Ultrafine-grained materials

Why are we concerned about it?

Inspired by Hall-Petch
Why are they appealing?
Dramatically improved and/or different
properties not seen in conventional
materials, for example, increased strength
and fracture toughness.
Ultrafine-grained materials
What do I mean?
Metals with grain size ~10-1000 nm
They are also appealing for processes
like superplastic forming
Inverse Hall-Petch
Ultrafine-grained materials
How does one obtain UFG materials?
Roughly speaking:
Consolidation of powder materials
(Mechanical Alloying)
Vapour deposition
Rapid solidification
Refining of coarse-grained materials
We will be concerned with the second
direction
UFG materials obtained via grain
refining
The standard way:
Severe Plastic Deformations (SPD) of
coarse-grained materials
Now the term SPD covers any large
plastic deformation obtained using
simple shear
Most popular SPD techniques
Equal Channel Angular Pressing
High Pressure Torsion
Standard SPD Techniques
Requirements to achieve UFG
fine grained material must have predominantly high angle
boundaries
structure must be uniform over the sample volume
large plastic strains may not have generated internal
damage or cracks
Equal Channel Angular Pressing
High Pressure Torsion
High Pressure Torsion
gives high quality UFG materials
specimen size: thickness ~10m, diameter ~
5mm, limited industrial use
Equal Channel Angular Pressing
lower quality materials, but still good enough
Discontinuous process difficult for scale-up
specimen size: length ~100mm, diameter
~20mm
Main properties of SPD techniques
21.04.2014 10

d
r n
=
t
c
2
Typical nanostructures of CP Ti (a) and Ti 64 (b).
a)
b)
High pressure torsion method
Material State Grain size,
nm
Strength,
MPa
El.,%
CP Ti initial 1500 450 24
HPT 80 1300 10
Ti-64 initial 1000 900 18
HPT 50 1700 8
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Equal Channel Angular Pressing ( ECAP) method

|
c
ctg
N

=
3
2
350 nm
Material State Grain size,
nm
Strength,MPa El.,
%
CP Ti CG 1500 450 24
ECAP+CR 150 1100 8
Ti-64 CG 1000 900 18
ECAP+
upsetting
400 1400 8
a) b)
Typical nanostructures of CP Ti (a) and Ti 64 (b).
21.04.2014 12
1 st stage ECAP routes

Route A
u u
Route B
C
90
u u
Route B
A
90
u u
Route C

180
u u

A- without rotation;
Bc- clockwise rotation
90;
Ba- counter-clockwise
rotation 90;
C- clockwise rotation
180
Image of the samples C 20-60 x 100-200 mm
21.04.2014 13
Titanium alloys for structural applications
N
Material Mechanical properties
o
-1
, N
f
US, MPa YS,MPa o, % , % MPa
1
Coarse-grained 460 400 27 60 255 4211
2
Nanostructured 820 800 15 60 400 34504
The important requirement for
structural materials is combination of
high strength, ductility and fatigue
properties.
One of the most perspective way
here is the fabrication of
nanostructures in commercial alloys.
fatigue limit (o
-1
) and number of cycles to failure (N
f
) of fasteners
High-strength fasteners
CP Titanium
21.04.2014 14
Nanostructured Titanium for medical
applications
Material Grain
size,m
UTS
,
MPa o
-1
, MPa
nano P
Ti
0.15 10101040 591
CG Ti-64 10 9901000 567
Screw implants for traumatology
Compression- distraction apparatus
Plate implants
Titanium possesses the highest bio-compatibility
Problem: to increase strength and fatigue properties
Way to achieve: nanostructure formation
15
Alternate to ECAP
Introducing continuity in the process
ECAP
Conshearing
process
Continuous
confined
strip
shearing
ECAP-
Conform
16
Other SPD Techniques
Accumulative Roll Bonding Asymmetric Rolling
Repetitive Corrugation and
Straightening
Twist channel
Twist Extrusion (TE)
Twist channel
The main idea of TE:
Equivalent strain e~1
The shape and the dimensions of the work-piece do not change!
Twist channel
The main idea of TE:
Equivalent strain e~2
The main idea of TE:
and so on
Refining is a result of large plastic deformations
Twist extrusion work-piece
Cross-section of a work-
piece can be arbitrary
(which is hard to achieve
in ECAP)
By extruding on a
mandrel, it is possible to
obtain products with inner
channels (which is
impossible in ECAP).
Technological schemes for Twist
Extrusion
Technological implementation of TE is
possible with the use of known metal
forming processes.
Twist Extrusion based on
Hydro-extrusion
Allows one to achieve:
high plasticity
small contact friction
high-speed deformation
(with the strain rate ~10
4
s
-1
)
Main disadvantage:
The necessity to
condense the workpiece.

Twist Extrusion based on hydro-
mechanical extrusion
Advantage: does not have
the problems of hydro-
extrusion-based scheme.
Metal plasticity is also high
(due to the pressure of
surrounding liquid)
However, the value of the
maximum deformation during
one pass is limited by the fact
that the workpiece can be
deformed outside the matrix.

Twist Extrusion based on direct
extrusion with a thick
lubrication layer
Metal plasticity is high.
The value of the maximum
deformation during one pass of
pressing is not limited by the
unstability of the workpiece.
Friction loss is higher than in
other schemes.

Semi-continuous hydrostatic
Twist Extrusion-Drawing
Allows one to obtain
long-length products (e.g.
wire)
Metal plasticity is lower
than in previous schemes
due to stretching strains of
drawing.

P
Relationship between TE and
other SPD processes
TE includes elements ECAP,
HPT and Forging. In the
extreme it is basically reduced
to these processes. For
example, when b/a is large,
then TE is similar to HPT. In
the case when the extrusion
axis is far from the specimen
boundary, then TE
corresponds to ECAP.

Torsion
Equal channel
angular pressing
L/b
0
2 b/a 1
10
Twist extrusion
L
b
a
Axis of twist matrix
+
Torsion Forging
Experimental results for copper
Figure: a specimen in a
twist die
Experimental results for copper (cont.)
The specimen after the TE based
on the direct extrusion with a thick
lubrication layer
Dimensions: 25x15x80mm,
Extrusion speed: V~0.002 m/s,
The pressure during the third
pass: P=600 MPa
The hardness after the first three
passes: (H

)
max
=1150 MPa
Experimental results for copper (cont.)
Figure: the specimen after high-
speed Twist hydro-extrusion.
Dimensions: 13x13x500mm,
Pressure: P=1100 Mpa,
Shot rate: V~100 m/s.
Interesting! Unlike in slow
extrusion, the specimen came out
twisted. This is due to the kinetics
of plastic deformations.