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Pnys Techno, Vo '4 '983 Prinied in Nonher- ,elaid

THE ANCIENT CRAFT OF


SUPERPLASTICITY

One of the pleasures of metallurgy lies in its


C Hammond historical perspective: the realisation that progress
in understanding the properties of metals and alloys
and the development of new manufacturing and
Superplastic parts are nowadays used in processing techniques are brought about not so
cars, helicopters and aircraft wings. much by the discovery of the new as by the
Theories of superplasticity are still rediscovery of old ideas and the reapplication of old
developing today - but years ago the techniques. The notion that we have nothing to
technique may have helped the Saracens learn from what has been done before-that our
to stay sharp current research and manufacturing problems are
entirely neu and unique-is quite erroneous. (No
doubt it is also erroneous in other applied sciences
and technologies.) This historical aspect of
metallurgy is perhaps nowhere better illustrated
than in the field of superplastic forming which was
discovered or rediscovered only fifty years ago and
which is now a fabrication technique of increasing
importance. particularly for aluminium and titanium
alloys. Starting from sheet material. complex
shapes with smooth surface contours can be made
without the need to weld or rivet many separate
pieces together. Parts now made superplastically
include titanium alloy aircraft wing components.
aluminium alloy casings. shaped architectural
panels and motor car bodies (figure 1).
In order to understand (as far as we are able) the
property of superplasticity and its current appli-
cations we must first discuss the plasticity- the
ductility or malleability - of metals and alloys which
is of course one of the distinguishing properties of
the metallic state. We shall then find that
~

superplasticity is a high temperature deformation


Dr Christopher Hammond is a senior lecturer in the
property associated with alloys having particular
Department of Metallurgy , Universit! of Leeds.
microstructures. Later in the article I shall review
His research interests include superplasticity.
current industrial superplastic fabrication methods
creep and the structure and properties of titanium
and applications. Finally. we shall see how the
alloys A Fellon of the Royal Microscopical
rediscovery of superplasticity has not only led to
Society, he is also honorarq editor of the RIMS
the development of advanced manufacturing
Microscop) Handbooks
techniques but has also provided the key to an

263
The geometry of the atom arrangements in
crystals, around dislocations and at grain boundaries,
may be represented by a simple two-dimensional
ball bearing model (figure 2). Here the perfect
crystals or grains (where the ball bearings are
hexagonally close packed) can be seen to be
bounded by regions of disorder or misregistry
(grain boundaries) and some of the grains also
contain slight linear deviations from perfect close
packing (dislocations). Under an applied stress
these dislocations move through the crystal
structure, restoring the perfection of the structure
in their wake and resulting overall in the translation
of one part of the crystal with respect to the other.
Deformation is therefore brought about by the
movement (‘glide’ and ‘climb’) of very many
dislocations and their generation and annihiliation
Figure 1 Aston-Martin Lagonda car door panel in principally at grain boundaries. Dislocations, it is
aluminium alloy Spural (photography courtesy Superform now realised, also exist in minerals and ceramics
Metals Ltd)
but because of the directed nature of the ionic
bonds between atoms the stress required to move
understanding of the lost craft or technique by them is extremely large and moreover generally in
which Damascus steel sword-blades were forged. excess of that required to cleave the atoms apart.
Minerals and ceramics are therefore brittle. Physical
Physical basis of superplasticity metallurgy in the last thirty years or so has largely
The individual crystals or grains which make up a been a study of how dislocations move and interact
metal or alloy structure generally vary between a with other dislocations, grain boundaries and fine
micrometre and a millimetre in size. They are precipitate dispersions both within the grains and
invisible to the naked eye except in some special at grain boundaries.
cases, for example the ‘speckly’ surface of Physical metallurgy has therefore not only led to
unpolished brass door handles. The problem which a greater understanding of the underlying processes
physical metallurgists earlier in this century had to occurring in metal forming processes - for example
solve was how metals and alloys could deform rolling and extrusion at high and low temperatures -
without at the same time causing the breakdown of but has provided the basis for alloy development in
the crystal structure or the fracture of the crystals terms of alloy chemistry, grain size, precipitate
either along the crystal planes or between the distributions, etc.
crystal (or grain) boundaries. The problem was of The concept of dislocations moving through the
course solved by the introduction of the concept of crystal structure provides the basis therefore of the
dislocations which represent local regions of misfit observed plasticity of metals and alloys. The
or misregistry in the crystalline structure. amount of plastic deformation which can be
achieved is not easy to define since it depends very
largely on the nature of the deformation process,
Figure 2 Ball bearing model of grains; GB, grain but in simple tensile tests of cylindrical bar or
boundaries; D, dislocations: v, vacant sites rod-shaped specimens it is generally of the order of
10-30%. However, in 1934 C E Pearson, an
English metallurgist, reported that bars of a
tin-bismuth alloy (a material of almost no practical
significance) could be extended over 2000% -the
alloy exhibited properties more akin to those of soft
toffee or hot glass! This viscous or glass-like
property was found to occur only when the
individual grains which make up the alloy structure
were less than a micrometre in size. Moreover the
grains underwent no perceptible change in shape or
size from the beginning to the end of the
deformation: they remained ‘equiaxed’ rather than
being elongated as might have been expected.

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Pearson’s discovery was subsequently almost stabilises it against further thinning: the higher the
wholly neglected - the very word superplasticity value of m, the greater is the ‘hardening’ effect and
used to describe it is a translation from later therefore the greater the extent of plasticity which
Russian work - until it was realised that other, can be achieved.
useful alloys could also be made to exhibit this For Newtonian viscous flow m = 1, the flow
property. They could therefore be formed into stress is directly proportional to the strain rate, any
shape not only by conventional hot rolling or incipient neck is completely stabilised and very
extrusion methods but by techniques more akin to large extensions (as in glass-blowing) can be
glass-blowing, enabling complex shapes to be made achieved. When the deformation is accommodated
from sheet material without the need for joining by the movement of dislocations through the
together many different parts. grains, as outlined above, m values of the order of
There are two aspects to an understanding of 0.25-0.4 are predicted as well as observed,
superplastic deformation: the rheological aspect incipient necks are not fully stabilised against
which explains why bars or sheets of metal can be further thinning and maximum extensions of the
extended so much without localised thinning-down order of 30% only can be achieved. However, in
or ‘necking’ (which gives rise to a limited plasticity) superplastic deformation m values of 0.5 and above
and the physical metallurgical aspect which are observed and the characteristic large extensions
explains, or attempts to explain, why fine grained are obtainable, as shown for example in figure 3
materials at high temperatures exhibit this property which illustrates superplastic titanium alloy tensile
and indeed whether the property is solely limited to test bars before and after testing. It should be
fine grained materials. noted that in practice the maximum extensions
which can be achieved depend also upon other
Rheological and metallurgical aspects factors such as the formation of voids or surface
Let us examine the rheological aspect first. During cracks in the material - but this brings us to the
high temperature deformation - that is at tempera- physical metallurgical aspect of superplastic
tures of 0.6Tm or above (where T,,, is the melting deformation.
temperature in degrees kelvin)-the flow or The high m values characteristic of superplastic
deformation stress increases with the strain or deformation suggest that it occurs by some
deformation rate, the relationship usually being combination or balance of Newtonian viscous flow
expressed by the empirical equation: and dislocation movements and this is indeed the
case.
o = Ktm (l) Metals exhibit Newtonian viscous flow when the
where 0 is the flow stress, K a temperature deformation is accommodated by diffusional
dependent constant, E the strain rate and m the movements of atoms - the repeated exchanges of
strain rate sensitivity index. Now the numerical places between atoms and neighbouring vacant
value of m is important in determining the extent of sites (as illustrated in figure 2 ) . Such movements
plasticity which can be achieved in the extension of are of course enhanced at higher temperatures,
bars or sheets of metal. The reason for this is in where the concentration of vacancies and thermal
principle very simple. Suppose a neck-a slightly energy of the atoms increase. The effect of an
thinner region - occurs along a bar or in a sheet of applied stress is to cause directional, rather than
metal. There will be a concentration of stress and random diffusional movements, and the net result
therefore a localised increase in strain rate in this is that atoms migrate from one part of the crystal to
region. However, a localised increase in strain rate another, resulting overall in a strain. Now although
leads (from equation 1) to a localised increase in this process represents the basis of viscous flow it
flow stress, the more so the higher the value of m. may manifest itself in a number of ways. The
The localised increase in flow stress effectively diffusional movements may occur through the
‘hardens’ the incipient necked region and therefore grains; but except for a very high temperature of

Figure 3 Titanium alloy IMI 318 tensile test bars a, before and b, after superplastic deformation

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grains A and B have moved together and C and D
apart, resulting in a net change of shape or strain
for this group of four. This model is of course
idealised and it is envisaged that such movements
occur repeatedly throughout the whole grain
structure. The model predicts that the overall grain
shape and size remains unchanged (as is observed)
but that each grain undergoes localised strains or
small changes in shape as it slides from one
neighbour to another as can be seen in figure 4a-c.
If the grains were rigid, voids would necessarily
open up between them. These localised strains
Figure 4 Ashby-Verrall mechanism for a-c, grain need to occur only in the surface regions of the
boundary sliding and d, the possible dislocation/diffusion
paths grain - or mantle to use a geological analogy - and
can be accommodated by a combination of
diffusional creep (m = 1) and dislocation move-
0.85Tmor above, and for very fine grain sizes, this -
ment ( m 0.3). Hence the observed m values of
process of diffusional creep is very slow and the 0.5 and above represent the net result of a
predicted strain rates are very small. combination of these two processes. The arrows in
However, the diffusional movements are particu- figure 4d show possible paths for the movement of
larly marked at the grain boundaries which behave dislocations and the diffusional fluxes of atoms in
therefore as viscous layers between the grains, the ‘mantle’ of a grain.
enabling grains under the action of an applied stress
to migrate or slide ‘past each other and again Practical problems
resulting overall in a strain. The important metallur- In developing a superplastic alloy there are two
gical factors to be considered in this grain boundary practical problems which must be overcome.
sliding process are the effects of grain size and Firstly, a fine grain size is required and secondly at
the mechanisms by which sliding grains exchange the moderately high deformation temperatures
neighbours. The finer the grain size, the greater involved (0.6Tm or above) grain growth or
is the proportion of grain boundary surface area coarsening must be prevented or inhibited. Grain
and hence the greater is ,the effect. This there- coarsening also occurs by diffusional movements of
fore explains why superplasticity is generally only atoms across the boundaries from one grain to the
observed in fine grained materials. next. The grain boundaries then migrate in the
The ways in which sliding grains exchange places reverse direction to those of the atom movements
is still a matter of controversy. Figure 4 shows one across them; some grains shrink and are eventually
model, proposed by Ashby and Verrall, for a group annihilated, others grow and the overall grain size
of four grains. Figure 4a shows the initial increases. The process is readily envisaged by
configuration, figure 4b the intermediate situation reference to figure 2: small (diffusional) movements
and figure 4c the final configuration. Note that of atoms in the disordered region of the grain
boundary (GB) into ‘registry’ with the close-packed
Figure 5 Microstructure of IMI in superplastic condition arrangement of one or other of the grains results in
showing the two-phase structure of equiaxed (Y grains
(light) and p grains (dark). Optical micrograph of
a net movement of the grain boundary. The
polished and etched section thermodynamic driving force is the reduction in
grain boundary surface energy per unit volume and
it is now possible to observe the process directly
using a high temperature photoemission electron
microscope.
The first problem is solved by controlled
hot-rolling of the alloy which breaks up and refines
the grain size. The second problem is more difficult
and can be tackled in two ways which are
represented in practice by two alloys of commercial
importance-the aluminium alloy Supral (Al-
6%Cu-0.5%Zr) and the titanium alloy IMI 318
(Ti-6%A1-4%V). In Supral (produced by Super-
form Metals Ltd) the zirconium partly combines
with the aluminium to give an intermetallic

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compound ZrA13 which under the correct proces-
sing conditions occurs as a fine precipitate or
dispersion about 10 nm in size and distributed
throughout the grains and at the grain boundaries.
These ZrAI3 particles have the effect of pinning or
‘pegging’ the grain boundaries and therefore inhibit
grain growth. The function of the copper in the
alloy is not fully clear: it certainly strengthens the
alloy but may also have an effect upon diffusional
rates.
In IMI 318 (produced by IMI Titanium Ltd) the
vanadium and aluminium give rise to a two-phase
structure consisting of grains of entirely different
crystal structure (figure 5): a grains (with a Figure 7 Superplastically formed sphere 200 mm in
hexagonal close-packed crystal structure) and /3 diameter (right) formed by inflating rim-welded discs
(left) at 900 “C; note the argon gas inlet nozzle
grains (with a body-centred cubic crystal structure). (photograph courtesy British Aerospace)
The aluminium tends to concentrate in the a grains
but the vanadium is almost wholly concentrated in such as shown in figure 3. The specimen is brought
the /3 grains. In order for grain coarsening to occur up to the required temperature in a furnace
in such a two-phase structure, where the grains mounted on the tensile test machine and a fixed
have different compositions, long range diffusional strain rate i. is imposed on the specimen by the
movements are required; a-0 interphase grain machine and the stress IJ recorded. E is then
boundaries cannot simply migrate by the short- successively increased or decreased in steps and the
range (few atomic distances) movement of atoms stress recorded at each step. The strain rate
from one side of the boundary to another, but long sensitivity m is then determined from the slope of a
range diffusion of the order of the grain diameter logarithmic plot of U and E, i.e. from equation (1)
particularly of vanadium, must occur in order to
maintain the required chemical composition differ-
I g u = 1gK + lgd
ences. Long range diffusion is the ‘slow step’ in a d(lgu)/d(lgi) = m = slope of curve
grain growth process and hence grain growth is A set of data for IMI 318 over a range of
inhibited. This was, or is, also the structure in temperatures is shown in figure 6. Note that such
Pearson’s tin-bismuth alloy which again has a data enable one to determine the optimum strain
two-phase structure consisting of tin-rich and rate and temperature ranges for superplastic
bismuth-rich grains. deformation. For example it can be seen from
figure 6 that at lower temperatures and higher
Superplastic fabrication methods strain rates the slope of the curves, and therefore
Having established the microstructural conditions the m values, decrease below a value of 0.5. In
for superplasticity, the first requirement is to these regions conventional dislocation controlled
ensure that high elongations and high m values are deformation becomes dominant and superplasticity
obtained. m values are normally measured by the is lost. The next requirement is to test sheet
technique of strain-rate cycling tensile test bars material (extended tensile test bars having a limited
practical usefulness!) and this can be accomplished
by simply inflating two circular sheets of the alloy
Figure 6 Plot of lg U against lg t- for IMI 318. Each curve circumferentially welded round the edge. Figure 7
represents the data at a different temperature shows such a specimen (left) with a gas pressure
pipe inlet nozzle in the middle and the resultant
perfect sphere (right).
More complex shapes can be made by inflating a
sheet of the alloy into a cavity or mould of the
required shape and figure 8 shows diagramatically
one possible arrangement for Supral. This is the
basis by which parts such as are illustrated in figure
1 are made. Needless to say the practical problems
are those of ensuring proper control over
temperature and gas pressure (i.e. strain rate) and
in the case of titanium alloys there is the further
requirement of preventing oxidation - the compo-

267
problem which is now being overcome by slight
modifications in alloy chemistry and processing
a routes. The second development concerns mod-
ifications to the alloy content of IMI 318 and here it
is found that small additions (1% of cobalt or
Toot nickel) enhance the superplastic properties such
plate that in principle the process could be carried out at
/
lower temperatures (-825 "C) with the concomitant
reduction in the problem of oxidation. These
alloying elements owe their effect both to changes
in the properties of the CY and p phases and to the
fact that they enhance the diffusional flow of atoms
around grain boundaries. Thirdly, and most
importantly. superplastic forming for titanium
alloys is now being combined in one operation with
a joining process: atoms diffuse across the interface
in exactly the same way as they do across a grain
boundary. the interface is then annihilated in a very
b short space of time and a perfect joint is made.
Figure 9 shows a joint in an engine bay
nozzle panel which is made by diffusion bonding
corrugated and flat titanium alloy sheets. The inset
micrograph shows that all trace of the original sheet
surfaces has disappeared. The opportunities pro-
vided by this technique for highly sophisticated
designs are enormous.
Damascus steels
'The best of the new is often the long forgotten
past'.
Figure 8 Schematic diagram of superplastic forming This old Russian proverb brings us back to our
process for Supral; a, sheet of alloy is clamped around its
edges in a heated mould (or muffle box) and b. a gentle starting point because the discovery - or rediscov-
air pressure blows out the sheet and forces it into the ery-of superplasticity has not only led to the
shape of the mould @holograph courtesy Superform development of the most advanced manufacturing
Metals L i d ) techniques but has also provided the key to an
understanding of the lost craft by which Damascus
nent must be kept in an argon environment in its steels were made. Damascus steels, so called
moulding box and the whole enclosed within a large because they were first encountered by Europeans
uniform temperature furnace. there. have been used for making swords and
There are three aspects to the further develop- armour probably from the time of Alexander the
ment of superplasticity as a fabrication method. Great. By the time of the Crusades Damascus
The first is cost. Superplasticity, compared for swords were famous for their strength. toughness
example with sheet-stamping, is a relatively slow and retention of a fine cutting edge. However, the
forming process and is currently limited to metallurgy of Damascus steels has been shrouded
'medium-run' or high-cost parts in which the in mystery. It was known that the basic
advantages of fewer joints and reduction in weight material - small cakes or castings called Wootz -
in complex shapes set a premium. Secondly, mould originated from India. The first modern study of
design must be such as to avoid any preferential Wootz was made by G Pearson, who presented his
thinning round sharp radii of curvature and this is a findings to the Royal Society in 1795. Subsequently
field in which great ingenuity has been rewarded D Mushet concluded (correctly) in 1804 that Wootz
with great success. contained a much higher percentage of carbon than
Thirdly, metallurgical research into new and the cast steels then available in England.
improved superplastic alloys is a very wide field and Thereafter Wootz was studied by Michael Faraday
mention will be made of only three developments. among others but the greatest step forward in
One of the problems associated with Supral was the understanding its nature was made by Jean Robert
initiation and growth of voids or holes in the alloy Breant, Inspector of Assays at the Paris Mint who
at the grain-growth inhibiting ZrA13 particles - a in 1824 published a Description for a Process f o r

268
fine (0.5 pm) two-phase structure of iron and
equiaxed cementite grains - not dissimilar to the
fine equiaxed two-phase microstructures character-
istic of superplastic titanium alloys and Pearson’s
tin-bismuth alloy. In this condition the steel
becomes ductile and easily forgeable and on
cooling down to room temperature hard and tough.
There is now little doubt that the ancient
swordsmiths evolved a similar forging technique,
whereby the deformation was governed, as in the
case of modern superplastic alloys, by grain
boundary sliding processes. The cycle from
Saracenic craft to aerospace fabrication is com-
plete!
Figure 9 Superplastically formed and diffusion bonded
engine bay nozzle panel with inset micrograph showing Further reading
diffusion bonded joint (photograph courtesy British
Aerospace) The general problem of the deformation of metals
in terms of the movement of dislocations, diffusion
Making Damasked Steel in which he correctly and grain boundary sliding is covered in many
identified the microstructural constituents. excellent metallurgy textbooks, e.g. Reed-Hill
It is the high carbon content - typically between (1964), Smallman (1970) and Rollason (1973).
1% and 2% (in comparison with the 0.6-0.8% of These books also cover the basic principles of alloy
‘plain carbon’ cutlery steels) -which is the charac- chemistry and the role of precipitates, etc. Of the
teristic feature of Wootz and it is surmised that this many papers concerned with the mechanisms of
was achieved by the prolonged heating of a mixture superplasticity the most useful are those by Ashby
of iron sponge and charcoal at a temperature and Verrall (1973) and Gifkins (1978). It will be
insufficient to cause complete melting but sufficient seen from these papers that the precise mechanisms
to allow a diffusion of the carbon into the iron. In and microstructural conditions for the occurrence
steels at room temperature a very small amount of superplastic flow are by no means fully
(0.01%) of carbon is dissolved in the iron; the understood - there is for example the possibility
resulting solid solution, in which the small carbon that the phenomenon occurs in some large-grained
atoms occupy the holes or interstices between the single phase p titanium alloys given certain
larger iron atoms, is called ferrite. The rest of the dislocation configurations within the grains. These
carbon combines chemically with the iron to form a matters, and the applications of superplasticity in a
compound Fe$ (cementite) or ‘carburetted steel’ wide range of alloys are covered in Paton and
to use Breant’s description. Cementite is hard and Hamilton (1982). Finally, the metallurgy of the
brittle and occurs in Wootz, as well as in modern Damascus steels is discussed in an excellent review
‘ultra-high carbon’ cast steels, as coarse angular by Wadsworth and Sherby (1982). This paper not
needles or platelets throughout the iron matrix only discusses the role of superplasticity in the
making the steel very difficult to forge. At high forging of these steels but also covers tempering
temperatures it crumbles under the hammer and at treatments and the origin of the damask patterns by
low temperatures it splits and cracks along the which Damascus swords are recognised.
cementite platelets. References
The problem that the Damascus swordsmiths had
Ashby M F and Verrall R A 1973 Acta Metallurgica 21
to overcome was to control both the forging 149
temperature and severity of forging in order to Gifkins R C 1978 J. Mater. Sci. 13 1926
break down the angular cementite platelets into Paton N E and Hamilton C H (eds) 1982 Superplastic
equiaxed grains or particles without at the same Forming of Structural Alloys (Metallurgical Society of
time cracking or crumbling the steel. It is the same AIME)
problem which faces the forgers of ultra high Reed-Hill R E 1964 Physical Metallurgy Principles (New
carbon steels today and is overcome not by forging York: Van Nostrand)
the steels at the highest temperatures (as might be Rollason E C 1973 Metallurgy for Engineers (London:
Edward Arnold)
expected) but by forging in a moderately low and
Smallman R E 1970 Modern Physical Metallurgy
moreover narrow temperature range, approximate- (Sevenoaks: Butterworth)
ly 800-900 “C. Furthermore the forging strain rate Wadsworth J and Sherby 0 D 1982 ‘On the
needs to be slow and carefully controlled. In this Bulat-Damascus steels revisited’ Prog. Mater. Sci. 25
way it is found that the steel is broken down to a 35

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