Powder Metallurgy

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High Pressure Triaxial Cell for Metal Powder

P. Doremus, C. Geindreau, A. Martin, L. Debove, R. Lecot & M. Dao

To cite this article: P. Doremus, C. Geindreau, A. Martin, L. Debove, R. Lecot & M. Dao (1995)
High Pressure Triaxial Cell for Metal Powder, Powder Metallurgy, 38:4, 284-287, DOI: 10.1179/
pom.1995.38.4.284

To link to this article: http://dx.doi.org/10.1179/pom.1995.38.4.284

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 High pressure triaxial cell for metal powder
P. Doremus, C. Geindreau, A. Martin, L. Debove, R. Lecot, and M. Dao
A triaxial press was developed to study the mechan-
ical behaviour of metal powders. This press is numeri-
cally controlled and it allows different load paths with
stress and/or strain control: isotropic, conventional
triaxial tests, and loading-unloading cyclic tests. The
confining pressure limit is equivalent to a specimen
radial stress of 400 MN m - 2 whereas the maximum
axial stress is 1250 MN m - 2. Experiments on an iron
powder showed that there was reproducibility of the
results and only a small error in measurement. With
respect to the mechanical behaviour of this powder,
the important influence of deviatoric stress on the
densification was observed, but no dilatancy effects
Downloaded by [UNSW Library] at 04:54 28 April 2016
were observed. PM/0682
© 1995 The Institute of Materials. Manuscript received
2 February 1995. Dr Doremus, Mr Geindreau, Mr Martin,
and Mr Debove are in the Laboratoire Sols, Solides,
Structures, Grenoble, France, Mr Lecot is at the Pechiney
Centre de Recherches de Voreppe, Voreppe, France and
Mr Dao is with Metro Mesures, Clamart, France.
INTRODUCTION
Die compaction followed by sintering is the most commonly
used process to manufacture components from metal
powders. The sizing of tools remains an important problem
of powder metallurgy. Numerical modelling of the process
should permit an optimisation of the industrial compaction
process. Modelling requires a perfect knowledge of t~e
mechanical behaviour of the powder and adequate constI-
tutive laws. Rheological experiments are then necessary to
identify the parameters of these constitutive laws. For this
reason an installation has been developed to carry out tests
with various loading paths such as isostatic and conven-
tional triaxial compaction. In these tests a confining fluid
pressure acts on a cylindrical specimen and an axial force
is superimposed on the flat end faces. This unit allows the
continuous control of the density of the specimen during
loading and the application of confining pressures up to
400 MPa.
Similar experimental set ups which can apply lower
pressures (350 MPa) and which use other technologies have
previously been described.1-7 The principal difference
between these examples of triaxial apparatus is the
measurement of the volumetric strain of the specimen from
which the density is deduced. Two methods have been used
to obtain this value. The first is based on the determination
of the height H and the diameter D of the specimen during
the test. The H value is commonly given by an external
transducer and D is obtained by local measurement with
an internal transducer using strain gauges.2,s Generally, the
volume V is deduced from Hand D assuming that the
specimen remains cylindrical. The second method consists
of a global measurement of the volume variation of the
specimen. Measurement of the air expelled from the
specimen3,4,7 or of the variation in volume of the con-
fining fluid in the cell1,6 have been also proposed. The last
method is the one used in the triaxial set up presented
here. The first part of the present work describes the
284 Powder Metallurgy 1995 Vol. 38 No.4
capabilities of this apparatus. The second presents the
experimental procedure and the first results obtained on
an iron powder.
DESCRIPTION OF TRIAXIAL APPARATUS
General description
The arrangement of the triaxial apparatus is described
in two stages. First, generalities on the triaxial testing
equipment are presented and, second, more technical details
about the triaxial cell are given.
General description of the triaxial apparatus
The triaxial cell is placed under a 400 kN vertical press
activated by a hydraulic jack (Fig. 1). The loading piston
of the press which can be displacement or force controlled
permits axial deformation of the specimen at a maximum
speed of 10 mm S-l and 5 kN S-l respectively. The connec-
tion between the upper punch of the cell and the piston of
the press is achieved through a spherical bushing to avoid
the transmission of moments to the specimen.
A strain gauge type force transducer (range 0-400 kN,
precision ± 0·4 kN) is fixed to the loading piston of the
press. It allows measurement of the axial force transmitted
to the upper punch of the cell which is 20 mm in diameter.
Thus, the maximum axial stress (Jz is about 1250 MN m -2,
the transducer permits force control if necessary. An optical
sensor which is placed between the upper punch and body
of the cell controls the displacement of the press piston
from which the axial strain of the specimen is deduced.
This sensor is extremely accurate (± 2 Jlm) and, because of
its position, is not affected by the elasticity of the press and
the spherical bushing.
The pressure in the cell is achieved by oil, compressed
by a pressure intensifier (Fig. 1). The oil used is synthetic
oil Fina Eolan SPO 46 with a viscosity about 35·7 mPa s
at 40°C. The pressure intensifier, which is composed of two
interdependent pistons with a surface ratio of 20, allows
the compression of the oil in the cell to reach a pressure of
400 MPa. This pressure is measured by a strain gauge type
high pressure transducer (range 0-400 MPa, precision
±0·5 MPa).
The position of the piston of the intensifier is measured
by a LVDT (range 0-150 mm, precision ±0·02 mm). The.
variation in volume of oil in the cell, and thus the variation
in volume of the specimen, is deduced from this measure-
ment. The range of this transducer allows a variation in
volume of up to 40 cm3 to be measured to an accuracy of
+0·006 cm3• These last two transducers permit pressure
~ntrolled tests (isotropic and conventional triaxial tests)
to be carried out by continuously measuring the variation
in volume of the specimen.
Technical details of triaxial cell
The triaxial cell (Fig. 2) is composed of a thick walled
cylinder (2), two caps (4, 11) and two punches (1, 10). The
cylinder is made of 35NCD16 steel with a yield strength of
about 1100 MN m-2• The dimensions are length 280 mm,
inner diameter 45 mm and outer diameter 160 mm. The
caps are made of 40CDV20 steel with a yield stress of
 Doremus et al. High pressure triaxial cell for metal powder 285

Oil20MPa
•.• from hydraulic group
Vertical press

Loading piston 400 kN

Force transducer
Optic
sensor Spherical bushing
Upper punch

~
Oil 400MPa
Pressure intensifier

~
O'r max
--.
= 400 MN m-2
Hornax=45mm

D
Oil20MPa
L.V.D.T
from hydraulic
group
.J

1 Schematic diagram of triaxial apparatus

1200 MN m-2• The specimen is placed between the upper

and lower punches constructed from NC40SW steel with a 3 Initial geometry of specimen and maximum triaxial
yield strength of 1700 MN m - 2. Two pieces of beryllium stress applied
bronze (3, 8) permit movement of the punches and mini-
mise the frictional force between the punches and the caps
by acting as bearing bushes. Static and dynamic tightness closed at both ends by the upper and the lower punches of
the cell. This bag prevents the penetration of oil into the
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is achieved through nitrile 0 rings (5) associated with

polyacetal backup rings. test specimen, so it has a low initial density. The ends of
the punches are greased to minimise the friction between
the specimen and the punches during the test.
EXPERIMENTAL RESULTS The initial diameter Do of the specimen was about
Powder material 20 mm. Preliminary isotropic and triaxial tests carried
An iron based powder (950/0 by weight) was studied. Its out on specimens with an initial height Ho of 42 mm and
composition included copper, wax, and zinc stearate, these 24 mm did not show important differences between
last two components being admixed as internal lubricants. measurements. The results presented were obtained with
The density of the solid phase was about 7·54 Mg m -3 and specimens with an initial height to diameter ratio HolDo
the tap density powder was about 3·67 Mg m -3. The of 2·1.
particles had an irregular shape and their size was between
10 and 100 Jlm.
Isotropic tests
During isotropic testing, the pressure p was increased by
Preparation of specimens 2·5 MPa s -1 until a pressure between 50 MPa and 400 MPa
The specimens were made in a cylindrical mould (Fig. 3), was obtained: this was maintained for 3 min. The axial and
The powder was poured into a latex bag which was then radial stress are both equal to the pressure p in the cell. At
present the uncertainty in the continuous measurement of
the density Pi during the isotropic phase is poor (~80/0)
and it was not possible to obtain accurate density-pressure
curves. Thus, it was decided to perform interrupted tests at
different pressures and to measure the density of the
specimens after unloading. This density has been determined
by pycnometry with an uncertainty of less than 0·10/0.
Continuous measurement during isotropic tests will be
upper punch (l) improved in future tests by measuring the diameter of the
specimen with a transducer inside the cell.
pressure vessel (2)
upper cycling ring (3)
top cap (4)
8----------------------.,
O-ring (5)

7
• • •
• •
M
oil400Mpa I
E
specimen (6)
latex bag (7) ~6
• •
(8) } lowe~ guiding ~~
(9) nng
lower punch (10) 005
z
•
w
0
O-ring (5) 4
II
bottom cap (11)
3
a 100 200 300 400
HYDROSTATIC PRESSURE, MPa

2 Details of triaxial cell 4 Density during isostatic compaction

Powder Metallurgy 1995 Vol. 38 No.4

 286 Doremus et al. High pressure triaxial cell for metal powder

900
(a)
N 800
I

E 700
z
~ 600
en
(/)
500
w
~ 400
~ 300
~ 200
<! 100

5 Comparison between (left) isostatically compressed and o

(right) triaxially tested specimens: actual size o 0.3 0.4
0.1 0.2 0.5
8
(b) 2
Figure 4 presents the evolution of the density measured
after unloading versus the hydrostatic pressure p. This 7.5
('t)

evolution is characteristic of metal powders. Densification I

E 7
of the iron powder is rapid for pressures < 250 MPa and C)
the rate decreases at higher pressures. The density measured ~
by this method is taken as a reference for triaxial tests at 6.5
the same confining pressure.
~
(j)
z 6
w
0
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Triaxial tests 5.5

During triaxial testing, the pressure in the cell was first
increased in the same way as in the isotropic tests. When 5
the required pressure was reached, the height, the volume
and the unloading density of the specimen were respectively
0 0.1 0.2 0.3 0.4 0.5
AXIAL STRAIN
Hi, J'i and Pi. The specimen was then compressed at a rate
of 0·1 mm s -1 while the radial stress was kept constant. a 1: 400; 2: 320; 3: 250; 4: 150; 5: 50; b 1: 400; 2: 320; 3: 250;
During axial loading, the height H and the volume V of 4: 150; 5: 50
the specimen are given by the optical transducer and the 7 Axial stress and density versus axial strain in triaxial
LVDT respectively, after removing the elastic deformation tests at given confining pressure, MPa
of the punches. The density P is deduced from V and the

diameter D is calculated from H and ~ assuming that the

700 specimen remains cylindrical. Figure 5 shows examples of
(a) specimens after isostatic compression and triaxial testing
N
I 600 and justifies the hypothesis. The variables D and P can be
E expressed as follows
~ 500 D = 4V/nH (1)
en
~ 400 P = Pi + bp (2)

.-
0:
(/)
...J
300
where bp is the increase of density during the triaxial phase .
Using experimental data it is possible to calculate the
<! following strains:
X
<! 200
volumetric strain Gy = In(V /J'i) (3)
100 axial strain Gz = In (H/HJ (4)
0 0.1 0.2 0.3 0.4
radial strain Gr = (Gy - Gz)/2 (5)
7.5
(b) The radial stress is given directly by the high pressure
transducer. Measurement of the axial force permits the
('t)

I
axial stress to be calculated. In this case, it is necessary to
E 7 eliminate the force due to the friction between the upper
C) punch and the 0 ring of the cell. Calibrations without
~ powder specimens in the mould showed that this force is
~ constant during the movement of the upper punch and
(j)
depends mainly on the pressure in the cell. Thus, the
z 6.5
w frictional force is easily obtained for each test from the
o
difference between the axial force applied on the upper
punch before its movement and during its movement as
long as the lower punch did not touch the bottom of the
6
cell. Therefore, the different stresses can be expressed as
o 0.1 0.2 0.3 0.4
AXIAL STRAIN radial stress (Jr = (J(J = p (6)

a axial stress v. axial strain; b density v. axial strain axial stress (Jz = 4F/nD (7)

6 Reproducibility of triaxial tests: for three tests in each where F is the axial force superimposed on the flat end
case; confining pressure p = 150 MPa faces of the specimen.

Powder Metallurgy 1995 Vol. 38 No.4

 Doremus et aI. High pressure triaxial cell for metal powder 287

8 600

I' 500
('I)
7 E
I
E ~ 400
0)6 vi
~ ~ 300
a:
~5
en
~
z ~ 200
w «
°4 ~ 100

3
o
o 100 200 300 400 500 600
a 0.05 0.1 0.15 0.2 0.25 0.3
AXIAL STRAIN
P, MPa
1: E = 61600 MN m-z, p = 6·75 Mg m-3; 2: E = 91400
-- triaxial tests; ~ isostatic tests
MNm-z, p=7'08Mgm-3; 3: E=117500MNm-z, p=
8 Density v. mean stress P: effect of deviatoric stress on 7·25 Mg m-3
densification 9 Loading-unloading cyclic test at confining pressure
of200MPa
The relationships between axial stress and axial strain
and between density and axial strain for three tests carried the axial stress versus the axial strain for a cyclic test
out at the same confining pressure (p = 150 MPa) are performed at a confining pressure of 200 MPa. Young's
Downloaded by [UNSW Library] at 04:54 28 April 2016

presented (Fig. 6). The comparison between the diameter,
height, and density of the specimen directly measured after
unloading and the same characteristics obtained from the
different transducers shows that the measurements obtained
by the triaxial apparatus are accurate. The uncertainty
levels are: 1% for the axial strain, 10;6 for the density, 40/0
for the axial stress and 0·5 % for the radial stress. The
results show good reproducibility. The difference between
the sets of results is not greater than 4% for the axial stress
and 1% for the density. These values lie between the
regions of uncertainty defined earlier.
The results obtained at the different confining pressures
are presented in Figs. 7 and 8. For pressures higher than
250 MPa, the axial stress seems to stabilise as the axial
strain of the specimen increases (Fig.7a) and the density
attains a limit value of about 7·5 Mg m -3 (Fig. 7b). This
value is smaller than the density of the solid phase
(7'54 Mg m -3), perhaps because the initial density before
axial compression is assumed to be the density after
isotropic unloading. Thus, curves obtained do not take
account of elastic deformation of the specimen during
loading. Figure 8 presents the relationship between the
density and the mean stress P for isostatic and triaxial
tests. The mean stress is defined as
(8)
It is possible to observe the important effect of deviatoric
stress on the densification while on the other hand, no
dilatancy effects have been found. For example, the differ-
ence between the density at. equal values of P (= 360 MN
m -2) for an isostatic and a triaxial tested specimen at a
confining pressure of 250 MPa is about 0·4 Mg m-3•
This difference is the result of the deviatoric stress and
represents 10% of the densification.
The triaxial set up also allows loading-unloading cyclic
tests to be carried out. Figure 9 presents the evolution of
modulus E calculated from elastic curves increases as the
density p of the specimen increases, i.e. the elastic mod-
ulus at adensity of 7·25 Mg m -3 is about 117 500 MN m-2
and is twice the value corresponding to a density of
6·75 Mgm-2•
CONCLUSION
A 400 MPa triaxial cell developed to study the mechanical
behaviour of metal powders allows kinematic or dynamic
loading tests to be carried out. Tests on· an iron· powder
gave measurements of good reproducibility. The important
effect of deviatoric strain on the densification of the powder
is observed. However, no dilatancy effects have been found.
Dilatancy is likely to occur for overconsolidated specimens:
namely specimens which have been precompacted at a
pressure higher than the confining pressure of the triaxial
test.
REFERENCES
1. D. BORTZMEYER: PhD thesis, Ecole Nationale Superieure des
Mines de Paris, October 1990.
2. M. HEHENBERGER AND J. E. CRAWFORD: 'IUTAM conference on
deformation and failure of granular materials', 381-390; 1982,
Rotterdam, Balkema.
3. M. KOENER: Powder. Metall. Int., 1971, 3, 186-188.
4. w. c. P. M. MEERMAN AND A. C. KNAAPEN: Powder technology,
1979, 22, 271-278.
5. G. COCCOZ, M. BELLET, L. LECOT, L. ACKERMAN, and
H.-A. HAGGBLAD: Proc. PM 94 Powder Metallurgy World Cong.,
Vol. 1, 709-712; 1994, Les VIis, Les Editions de Physique.
6. A. GURSON and T. McCABE: in 'Advances in powder metallurgy
and particulate materials - 1992', (ed. J. M. Capus and
R. M. German), Vol. 2, 'Compaction and other consolidation
processes', 133-145; 1992, Princeton, NJ, MPIF.
7. A. BROESE VAN GROENOU: Powder. Metall. Int., 1978, 10, 206-
211.

Powder Metallurgy 1995 Vol. 38 No.4