Unit-IV Powder Metallurgy of Superalloy

Forming Processes of Superalloys
Forming of Superalloy
Superalloys
UNIT-I: Introduction to superalloys
Guide to selection of superalloys, wrought superalloys, Heat Resistant alloys. Physical Metallurgy:-
Microstructure of wrought Heat-Resisting Alloys, Microstructure of Ni-base & Co-base heat-resistant casting
alloys. Temperature and Time-dependent Transformation. Application to Heat Treatment of High Temperature
Alloys.
UNIT-II: Relationship of properties to microstructure in superalloys.
Fracture properties of superalloys. High temperature corrosion and use of castings for protection. Effect of
Physical Metallurgy and process variables on the microstructure of wrought superalloys. Process and
Metallurgical factors affecting on superalloys and other high temperature materials.
UNIT-III: Melting Process
Melting of Superalloys; Principles and practices of Vacuum Induction Melting and Vacuum Arc melting.
UNIT-IV: Forming Methods
Forming and Fabrication of superalloys; Recent developments in P/M of superalloys-Production of
components by Hot-Isostatic Pressing.
UNIT-V: Casting Methods
Improving turbine blade performance by solidification control-the development of single crystal turbine
blades. Quality of superalloys castings; Heat Treating of Heat resistant alloys
TEXT BOOKS:
1. Superalloys: Source book; Mathew J. Donachie. Jr. Editor; 1984.
2. The Superalloys: Edited Chester T. Sims and William C Haagel; 1972
REFERENCE:
1. High Temperature MATERIALS - Campbell IE, John Wiley and Sons Inc.;1956
2. The Superalloys: Fundamentals and Applications - Roger C. Reed
3. Superalloys: A Technical Guide - Elihu F. Bradley - 1988 - 280 pages
4. Superalloys: A Technical Guide - Mathew J. Donachie, Stephen J. Donachie
Paradigm Shift in the Technology Development of Superalloys
Fig: Trends in the alloy and processing

development of superalloys
Forming Processes of Superalloys:
 Wrought heat-resistant superalloys are manufactured in all mill forms common to the metal
industry.
 Fe-based, Co-based and Ni-based superalloys are produced conventionally as bar, billet, extrusion,
plate, sheet, strip, wire, and forgings by primary mills.
 Inconels and Hastelloys also are available as rod, bar, plate, sheet, strip, tube, pipe, shapes, wire,
forging stock and specialty items from secondary converters.
 Cast structure is refined by a working operation known as cogging.
 In this process, hydraulic presses are used with open dies.
 Uniform billet structure and improved surface finish are additional objectives of this process.
 Initial ingot break-down is followed by methods such as forging, rolling, or extrusion.
 Sheet, bar, and ring rolling are commonly employed for secondary hot working of superalloys.
 Edge cracking is a problem i.e. minimized by rapid handling.
 Working temperature ranges for many Ni-based superalloys are seen in below figure.
Forming Processes of
Superalloys
Fig: Temperature ranges for the

hot forming of various Ni-based
superalloys.
 Forgings are used in both the turbine and compressor sections of gas tubes.
 Rates of die closure vary from 0.3mm/s for hydraulic presses to 7.5 m/s for hammers.
 While most forging is carried out with steel tooling heated in the range of 200 to 430ºC, isothermal
forging is now widely used for near-net shape processing.
 Superalloy or Mo alloy dies are heated to the same temperature as the forging, in the range of 650 to
980ºC.
 Isothermal forging produces a uniform microstructure while requiring less material, thereby lowering
machining costs.
 For temperatures at which superplastic behaviour of superalloys occurs, less powerful presses or
hammers and slower die closure rates can be used.
 But these benefits are overtaken by the increased costs of hot die tooling for expensive input materials.
 Extrusion is used for the conversion of ingot to billet, especially for the stronger, crack-prone alloys, as
well as for powder-processed alloys.
 During extrusion, canning in mild steel or stainless steel is required to avoid chilling and surface
cracking.
 Glass is the most common lubricant. Seamless tubing is also produced by this method.
 Sheet and other semi-finished products are produced by rolling, often with many reheats, frequent
conditioning, and possibly encasing of the alloy in a can.
 Open-die forging is carried out in flat or swaging dies.
 Closed-die forging is used to produce shapes that match the impressions of dies attached to the ram
and anvil.
 Both hammers and presses are used, for the hammers, stresses required for deformation are higher
because of the higher strain rates employed.
 A few superalloys can be cold formed on high –capacity equipment by drawing, extrusion, pressing
and deep drawing , spinning or rolling.
 For all processes except rolling, a lubricant is usually required and speeds are relatively low.
 The uniform fine-grain microstructures resulting from cold working and re-annealing lead to
improved mechanical properties.
 Grain structure may be controlled by thermo-mechanical processing in several Fe-Ni-based alloys that
have two precipitates present, the primary strengthening precipitate (γ’’ [Ni3Nb] in Inconel 718 and γ’
[Ni3Ti] in Inconel 901) and a secondary precipitate (δ in Inconel 718 and η [Ni3Ti] in Inconel 901).
 The secondary precipitate is produced first, by an appropriate heat treatment (8 h at 900ºC for Inconel
901), followed by working at about 950ºC, below the η solvus.
Thermo-mechanical Processing of Superalloys
 Final working is carried out below the recrystallization temperature and the alloy is subsequently
recrystallized below the η solvus.
 Finally, the alloy is aged by standard procedures. The result is a fine-grain alloy with higher tensile
strength and improved fatigue resistance.
 The critical warm-working temperature range for Inconel 718  900 to 955ºC.
 The upper limit avoids grain coarsening at higher temperatures due to re-solution of δ, while the lower
limit is established to avoid an excessively high flow stress during working.
 δ and γ’’ precipitates compete for the available Nb, hence any factor suppressing δ tends to favour γ’’
formation and vice-versa.
 δ does not strengthen Inconel 718, but it reduces the room temperature ductility.
 However, when some δ phase is precipitated prior to or during working, the grain size can be reduced
substantially, leading to increased tensile and fatigue strength.
 Other thermo-mechanical working schedules are used to produce a double necklace structure of fine
grains surrounding the large grains formed during high-temperature recrystallization.
 Reductions of 25 to 50% are needed in the final working operations at 1080 to 1110ºC to produce the
small recrystallized grains in cast/wrought Rene 95.
Powder Metallurgy of Superalloys
Powder Metallurgy of
Superalloy
Relevance of Powder Metallurgy of Superalloys:
 Powder-based superalloys are used when “Conventional” cast or wrought components will not
meet the performance requirement of the application which leads to increased of power generation.
 Superalloy parts made of P/M techniques are being used in advanced turbine engines because of
the following ADVANTAGES:
1. Ability to produce near-net shapes which results in reduced materials input and less machining to
produce a finished component.
2. Reduced segregation due to rapid solidification rate, resulting in smaller intermetallic particles and
reduced inter-dendritic spacing not achievable in practical sized components through casting
process.
3. Reduced energy requirements and shorter delivery time because the P/M process requires fewer
processing steps than conventional ingot technology. Forgeable microstructure to achieve very
high level of mechanical properties.
4. Ability to achieve unique structure for special environments (e.g. ODS Superalloys) not achievable
other than P/M process.
Relevance of Powder Metallurgy of Superalloys:
 LIMITATION of P/M techniques for the broader application in turbine components
1. Increased residual gas content
2. Carbon contamination
3. Ceramic inclusions
4. Formation of prior particle boundary made by oxide and/or carbide films.

Application of Powder Metallurgy processing:
1. Compressor and Turbine Disks (Operating temperature: 540 – 760 ºC):
 The powder metallurgy components are produced from pre-alloyed atomised powder.
 The powder (for majority of applications) is consolidated by Hot Isostatic Pressing (HIP) or
hot extrusion.
 These billets or preforms are for the most part subsequently forged to near-net shape.
 In general, the strength of these superalloys is a direct function of the γ’ content.
 Powder processing permits attainment of a fine grain size, which lends superplastic forming
capability.
 These superalloys are characterized by a high homogeneous concentration of both solid-

solution forming and γ’ forming elements of Al, Ti.
Application of Powder Metallurgy processing:
2. Static Vanes in Turbine section (Operating temperature upto 1100 ºC):
 These components are produced from ODS superalloys.
 In this process, elemental or master alloy powders including very fine oxide powder, are mixed
together in the solid state and form homogeneous powder particles by mechanical alloying.
 This powder is then consolidated to full density by hot extrusion and is subsequently
directionally recrystallized to a specific crystallographic texture which result in stable but
anisotropic structures.
 The oxide dispersion provides strength through dislocation pinning at temperature above those
where γ’ strengthening is ineffective.
 These alloys also show very good environmental surface through generating adherent oxide
coating.
Main components of Powder Metallurgy superalloy processes:
1. Production of spherical pre-alloyed powder.
2. Sieving to remove oversize particles.
3. Blending the powders to homogenize the powder size distribution.
4. Consolidation process.
5. Thermo-mechanical processing.
Powder Making processes:
 All the powder making processes are necessarily carried

out in inert atmosphere (either gaseous environment or
vacuum).
 It is necessary to achieve powder free from oxides,

carbides, nitrides, to be able to obtain sound inter-
particle bonding in the consolidated product.
Fig: Schematic of melt stream
 These processes for superalloy powder making are breakup during gas
atomization
named as
1. Inert Gas Atomisation (IGA).
2. Soluble Gas Atomisation (SGA).
3. Rotating Electrode Processes (REP and Plasma REP).
 The atomized superalloy powders are generally spherical in nature and are used in fine – mesh
cuts {-100 mesh, [150 μm] to -325 mesh [43 μm] in order to minimize contamination effects on
critical flow size considerations.
Powder Making Processes of Superalloys
1. Inert Gas Atomisation (IGA):
 Vacuum induction refined superalloy is remelted in an inert-gas

atmosphere and poured into a tundish through which the molten
metal exits as a stream and is inserted through a gas nozzle.
 The nozzle delivers a continuous stream of inert gas at high

pressure to the molten metal stream which is disintegrated into
spherical particles.
 Inert gases (mainly argon, but also helium) are used for
atomizing nickel-base superalloys, whereas steam, which
oxidizes the melt, has been reported as an alternative atomizing
medium for the production of cobalt-base superalloy powders.
 IGA consists of a long cooling tower with a nozzle at its upper

end, through which a stream of molten metal is atomized by
argon at high pressure. These particles cool at rates ~ 102C/s.
 The powder is collected at the outlet of the atomization

chamber.
 The whole unit can be evacuated to a pressure of 0.2 atm (0.2

μm) during the melting procedure. Fig: Schematic cross-section of an inert-gas
atomization (IGA) unit
1. Inert Gas Atomisation (IGA):
 In order to decrease any pressure differences (which

might develop by thermal expansion of the argon
during atomization and which could cause closure of
the nozzle opening), excess gas is re-circulated, and
cooled, from the cooling tower to the melting chamber,
hence allows the processing of fairly large amounts of
melt stock into powder.
 The solidified metal particles are further cooled by a

cooled plate at the bottom of the unit and are
transported into a series of glove boxes, where sieving
and size classification can take place.
 The oxygen content of the powders processed by inert-

gas atomization is typically between 40 and 200 ppm.
Figure: Schematic view of powder

atomization nozzles: atomizing gas Fig: Schematic cross-
stream impinging (a) at an angle α section of an inert-gas
and (b) tangentially from a nozzle atomization (IGA) unit
 SGA process involved atomization upward from an lower

induction melting crucible in a melting chamber maintain
either pressure or vacuum and an upper expansion
chamber, maintained under a vacuum of less than 10000
μm.
 The melt environment, (above atmospheric pressure)

contains a partial pressure of gas i.e. soluble in the molten
alloy (usually H2).
 A valving mechanism is actuated in the upper chamber and

the gas-saturated molten metal is transferred to the
expansion chamber through a ceramic transfer tube.
 The atomization takes place by immersing a tube (usually

ceramic) into the melt.
 The metal leaves the tube orifice as a fine spray of molten

droplets formed by the sudden release of the soluble gas.
 The droplets are directed primarily in upward atomization

chamber (under a low vacuum) by an open end of the tube Fig: Schematic of the soluble-
in nozzle arrangement. gas atomization process
 The molten metal in the tube is subjected to the combined

effect of the pressure to vacuum and the dissolution of the
soluble gas causes the metal to be atomized.
 Cooling rates of 103C/s are typical as measured from dendritic

arm spacing.
 The cooled powder is drained from the expansion tank under

vacuum into a tank, which is then sealed off and back-filled
with a non-reactive gas.
 The contamination of alloy powder in this processes is from

the refractory system for melting and molten metal transfer.
 At a pressure of 7atm, the order of 5 moles of H 2 in solution

can be held in100-kg molten metal.
 The powder produced by the vacuum atomization process is

spherical, with few satellites, and has a typical tap density of
69% of theoretical.
 Large number of Ni-based superalloys manufactured: IN100, Fig: Schematic of the soluble-
MERL 76 and LC Astroloy. gas atomization process
3. Rotating Electrode Process (REP and Plasma-REP).
 In both REP and PREP, an electrode of the alloy

composition with typical diameters from 15 to 75 mm
is rotated at very high speeds (ranging from 10000 to
20 000 rpm). in an inert chamber.
 In REP, a non-consumable W electrode is used to strike

an arc to the surface of the alloy electrode.
 The face of the rotating consumable alloy electrode is Fig: Schematic of the REP
melted by a direct-current (d.c.) electric arc maintained
between the stationary W electrode (-ve), and the alloy
electrode (+ve).
 The melting surface of the rotating electrode

centrifugally removes the molten metal surface to fly
off in the form of spherical droplets which freeze in
flight and drop to the floor of the tank.
 The tank interior is evacuated and back-filled with

helium or argon before powder is made, with the result
that no change occurs in the gas content of the powder
as compared to the starting electrode.
Fig: The principle of the transferred arc plasma REP (PREP)
3. Rotating Electrode Process (REP and PREP).
 In contrast to gas atomization, potential slag or

refractory contamination is eliminated.
 Cross-contamination by W inclusions originating from

the W tip electrode has been of major concern, and
hence, Ti alloys considered as an alternate.
 One major drawback of this method  It is

discontinuous, since it requires the use of well- Fig: Schematic of the REP
machined bars to be used as electrodes.
 A process variant (the plasma rotating-electrode

process, PREP) utilizing a plasma torch with a d.c.
transfer arc used to melt the superalloy electrode
surface instead of a W electrode, has been developed.
 The torch is water cooled, and He gas flows between

the W anode and the nozzle.
 The stream of He gas keeps the alloy powder from

reaching the W cathode, thus preventing W erosion
and powder contamination.
Fig: The principle of the transferred arc plasma REP (PREP)
3. Rotating Electrode Process (REP and PREP).
 The radius of atomization has to be equated with the radius of the

spinning consumable rod.
 By suitable heating, a metal film is obtained which flows outward under

the effect of centrifugal force.
 Primary disintegration of the melt occurs at the rim of the rod, ideally a
mono-size particle diameter results, (value depends on the equilibrium
between the centrifugal force acting on the droplet and the surface
Fig: The general principle of
tension force exerted by the melt on the droplet). centrifugal atomization (REP)
 Cooling rate as high as 105C/s for IN 700 powder have been produced from PREP instead of REP.
 Most superalloy powder produced currents is spherical and has a tap density of ~ 65%.
 Superalloys subjected to atomization processes have high volume fraction of γ’ and refractory element
composition showing unacceptable segregation in conventional cast/ wrought processing.
 Alloy composition for powder processing remains same except for lower C content since carbide are not
necessary for grain size control and may cause problem in particle bonding.
 Ni-based superalloys commonly used are Rene 95, Low C IN 700, MERL 76, Low C Astroloy –
Forging Bar
4. Rapidly Solidified Powder (Gatorizing):
 Rapid Solidification Rate of Powder production:

Solidification rate of powders exceeds 10 5 K/s
 For superalloys, the objective of the high rates is to

obtain a micro-crystalline alloy rather than an amorphous
materials.
 Apart from extremely fine grain size, such powders

display non-equilibrium solubilities and very uniform
composition because of the very fine dendritic arm
spacings resulting from rapid solidification.
 Both conventional superalloys and new alloys based on

Ni-Al-Mo-X alloys, where X=Ta or W, have been Fig: Schematic of the rapid-solidification-rate
prepared by RSR. (RSR) atomization process
 Rapid Solidification processing can be done by centrifugal atomization with forced convective cooling as
shown in Fig.
 In this method, the alloy is vacuum induction melted in the upper part of a chamber.
 The chamber is then back-filled with He gas and the alloy is poured in pre-heated tundish.
 The liquid is poured through tundish nozzle onto a rotor that is spun at 24000 rpm.
4. Rapidly Solidified Powder (Gatorizing):
 The melt is accelerated to rim speed and then ejected

longitudinally as droplets.
 Further atomization and cooling of the droplets is

accomplished by the injection of He gas through annualr
nozzzles.
 Spherical powder in the 10 to 100 μm diameter range is

produced.
 The cooling rates typically varies between 10 5 and 107

K/s, the higher rates being achieved with the smaller
particles.
Fig: Schematic of the rapid-solidification-rate
(RSR) atomization process
 Rapidly solidified powder may be prepared from melt
spun ribbon i.e. pulverized after solidification.
 The ribbon is produced by pouring the melt through an orifice under pressure and impinging it on a
rotating wheel of e.g. Cu, that acts as a heat sink.
 Typical cooling rates are approx. 106 K/s and ribbon thicknesses are less than 25 μm.
 The ribbon must be mechanically pulverized .
 This method is generally limited to small quantities of experimental superalloys.

Fig: Typical RSR atomized powder, screened to -140+ 170

Fig: Typical argon atomized Fig: SEM of Soluble-gas-atomized
mesh (average diameter 98 μm). Note the lower incidence
superalloy powder, screened to -- Ni-based superalloy powder
of satellites in comparison to vacuum or argon atomized
140+170 mesh (average diameter powder.
98 μm).
(a) (b)
Fig: As-HIP Rene 95 turbine disks

(a) As-HIP, (b) Sonic shape, (c) Finished machined disk
(c)
Mechanical Alloying process for Powders :
Fig: Schematic of a high energy ball mill

(attritor) for mechanical alloying
Fig: Representative constituents of starting powders used in mechanical alloying,

showing deformation characteristics during attritor ball milling
Mechanical Alloying process for Powder s :
 Mechanical Alloying process is followed for making

components based on ODS alloys.
 Mechanical Alloying is solid-state process (i.e. No melting

takes place) in which elemental or master alloy particles and
oxide particles in predetermined proportion are mixed together
in a high energy ball mill.
 The particle size of the master alloy mix: 2-200μm
 The particle size of the oxide alloy mix: <10 μm Fig: Sketch showing formation of
mechanically alloyed superalloy
powder particles in a ball mill
 During milling the energy of the rotating balls is dissipated
either as heat or in collision with powders.
 The collision causes inter-particle welding, plastic deformation

and fracturing.
 The process is carried out in an inert atmosphere, so that

welding and fracturing takes place between atomically clear
surfaces.
 The process is done for 24 h. Fig: Surface morphology of mechanically

alloyed superalloy powder
Mechanical Alloying process for Powder s :
 X-ray analysis of properly milled powder reveals only one

crystal structure , intermediate to the elemental constituents.
 The incorporation of very fine (200-400Å) inert oxide

particles (usually Y2O3-Al2O3) provide the basics of
dispersion strengthening of the subsequently consolidate
powder.
 The oxide particles represent ~ 1% volume of the alloy.
 This powder is not spherical but is rather acicular or plate-

like.
 ODS processing has been applied to solid-solution

strengthening alloy (MA 754) or γ’ strengthened (MA 6000)
alloys or ferritic (MA – 956) alloys.
 MA 6000 alloys offers a good intermediate temperature

strength, a shortcoming of MA 754 and MA 956.
 It is reported that at least 4 wt% Al is required to provide Fig: Progress of

oxide scale formation. mechanical alloying.
Powder Properties:
 Atomized Powder:
 Shape morphology = Spherical;
 [O]= ~100 ppm
 Power size distribution = Gaussian
 Structure = Either microcrystalline or dendritic (governed by
particle size and cooling rate)
 Oxidized powder particles are deleterious to properties such

as ductility and LCF life.
 These particles are generated during atomization as a result of

Fig: Powder size distribution for similar
transient air leaks in the system. alloys atomized via different processes
 Hollow particles are also found in atomized powdered arising form either entrapped Ar or Solidification
shrinkage.
 These pores generally close during consolidation and only the entrapped Ar variety can open during
subsequent high temperature exposure.
 Contamination from other alloys (Gross-contamination) produced in the same equipment is a source of
defect generation that can limit the minimum properties of the component.
 Gross-contamination can lower hardness of the alloy or an alloy with a different γ’ solvus resulting in a
few scattered coarse grains or carbide-powder boundary problems in the consolidated powder.
SEM micrographs of microstructures

typically observed in superalloy powders,
(a) dendritic, (b) cellular.
SEM micrographs of microstructures

typically observed in superalloy powders,
(c) microcrystalline, and (d)
splat cooled.
Mechanically alloyed powder:
 Shows significantly different powder

characterization than atomized powder.
 When looked at on a microscopic scale, the

powders shows a banded structure with
spacing of ~0.5μm with Y2O3 oxide particles
of 200-400Å spaced at ~0.1μm.
 The banding can be eliminated in the powder

by annealing at 1200ºC, which causes
recrystallization to irregular equiaxed grains.
 This type of thermal excursion occurs during

densification.
 The typical particle size is plate-like discs of

Fig: Various microstructural stages during mechanical alloying
about 200x100μm by 50 -100μm thick.
Powder Consolidation:
 Pre-consolidation steps: The powders before consolidation must be stored under inert or at least
controlled environment condition to minimize contamination.
 Various studies have shown that the desorption of surface gases occurs over a range of temperatures and
the deleterious species, i.e. H2O, CO, CO2 and CH4, evolve from the surface from 100ºC for H2O to
about 600ºC for CO (peak desorption).
 These contaminants will be responsible for particle-particle bonding (PPB) retention and attendant
properties.
 All densification involves the containerization of the powders under vacuum.
 The container is disposed off subsequent to densification of the powder.
 The powder is usually loaded into its consolidation container (metal) under a dynamic vacuum.
 The evacuated container is then sealed and ready for consolidation.

Fig: Possible processing sequences for a gas turbine

compressor disk illustrating the input weight
reductions possible with P/M superalloy technology
Fig: Schematic of thermo-mechanical processing sequence in the

production of consolidated mechanically alloyed superalloy components
Powder Consolidation and Thermo-mechanical processes:
 Superalloy powders are consolidated to full density using a combination of temperature and pressure.
The two principal techniques used to consolidate superalloy powders for aerospace applications.
(a) Hot Isostatic Pressing (HIP): Followed by conventional forging.

(b) Extrusion followed by isothermal forging.
Fig: Schematic of a hot isostatic pressing (HIP) facility

Fig: A complex HIP consolidation container
Powder Consolidation and Thermo-mechanical

processes: (a) Hot Isostatic Pressing:
 Powder-filled container are placed in an

autoclave that is subsequently heated and
pressurized
 Typical temperature 1095ºC -1205ºC

 Pressure 103 MPa
 The combination of pressure and temperature, as

the container is transferred to the powder mass
and affects densification.
 The general goal of the HIP consolidation is to

have a fully dense product (~98% of TD)
Powder Consolidation and Thermo-mechanical processes:
 Container used range from single cylindrical container to be

made into sheet pipe to complex-shape containers.
 By P/M process, a preform shape is obtained which can be

worked into a desired by final shape, thus preventing
segregation and workability problem encountered in casting
an ingot and working it to a final shape.
 For Hipping and forging process, Powder of spherical shape

with low [O] are used as produced by IGA/SGA/PREP
processes.
Fig. Schematic of tooling used for
direct hot forging of powders to
 Typical alloys are Rene 95, Astroloy, IN 100 and MERL-76. prevent container buckling
Fig: Schematic of extrusion consolidation using a

filled billet to achieve a shaped final consolidate
Fig: Schematic of powder extrusion
Powder Consolidation and Thermo-mechanical processes: (b) Extrusion of Loose Powder:

 Extrusion of Superalloys powders can be done either as extrusion of loose powder or extrusion of a pre-consolidated
billet.
 Extrusion will result in achieving full density.
 It requires a specialized container with a nose plug designed to protect the evacuation stem on the container from
rupturing prior to entering the extrusion die .
 With extrusion of pre-consolidated billet, (if the powder pre-consolidated by HIP), in a separate forging press or in the
Fig: Schematic of extrusion consolidation using a

filled billet to achieve a shaped final consolidate
Fig: Schematic of powder extrusion
Powder Consolidation and Thermo-mechanical processes: (b) Extrusion of Loose Powder:

 Typical extrusion temperature for P/M superalloys: 1040ºC -1175ºC.
 Isothermal forging is carried out a low strain rates to reduce force requirements and cracking tendencies of these
materials.
Fig: Integrally bladed turbine disk

produced by isothermal forging in
segmented dies
Fig: Schematic of a die set for forging of
integrally bladed disks by isothermal forging
Fig: View of a hydraulic isothermal forging press

utilizing TZM tooling; the vacuum chamber surrounding
the die set has been opened
Isothermal Forging:
 In the isothermal forging process, the dies are maintained at same temperature as the forging stock.
 This eliminates the die chill completely and maintains the stock at a constant temperature throughout the forging cycle.
 The process permits the use of external slow strain rates, then taking advantage of the strain rate sensitivity of the flow
stress of strained alloys.
 This process is able to produce near-net shape forgings that do not required any machining.
Hot Compaction and Extrusion:
 In this process containerized powder is hot compacted (usually is closed die, although HIP can be used) at a sub-solvus
temperature.
 The consolidated powder (>95% denser) is subsequently extruded between a ratio of ~ 6:1 to fully dense billet.
 The structure of subsequent extruded billet has a fine recrystallized structure with almost complete elimination of prior
powder boundaries and any dendritic structure carryover from the starting powder production process.
 Typical extrusion temperature for P/M superalloys: 1040ºC -1175ºC.

Hot Compaction and Extrusion:
 In the subsequent hot isothermal forging, both the work piece for the die are heated to the same temperature and forging
at low strain rate to achieve the net-shape of the component.
 This also eliminates die chill problems. This results in significant cost saving due to reduced material usage and reduced
machining.
 Alloys such as Astroloy, IN 100, Rene 95, MERL 76 comprise of bulk isothermally forged P/M tonnage.
 Properties of P/M Superalloy:

Grain size: Typical grain size of the current P/M superalloys: ASTM 7-12
Typical grain size of the Cast and Wrought superalloys: ASTM 3-6
 Tensile strength and ductility increases as grains become finer.
Fig: Micrographs of typical P/M processed superalloys:

(a) extruded and isothermally forged Rene 95 and (b) hot isostatically pressed Rene 95
 The as-consolidated microstructures of extruded and HIPed superalloy powder is shown in Fig.
 The very fine microstructure of the powder is retained.
 Fig. a - Extruded and forged material, has a somewhat finer structure, due to the higher degree of
deformation, which can lead to recrystallization.
Consolidation of ODS powder:
 ODS powders are not necessarily handled inertly and can be cold compacted to ~ 80% density.
 This can be done by uniaxial pressing or cold isostatic pressing.
 The cold compacted mass or loose powder is then containerized, heated to a high temperature and
extruded to full density.
 The resultant product (due to oxide dispersion) extremely fine grained (1μm).
 The extruded bar may be used in post-consolidation heat treated condition or further worked (forged).
 Regardless of whatever consolidation operation, the final step in processing is a recrystallization step
in a thermal gradient that results in elongated grains that are very stable due to inert oxide pinning.
 This step is performed at ~ 1260ºC. Often each grain can be several inches long.
 This grain size and directionality contributes to the excellent high temperature strength and stability to
the material.
Mechanically Alloyed Product Availability.
 Mechanically alloyed material is available as mill products or custom forgings.
 The mill product forms of mechanically alloyed ODS alloys vary, depending on factors such as ease of fabrication and
applicable forming methods.
 Common forms include bar, plate, and sheet.
 All of the bar products can be precision forged.
 Plate is readily amenable to a variety of hot forming operations, including hot shear spinning.
 Optimal formability and minimum flow stress are obtained when the plate is in the fine-grain (unrecrystallized)
condition.
 Later on the standard grain-coarsening annealing is applied to the formed component.
 The only alloy currently available in sheet form is MA-956 and also has been produced in a number of other forms,
including pipe, thin-wall tube, and fine wire, for special applications.
 MA-956, which is readily cold rolled to standard sheet tolerance, is commercially available in gages down to
thicknesses of 0.010 in. (0.25 mm) and widths up to 24 in. (610 mm).
 A wide variety of components have been cold formed from MA-956 sheet by standard metal-forming operations.
 Warming to about 95ºC is necessary to prevent cracking, because this alloy undergoes a ductile-to-brittle transition in
the vicinity of room temperature.
Mechanically Alloyed Product Availability.
 MA-754 has been produced as hot rolled wire.
 In addition, (although not a mill product) both seamless and flat butt-welded rings have been made from MA-754 and
MA-758.
 Alloy MA-754 was the first mechanically alloyed ODS superalloy to be produced on a large scale. This material is
basically a Ni- 2O-Cr alloy strengthened by about 1 vol% Y2O3.
 It is comparable to thoria-dispersed TD Ni-Cr (an earlier ODS alloy strengthened by thoria), but it has a nonradioactive
dispersoids.
 Alloy MA-758 is a higher-Cr version of MA-754 and was developed for applications in which the higher Cr content is
needed for greater oxidation resistance.
 The mechanical properties of alloy MA-758 are similar to those of MA-754, when identical product forms and grain
structures are compared.
 Alloy MA-956 is a ferritic Fe-Cr-Al alloy, dispersion strengthened with yttrium aluminates formed by the addition of
about 1 vol% Y2O3.
 Due to good hot and cold fabricability, MA-956 has been produced in the widest range of product forms of any
mechanically alloyed ODS alloy.
 In sheet form, MA-956 alloy is produced by a sequence of hot and cold working, which yields large pancake-shaped
grains following heat treatment.
 This grain structure ensures excellent isotropic properties in the plane of the sheet.
Applications for MA Alloys.
 Mechanically alloyed ODS alloys were used first in aircraft gas turbine engines and later in industrial turbines.
 Components include vane, airfoils and platforms, nozzles, and combustor assemblies.
 Manufacture of diesel engine glow plugs, heat treatment fixtures (including shields, baskets, trays, mesh belts, and
skid rails for steel plate and billet heating furnaces), burner hardware for coal- and oil-fired power stations, gas
sampling tubes, thermocouple tubes, and a wide variety of components used in the production or handling of molten
glass.
 Due to high long-time elevated temperature strength, alloy MA-754 has been extensively used for aircraft gas turbine
vanes and high-temperature test fixtures.
 Alloy MA-758 has found applications in the thermal processing industry and the glass processing industry.
 Alloy MA-956 is used in the heat treatment industry for furnace fixturing, racks, baskets, and burner nozzles.
 Alloy MA-956 is also used in advanced aerospace sheet and bar components, where good oxidation and sulfidation
resistance are required in addition to high-temperature strength properties.
 Other P/M Applications.
 The shaft and disk of the back section of the compressor in F-404 turbofan engines were made of HIP Rene 95.
 Rene 95 P/M superalloy parts produced as near-net shapes by direct HIP were cost-effective due to improved
material use and significant reduction in machining requirements.
Biomedical Applications of P/M Superalloys.
 Since Co-based alloys used in orthopaedics are difficult to machine, near-net shape
capability is desirable.
 Both casting and P/M processes have the ability to produce near-net shapes.
 However, the inherent ductility and toughness of wrought products (P/M or

conventional forged) is to be preferred in the demanding environment of the human
body.
 Although many orthopaedic implants are made by casting, P/M techniques are used to
make some implants.
 Fully dense implants are made by HIP of pre-alloyed powders to provide materials with
excellent mechanical properties.
 Figure shows hip and knee joints, which constitute the most common total joint
replacements.
Fig: Sketch showing
location and shape of
 The major implants produced by HIP are total hip replacements made from a Co-Cr-Mo some conventional
alloy that meets the composition requirements of ASTM F 799. orthopaedic implants
made of P/M cobalt-
 Requirements for powders used in implant production include compositional control, base superalloys
consistent tap densities (to ensure consistency of final part dimensions when working
with fixed-mould cavity dimensions), and a high degree of powder cleanliness.
 The standards of aerospace P/M are applied to powders used in biomedical applications.
 Currently, all P/M-processed orthopaedic implants have been made with powders

Unit-IV Powder Metallurgy of Superalloy

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Unit-IV Powder Metallurgy of Superalloy

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Forming Processes of Superalloys

Fig: Trends in the alloy and processing

 Cast structure is refined by a working operation known as cogging.

 In this process, hydraulic presses are used with open dies.

 Initial ingot break-down is followed by methods such as forging, rolling, or extrusion.

 Edge cracking is a problem i.e. minimized by rapid handling.

Fig: Temperature ranges for the

 Open-die forging is carried out in flat or swaging dies.

 LIMITATION of P/M techniques for the broader application in turbine components

1. Increased residual gas content

4. Formation of prior particle boundary made by oxide and/or carbide films.

1. Compressor and Turbine Disks (Operating temperature: 540 – 760 ºC):

 In general, the strength of these superalloys is a direct function of the γ’ content.

 These superalloys are characterized by a high homogeneous concentration of both solid-

2. Static Vanes in Turbine section (Operating temperature upto 1100 ºC):

 These components are produced from ODS superalloys.

1. Production of spherical pre-alloyed powder.

2. Sieving to remove oversize particles.

3. Blending the powders to homogenize the powder size distribution.

 All the powder making processes are necessarily carried

 It is necessary to achieve powder free from oxides,

1. Inert Gas Atomisation (IGA).

2. Soluble Gas Atomisation (SGA).

3. Rotating Electrode Processes (REP and Plasma REP).

 Vacuum induction refined superalloy is remelted in an inert-gas

 The nozzle delivers a continuous stream of inert gas at high

 IGA consists of a long cooling tower with a nozzle at its upper

 The powder is collected at the outlet of the atomization

 The whole unit can be evacuated to a pressure of 0.2 atm (0.2

 In order to decrease any pressure differences (which

 The solidified metal particles are further cooled by a

 The oxygen content of the powders processed by inert-

Figure: Schematic view of powder

 SGA process involved atomization upward from an lower

 The melt environment, (above atmospheric pressure)

 A valving mechanism is actuated in the upper chamber and

 The atomization takes place by immersing a tube (usually

 The metal leaves the tube orifice as a fine spray of molten

 The droplets are directed primarily in upward atomization

 The molten metal in the tube is subjected to the combined

 Cooling rates of 103C/s are typical as measured from dendritic

 The cooled powder is drained from the expansion tank under

 The contamination of alloy powder in this processes is from

 At a pressure of 7atm, the order of 5 moles of H 2 in solution

 The powder produced by the vacuum atomization process is

 In both REP and PREP, an electrode of the alloy

 In REP, a non-consumable W electrode is used to strike

 The melting surface of the rotating electrode

 The tank interior is evacuated and back-filled with

 In contrast to gas atomization, potential slag or

 Cross-contamination by W inclusions originating from

 One major drawback of this method  It is

 A process variant (the plasma rotating-electrode

 The torch is water cooled, and He gas flows between

 The stream of He gas keeps the alloy powder from

 The radius of atomization has to be equated with the radius of the

 By suitable heating, a metal film is obtained which flows outward under

 Rapid Solidification Rate of Powder production:

 For superalloys, the objective of the high rates is to

 Apart from extremely fine grain size, such powders

 Both conventional superalloys and new alloys based on

 The melt is accelerated to rim speed and then ejected

 Further atomization and cooling of the droplets is

 Spherical powder in the 10 to 100 μm diameter range is