahead of the columnar
dendritic tips and have been associated with
occurrence of defects.

 However, Tree Rings do not have significant

effect on materials properties as compared to
Freckles and White Spots

Fig. Micrograph of IN-718 structure illustrating non-uniform

microstructure. Severe dendritic segregation produces variations in
the gamma prime solvus which affects grain growth parameters
(Kalling's etch).
 Vacuum Arc Remelting (VAR) of Superalloys

Fig: Section from static-cast Waspaloy electrode showing both

longitudinal and transverse planes. Note the circular appearance of
Fig: Freckles in IN-718 nickel-base superalloy billet forged freckles on the transverse plane and the obvious ‘‘channel’’ nature of
from vacuum arc remelted ingot in which control of melt the freckles in the longitudinal plane
conditions was lost. Note: Composition of freckle vs.
matrix was by microprobe and does not show carbon, which
would be elevated in the freckles.

Ingot Defects in VAR Process: “Freckles”

 These are dark-etched circular or nearly circular spots that are generally rich in carbides or carbide
forming elements (Ti, Nb).

 Freckle formation is a result of a high metal pool depth and sometimes of a rotating pool.

 The liquid pool can be set in motion by strong magnetic fields.

 Freckles can be avoided by eliminating disturbing magnetic fields or by maintaining low pool depth.
 Vacuum Arc Remelting (VAR) of Superalloys
Ingot Defects in VAR Process: “White Spots”

 Typical defects in VAR ingots.

 These are recognized as light-etched spots on a

macro-etched surface.

 They contain low amount of alloying elements e.g. Ti

in IN 718.

Mechanism of White Spot formation:

Fig: Transverse billet section of IN-718 Ni-base
superalloy, macro-etched to show solidification
• Residues of unmelted dendrites of the consumable white spots resulting from too low a VAR melt rate
electrode in the ingot.

• Pieces of ingot crown that fall in metal pool and are

not dissolved or remelted and get embedded in the
ingot .

• Pieces of ingot shelf region transported into the

solidifying interface of the ingot.

 All the mechanism are singularly or in combination

Fig: Transverse billet section of IN-718 Ni-
may be responsible for ingot defect in the VAR base superalloy macro-etched to show VAR
process. shelf location and depth at billet surface
 Electroslag Remelting (ESR) of Superalloys
 Electroslag Remelting (ESR) is another secondary refining technique. Here,
remelting does not occur by striking an arc under vacuum.

 The process is conducted in air under molten slag.

 Both ESR and VAR allow directional solidification of an ingot from bottom to
top yielding high density and homogeneity in its microstructure as well as an
absence of segregation and shrinkage cavities.

 Primarily, ESR consists of producing an ingot from a cast or forged electrode

immersed in a molten slag with heat supplied by an electrical energy.

 Melting is usually done in an air environment.

 However, an inert gas cover of Ar can be preferably maintained over the melt
surface.

 The ingot is built up in a water-cooled Copper mould by melting the consumable

electrode that is immersed in a liquid slag which is superheated by resistance
heating
 Electroslag Remelting (ESR) of Superalloys
Equipment and Process
 Power Source:
40 – 50 V, 5000 – 30000 A, AC, 50 Hz

 Slag composition:
CaF2 with additions of Al2O3 and CaO.

 Ingot size:
30 – 70 cm rounds or (30 cm x 122 cm) section.
Process:
 ESR is initiated by pouring hot liquid slag into
the Cu crucible or by causing arcing between the
electrode and metal chips on the mould base,
thereby melting an initial slag volume placed in
the mould. This is called hot start or cold start
respectively.

 Melting is conducted at a controlled voltage with the current linked to the melt rate and electrode feed
rate linked to the voltage controls.

 As the melting about to complete, the ingot is hot tapped to prevent pipe and stripped after allowing
enough time for the slag to solidify.

 The ingot may be air cooled or slow cooled (or annealed) depending upon alloy and size.
 Electroslag Remelting (ESR) of Superalloys
Equipment and Process

 ESR furnace operates in an open air environment with fume collection equipment to remove
vapourized CaF2.

 Electrode position in the slag is very important (Electrode immersion is shallow).

 The immersion depth must be accurately controlled because of heat balance an current flow
requirements.

 ESR is mostly used for solid-solution hardened alloys.

Metallurgical Reactions:

 ESR is done under a slag blanket in an air or gas environment.

 Interactions among the molten metal, slag and environment result in a much more complex
metallurgical process than in VAR.

 Al, Ti, Si, Ta, Zr are the elements that have a high degree of affinity to O 2.

 Less reactive elements Ni, Mo, W are not affected.

 Electroslag Remelting (ESR) of Superalloys
Metallurgical Reactions:

 ESR has a potential for shipping S from superalloys during the remelt cycle. S removal reactions are
as follows:

[S] metal + CaO  CaS + MO : metal/slag interface

CaS + 3/2 O2 CaO + SO2 : slag/metal interface

 It shows that saturation of slag with S does not take place and desulphurization capacity of slag
remains intact throughout the remelting process.

 Tramp elements such as Mn, Bi, Pb, are not removed in ESR – since there is no vapourization.
Therefore, remove them through appropriate slag composition.

 O2 and N2 cannot be removed by ESR.

 ESR is very suited for inclusion removal through electrode/slag interface by the method of
dissolution.
 Electroslag Remelting (ESR) of Superalloys
ESR - Advantages and Disadvantages:

 ESR is at a disadvantage due to complexity of the process of metallurgical reactions.

 ESR ingots have very good surface quality. A smooth ingot surface requires no
conditioning prior to hot working. This gives higher yields.

 VAR defects such as Freckles, Tree Rings also occur in ESR ingots. However, there is no
white spot in ESR ingots.
 Future Option for Melting of Superalloys
 Modification of existing processes and the development of alternatives in an effort to provide cleaner
and more uniform microstructures are ongoing.

 Future options in processing sequences may involve Argon/Oxygen degassing prior to VIM in the
primary step.

 Secondary melting techniques may include Electron Beam Cold Hearth (EBCH) refining, in addition
to VAR and ESR techniques.

 This EBCH is attractive because it is refractoryless and has demonstrated an ability to remove oxides,
and offers a greater degree of process control.

 Triple melting alternatives may be represented by the VAR and Vacuum Arc Double Electrode Remelt
(VADER) processes.

 VADER is unique process because it can accept ultraclean electrode being semi-continuous and yields
the material in a refractoryless environment.
 Types of Superalloys Vs Melting Process
 The austenitic high Ni superalloys and Ni-base solid-solution superalloys are generally Electric Furnace
(EF) melted.

 Inconels and Incoloys are EF melted followed by Argon-Oxygen Decarburization (AOD) processing

 Hastelloys are generally EF melted and then ESR, although VIM followed by ESR may also be
employed.

 Some other superalloys may be simply Electric Arc Furnace (EAF) melted.

 Precipitation-hardening Fe-based superalloys are melted by EF or VIM and then VAR or ESR.

 Double VIM may be employed when critical applications are involved.

 In general, vacuum melting improves cleanliness and trace-element sensitive properties such as fatigue
strength, ductility and impact strength, but no significant effect on tensile strength.
 Types of Superalloys Vs Melting Process
 The precipitation-hardening Ni-based superalloys are generally Double VIM and then VAR or ESR.

 VIM lowers the gas content (H2, N2, and O2) and evaporates trace elements (such as Pb, Bi, Cd, Te, As,
Sb, and Se).

 Presence of these trace elements can adversely affect the mechanical properties and workability of ingots
and some these elements can also adversely affect service life.

 Secondary remelting using VAR and ESR processes further refines the alloy by eliminating gases, non-
metallic and metallic impurities and inclusion.

 Secondary remelting also produces larger ingots of uniform composition and dense homogeneous
structure.

 ESR is done by arc melting under a cover of slag and the removal of S is quite easy compared to vacuum
melting processes.

 High S levels are deleterious to the workability and properties of wrought heat-resisting alloys,
particularly high Ni- based superalloys.
 Advantages of Remelting (VIM + VAR)
 Low oxygen/better cleanness.

 Increased uniformity, top to bottom and centre to edge of ingot

 Reduced anisotropy in mechanical properties

 Reduced micro/macro segregation

 Greater cast to cast reproducibility

 Improved forgeability

 Less forging required to achieve consolidation

 Low inclusion content and fine size

0.2% Yield Strength, MPa

% Reduction in area

Potential of vacuum remelting is high with the usage of virgin metals

compared to scrap