A TECHNICAL MEMORANDOM ON

Mg Superplasticity

Submitted By: Under The Guidance Of:

Ashvani Kumar Dr. Rahul R. Kulkarni
(FF18M06) Assistant Professor
M. Tech (Foundry - Forge Technology) Department of Forge Technology

“NATIONAL INSTITUTE OF FOUNDRY & FORGE TECHNOLOGY”

RANCHI
Acknowledgement

I would like to express my special thanks of gratitude to my professor Dr. Rahul

Ramesh Kulkarni who gave the valuable guidance for this assignment which
was like a golden opportunity to do the wonderful work on the topic “Magnesium
Superplasticity”, which also helped us in doing a lot of work and we came to
know about so many new things regarding the work and its presentation.

I would also like to thank Dr. Manoj Kumar for sharing his views and sparing
his valuable time over “Magnesium Forging” in his regular classes.

I would also like to thank my friends and colleagues who helped me a lot in
finalizing this report within the limited time frame.
 Overview

 Superplasticity
 Mechanics
 Requirements
 Advantages
 Disadvantages

 Methods to develop the superplasticity

 Application of superplasticity in commercial magnesium alloy for

fabrication of structural components

 Experimental investigation of superplastic behaviour in Magnesium

alloys

 Applications

 References
 Superplasticity

 Superplasticity is a state in which solid crystalline material is deformed well beyond its
usual breaking point, usually over about 600% during tensile deformation.[1]

 Superplasticity is the capability of a material to endure strains while applying low flow
stresses without constriction and practically no strain-hardening.[2]

 Superplastic forming is a viable technique to fabricate hard to form materials into

complex shapes.[3]

 Instead of trying to restrict the creep deformation, this approach takes full advantage of
the ease of deformation at elevated temperatures; metals, alloys, intermetallics, and
increasingly ceramics, can be made to deform to very large strains in tension. The
extremely large ductility associated with such deformation is termed superplasticity.[4]

Mechanics of Superplasticity-The large neck-free elongation during superplasticity comes

from the resistance to necking in certain microstructural and deformation conditions. This
resistance to necking is best measured by the value of the strain rate sensitivity parameter, m,
given by ϭ ∝ϵm, where ϭ is the stress and ϵ is the strain rate. For m=1, often referred to as
Newtonian viscous flow, the change in cross section area becomes independent of Area, a
reason for the large ductility exhibited by glass at elevated temperatures. Crystalline materials
exhibit m=1 at very slow strain rates, and the regime is not considered practical for forming
processes.

One of the dominant microstructural features in superplasticity is the role played by grain
boundary sliding (GBS). Concurrent accommodation processes, which may involve grain
boundary migration (GBM), maintain the grain compatibility during GBS, grain rotation,
diffusion, or dislocation motion. The accommodation mechanisms considered can be divided
into three groups: (i) diffusion accommodation, (ii) accommodation by dislocation motion, and
(iii) combined models having elements of both dislocation and diffusional accommodation.

The three prime requirements for the manifestation of micro grain superplasticity are:
(i) a fine and equiaxed grain size (less than about 10 µm for metallic materials and 1 µm for
ceramic materials) that is reasonably stable during deformation, (ii) a temperature that is more
than about half of the melting point of the matrix in absolute degrees, and (iii) a strain rate that
is typically not too high (less than 10-2 s-1) or too low (more than10-6 s-1).

The phenomenon of grain boundary sliding constitutes an important topological requirement

in superplasticity. In order to facilitate the process of grain boundary sliding, the sliding
interfaces should be high-angle boundaries. For similar reasons, the grain shape should be
equiaxed, because three-dimensional grain boundary sliding cannot take place easily in a
matrix with elongated grain structure. The phenomena of grain boundary sliding and migration
are often intimately linked processes. Hence, the grain boundaries of a superplastic matrix
should also be mobile. [4]
  The low temperature Superplasticity as well as high strain rate Superplasticity is due to
the grain size effect.[3]

 The exploitation of the superplastic behaviour is especially reasonable for magnesium

alloys because of their restricted cold-working properties [5] low density-1.738g/cc. Mg
alloys exhibit poor ductility near the room temperature, because of the h.c.p. lattice,
which does only provide 3 of the necessary 5 independent slip systems for arbitrary
deformation at RT. The activation of additional slip systems above 200 °C is therefore
important for any major forming operation. The critical resolved shear stress for
deformation in these systems at lower temperatures is much higher. This shortage of
slip systems with easy movable dislocations is the reason for small plasticity of
hexagonal metals. [6]

 Grain refinement in magnesium 1.)Increase the strain rate (or stress) leads to faster
forming rates, thereby reducing forming time in the process, 2.)Decrease the
temperature below recrystallization temperature.[3]

 Superplastic forming is suitable to fabricate a structural component of magnesium with

a reasonable high strength as well as high ductility.[3]

Advantages:[7]

1. Vastly improved formability is obtained compared with conventional forming

processes even for high-strength low-ductility materials. Thus processes requiring large
amounts of deformation can be performed in one operation, often producing
components with complex shape. As a result, multistage manufacturing processes that
involve extensive welding or machining may be bypassed, or previously unattainable
shapes may be produced.
2. Forming pressures are drastically reduced; in some cases enough to make feasible the
use of cheaper, novel, or more lightweight, forming equipment.
3. Considerable cost savings may be made mainly because extremely close tolerance can
be guaranteed which reduces machining costs and the process is not, therefore, labour
intensive.
4. Wastage is minimized so that there is maximum utilization of material, which is an
important saving in energy intensive materials such as Ti or Al or Mg alloys.
5. A uniform microstructure is produced which leads to uniform, reproducible,
mechanical properties throughout the body of the finished product.
6. Service properties are generally improved over conventionally formed material because
a fine, uniform grain size is obtained which leads to better strength, ductility, and
fatigue resistance.

Disadvantages:[7]

1. The creep properties of the component are often inferior to those obtained by
conventional forming routes, primarily because of the fine grain size.
2. The process is not, in general, suitable for rapid mass production techniques although
reasonably short forming times are possible. Consequently, superplastic forming is only
feasible for low-to-medium batch production.
 Methods to develop the superplasticity

In order to reduce grain size, several processes have been used: severe plastic deformation,
powder metallurgy techniques, rapid solidification, friction stirring or hot rolling.

1.) Hot extrusion- Alloys are processed by powder metallurgy (PM) or ingot metallurgy
(IM) or rapidly solidified (RS) and then extruded. The superplastic behaviour is
estimated in PM samples at higher strain rates compared with samples prepared with
IM route.[6]

Figure 1. Hot extrusion [8]

2.) Thermomechanical treatment- An alternative route to prepare superplastic alloy is

the thermomechanical treatment (TMT) consisted from the heat treatment in two stages
(homogenisation at 470 oC for 10 h and ageing at temperatures from 200 to 380 oC).
Aged samples were hot extruded at 350 oC .The grain size of samples and superplastic
behaviour depends on the ageing temperature. This method is relatively simple and big
bulks of the material may be prepared. It is an advantage against other methods, for
example, high-pressure torsion technique, which is able to manufacture only small
samples. [6]

3.) Equal channel angular pressing- Excellent superplasticity of samples prepared by

equal channel angular pressing (ECAP) was observed at a relatively high temperature
of 300 oC. Then superplastic behaviour after ECAP at a constant temperature (eight
passes) of 265 oC (CT) and at decreasing temperature in each following pass from 265
down to 150 oC in the last one was developed. A substantial grain refinement was
observed for both ECA extrusion techniques. ECAP technique with decreasing
temperature caused a decrease in the grain size up to submicrocrystalline region. Later
researchers developed a new method for preparation of fine-grained materials involving
sequential application of hot extrusion and ECAP. Very small grain size (about 1 µm)
was very probably the reason for the occurrence of superplastic flow at a relatively low
temperature of 0.48TM. [6]
 Figure 2. Equal channel angular pressing [9]

4.) Hot rolling -Sheets are prepared by repeated rolling (RR) at 400 oC. The rolls are
annealed between rolling passes at 130 oC. Resulting grains are equiaxed and no twins
are observed in the microstructure. Rolling and heating are applied around 11 times. [6]

Figure 3. Hot rolling [10]

5.) Friction stirring- Friction stir processing (FSP) is usually used for the friction stir
welding purposes. This method may be applied as a novel grain refinement technique.
[6]
In the friction stir processing, a rotating tool, with a specially designed rotating probe,
travels down the surfaces of metal plates, and produces a highly plastically deformed
zone through the associated stirring action (as shown in Fig.4). The localized thermo-
mechanical affected zone is produced by friction between the tool shoulder and the
plate top surface, as well as plastic deformation of the material in contact with the tool.
The probe is typically slightly shorter than the thickness of the work piece and its
diameter is typically the thickness of the work piece. The friction stir processing (FSP)
process is a solid-state process and therefore solidification structure is absent and the
problem related to the presence of brittle inter-dendritic and eutectic phases is
eliminated. The frictioned zone consists of a weld nugget, thermomechanically affected
zone (TMAZ) and a heat affected zone (HAZ). In this case, the stirring action of the
tool on the bulk material is used for a forging/extrusion treatment at very high
temperatures. Dynamic recrystallization and grain rotation leads to a very fine
microstructure. Submerged friction stir processing (SFSP) is realised underwater and it
has a great potential in the preparation of ultrafine-grained materials .[11]An excellent
 superplastic behaviour of SFSP samples especially at higher strain rates was ascribed
to finer structure and larger fraction of grain boundary. A combination of the high-
pressure die casting (HPDC) with the FSP resulted into ultrafine material with the grain
size lower than 1 μm and excellent superplastic properties at 330 oC and at relatively
high strain rates.[6]

Figure 4. Schematic illustration of (a) friction stir processing, and (b) the tool used in
the present investigation. [12]

6.) High-pressure torsion- Samples processed by high-pressure torsion (HPT), have a

fine-equiaxed grain structure with a significant thermal stability .The thermal stability
is due to high volume fraction of nanosized γ-phase particles. The main mechanism is
grain boundary sliding accommodated by dislocation creep process and diffusional
process. The fine fibrous microstructure resists cavitation and links the disconnected
grains. [6] The HPT processing was conducted under a quasi- constrained condition at
room temperature and at a speed of 1 rpm using an applied pressure of 3.0GPa for
differing numbers of turns (N): 1, 3, 5, and 10 turns. The peripheries of both anvils were
coated with a lubricant containing MoS2 to avoid any possible damage to these areas
during processing. [13]

Figure 5. High-pressure torsion [14]

7.) Vertical Twin-Roll Strip Caster-The vertical twin-roll strip caster is composed of two
equal diameter counter-rotating rolls (as shown in Fig. 6). The rolls are normally made
of high thermal conductivity of copper/steel alloys. Their axes of rotation are located
in the same horizontal plane. The main equipment used within this process is the
crucible, the tundish, the molten metal feeding system (nozzle), and the rolls. In this
process, the liquid metal is supplied from the tundish through a nozzle into the wedge-
shaped region formed by the two counter-rotating rolls. When the superheated liquid
metal comes in contact with the moving rolls, solidification starts with the extraction
of heat from the liquid metal to the roll surface and a thin solidified shell is formed on
each of the roll surfaces. With the continuous extraction of heat through the moving
rolls, the solidified shells gradually grow in thickness. Finally, the two solidified shells
contact with each other and weld together at the nip of the rolls (minimum distance
between the rolls) and the material exits from the caster in the form of a solidified strip.
From the microstructural observation, they found that the microstructure of the strip
has smaller grains with better mechanical properties as compared to strip prepared by
continuous casting The solidification phenomena in twin-roll strip casting process
depend on the following process parameters of twin-roll strip caster:
(i) Diameter of the roll.
(ii) Roll material.
(iii)Casting speed.
(iv) Roll gap.
(v) Metal delivery system.
(vi) Metal-roll heat transfer coefficient

Figure 6. Schematic diagram of vertical twin-roll strip caster [15]

Application of superplasticity in commercial magnesium alloy for
fabrication of structural components [3]
Effect of grain refinement on superplastic characteristics
To investigate grain size effect, three materials were selected. A coarse grain material
AZ31(Mg-3Al-1Zn-0.2Mn,wt-%) which were received in the form of as rolled sheet with an
average size of ~130µm;an extruded AZ31 bar which had a fine grained structure with an
average size of ~5 µm and AZ61(Mg-6Al-Zn-0.2Mn,wt-%) extruded sheet with an average
grain size of 17 µm .All three materials have been tested at different temperatures and strain
rate ranges where their respective superplastic flow behaviour was determined.
OBSERVATION
Flow stress at a given temperature and strain rate decreases with grain refinement. The slope
of the curves at 598K indicated that that the stress rate sensitivity m increases from 0.33 to 0.5
with grain refinement. The optimal strain rate, where a maximum elongation to failure is
obtained, also increases with grain refinement as shown in Figure.7.

Figure 7.
MATERIAL
A commercial ZK60 alloy of chemical composition Mg-6Zn-0.5Zr (wt-%) was used in the
present study of superplastic forming. The material was received in an as extruded condition.
As received alloy of fine grains of size 2-5.The alloy would be expected to deform
superplasticity at a reasonable strain rate of 10-2 s-1 owning to the fine grained structure.
MECHANICAL PROPERTIES AT ELEVATED TEMPERATURES
a) The slope of the curve at a high strain rate of 10-1 s-1 exhibits m ~0.5 corresponding to
the dominant deformation mechanism of grain boundary sliding.
b) The present alloy exhibits a large elongation to failure, more than 200% for the
temperature examined as shown in Figure 8. The above deformation behaviour supports
the possibility of grain boundary sliding during deformation.

Figure 8.
The elongation to failure increases with temperature and reaches almost a constant value of
~300% above the temperature of 673K, while the flow stress decreases monotonically with
increasing temperature as shown in Figure. 9.

Figure 9.
Summary
An investigation of the superplastic characteristics of magnesium alloys with several grain
sizes revealed that grain boundary sliding took place more easily with grain refinement. The
required grain size for high strain rate superplastic forming was estimated to be ∼2 µ
Experimental investigation of superplastic behaviour in Magnesium alloys

The required grain structure could be obtained by several procedures, hot extrusion with a high
extrusion ratio, severe plastic deformation via equal channel angular extrusion, consolidation
of machined chip, and/or powder metallurgy processing of rapidly solidified powders, on a
laboratory scale.

1.) As a result of the subsequent two-stage heat treatment of the cast material(solution
treatment at 470 oC for 10 h and air quenching; overageing at a temperature in the range
of 200–380 oC for 10 h; and., the precipitates at the grain boundaries are dissolved, and
a homogeneous structure results. The grain size of the structure after deformation
process (warm extrusion moulding at 350 oC) has decreased to the range of 0.7–6.4
microns; this condition is highly favourable for good superplastic properties. [2]

2.) A powder metallurgy (PM) process can give rise to a smaller grain size, compared to
an ingot metallurgy (IM) process. The PM Mg alloys exhibited superplastic behaviour
at higher strain rates, compared with the IM Mg alloys. It has recently been pointed out
that a liquid phase plays an important role in high strain rate superplasticity in the case
of aluminium alloys exhibiting superplasticity at very high strain rates, >10-1 . [16]

3.) Extensive grain refinement through intense plastic straining (IPS) is an effective route
to enhance superplastic properties of Mg alloys. Superior superplastic properties in
sheets of the ZK60 magnesium alloy by IPS through combination of conventional
extrusion, compression and subsequent isothermal rolling are developed. [17]

4.) Grain refinement by isothermal rolling was found to be beneficial to enhancement of

superplasticity in AZ61 alloy, while it was not in AZ31 alloy because of rapid grain
growth during forming. It was found that rolled AZ61 alloy exhibited a maximum
elongation of 580% at 2×10-4 s-1 and 673 K. [18]

5.) Superplasticity with an initial grain size of 300 microns has been observed.
Superplasticity of coarse-grained Mg–3Al–Zn alloys (AZ31) has been investigated.
Elongation of 320% has been obtained at 773 K and a strain rate of 10 -3 s -1. The grains
were refined from initial 300 to 25 microns when the stress reached its maximum. The
grain size maintained about 25–30 microns dynamically in the proceeding deformation.
The deformation includes two stages, i.e. grain refinement stage and superplastic
deformation stage. The former is controlled by dislocation slip and climb, while the
latter is controlled by a competing mechanism between grain growth and grain
refinement. [19]
 Applications

Historically, the Volkswagen 'Beetle' motor car has represented the largest single application
of magnesium alloys which were used for crank case and transmission housing castings that
weighed a total of 17 kg. This was said to represent a saving of 50 kg when compared with
using cast iron which was critical for the stability of this rear engine vehicle.

In this latter regard, it has been estimated that each 10% saving in the deadweight of a motor
vehicle corresponds to an increase in fuel economy of 5.5% which, In turn, means reduced
exhaust emissions.

Figure 10. [20] is the seat frame for a Mercedes- Benz roadster which has been produced from
five AM20 and AM50 magnesium alloy die castings and weighs 8·4 kg. It is claimed that a
comparable steel seat design would weigh an estimated 35 kg and require between 20 and 30
stampings and weldments.
Figure 11. [20] Shows a Ford steering column assembly which comprises three magnesium
alloy die castings and weighs 1·2 kg. Magnesium castings in the high performance Porsche
911 model motor car have a total finished weight of 53 kg.
Figure 12. [21] Shows some automotive components made of Mg alloy and obtained weight
reduction
Figure 13. [20]
Figure 14. [21]Examples of automotive components made of Mg alloys (a: Engine block, b:
Steering column module, c: Door frame / Key lock housing, d: Oil pan,
Figure 15. [21]Examples of automotive components made of Mg alloys (e: Steering wheel, f:
Transfer case/Transmission housing, g: Seat frame,
Figure 16. [21]Examples of automotive components made of Mg alloys (h: Wheel
 References

[1] https://en.wikipedia.org/wiki/Superplasticity

[2] V. Wesling, T. Ryspaev, A. Schram, Effect of overageing temperature on the

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[3] Mukai, T. & Watanabe, H. & Higashi, K., Application of superplasticity in commercial
magnesium alloy for fabrication of structural components, Materials Science and
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[4] A.K. Mukherjee, R.S. Mishra, Superplasticity, Encyclopedia of Materials: Science and
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[5] V. Wesling, T. Ryspaev, A. Schram, Effect of overageing temperature on the

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[6] Zuzanka Trojanová, Zdeněk Drozd and Pavel Lukáč (November 5th 2018).
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[7] Mukai, T. & Watanabe, H. & Higashi, K., Application of superplasticity in commercial
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[8] https://www.meks.in/2019/08/extrusion-and-its-types-with-advantages.html

[9] https://www.totalmateria.com/page.aspx?ID=CheckArticle&site=ktn&NM=367

[10] https://www.google.com/amp/www.engineersgallery.com/hot-rolling/

[11] P. Cavaliere, P.P. De Marco, Superplastic behaviour of friction stir processed AZ91
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[14] https://www.intechopen.com/books/severe-plastic-deformation-techniques/ultrafine-
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[15] M. Mabuchi, T. Asahina, H. Iwasaki & K. Higashi, Experimental investigation of

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[16] Galiyev, A & Kaibyshev, Rustam. Superplasticity in a magnesium alloy subjected to

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