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2D and 3D Characterization of Metal Foams

RESEARCH NEWS
Using X-ray Tomography
By Abdelmajid Elmoutaouakkil, Luc Salvo,* Eric Maire,
and Gilles Peix

The aim of this paper is to present a methodology for 2D and 3D character-


ization of different foams using X-ray microtomography with a resolution
of 30 micrometer. 2D and 3D quantitative image analyses have been
performed to obtain information about the cells. The main parameters of
interest are the cell size, the cell size distribution, morphology of the cells,
connectivity of the cells, and fraction of matter at the edges. We use morphological operations such as
opening granulometry to separate cells when they are not perfectly closed. This characterization was
performed on Alporas, IFAM, and Norsk-Hydro foam.

1. Introduction 0.32 g/cm3 on foams made with process route 2.[7] A very
detailed study that compared different metal foams with
Aluminum closed-cell metal foams can be produced by Alporas and Alcan foams in 2D in orthogonal directions was
several techniques and from different constitutive materials. published:[8] using a fabric ellipse this study clearly showed
There are three main routes: firstly, the powder metallurgy the orientation of the cells in the Alcan foams and the isotro-
route (IFAM, Alulight), which consists of generation of the py in Alporas. Furthermore, different moments of distribu-
foam from a precursor made of aluminum powder and TiH2 tion were measured since no conventional distribution can fit
agent, heated to cause foaming.[1] The second route (Norsk- the data. These results indicate clearly the better uniformity
Hydro, Cymat, Alcan) uses aluminum based composites and of the cell size distribution in Alporas foam. It can be seen
gas introduction to give continuous production of foam.[2]
The third mechanism (Alporas) involves the enrichment of
aluminum with Ca to increase its viscosity and subsequent
mixing with TiH2 in a mould to form large blocks of foams.[3] ±
Another original route was published, which combined the [*] Dr. A. Elmoutaouakkil, Dr. L. Salvo
use of aluminum-based composites and TiH2 (oxidized) and GPM2, ENSPG, Domaine Universitaire
which can produce very nice microstructures.[4] There is a B.P. 46, F-38402 Saint Martin d'H›res Cedex (France)
wide dispersion in mechanical properties (Young's modulus, E-mail: elmou@esrf.fr
peak strength, absorbed energy) between these foams. There Dr. E. Maire
are a lot of reasons for such dispersion and one of them can GEMPPM, INSA de Lyon
be found in the microstructural differences between these 20 Av. A. Einstein, F-69621 Villeurbanne cedex (France)
foams. A foam can be characterized on various scales: the mi- Dr. G. Peix
croscopic scale, which mainly deals with cell walls, and the CNDRI, INSA de Lyon
mesoscopic scale, which mainly deals with the pore size. 20 Av. A. Einstein, F-69621 Villeurbanne cedex (France)
A 2D study that compared the mean pore size and wall [**] The authors thank J. Banhart, P. Asholt, and M. F. Ashby for
thickness between these foams emphasizing the differences supplying materials. They thank the French Ministry of Indus-
between them has been published.[5] More recent work was try for the post-doctoral grant given to one of them. Finally,
carried out to determine u, a parameter that comes into the authors thank the team of the ID19 line at ESRF, J. Baru-
mechanical formulation,[6] where 1-u is the fraction of solid chel, P. Cloetens, E. Boller, F. Peyrin for all the work they have
that is contained in the cell faces. A value of 0.7 was mea- done to allow tomography images of such quality and volume
sured for a density of 0.15 g/cm3 and 0.85 for a density reconstruction.

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Elmoutaouakkil et al./2D and 3D Characterization of Metal Foams Using X-ray Tomography

that the characterization of microstructure so far has dealt sample and without X-rays have been obtained in order to
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mainly with the foams processed by route 2 and 3. Simancik increase the quality of the images during back filtering recon-
et al.[9] have characterized foams produced by the powder struction. The energy was set to 25 keV. A complete scan lasts
route under specific conditions in order to study the influence approximately 15 minutes and two scans on each sample
of processing parameters on cells characteristics. A 2D char- were performed since the X-ray beam is limited to 14 mm in
acterization of the cell walls has been performed on Alporas height. One complete volume is approximately 200 Megabyte
and Alcan foam[8] indicating that the mean cell walls thick- using gray scale tones between 0 and 255.
ness range between 40 lm to 160 lm depending on the den- 2D image analyses were performed using IMAGE PRO
sity: the higher the density the thicker the cell walls. At PLUS software. Three slices of each volume have been stud-
microscopic scale the microstructure of the cell walls have ied which means that a quantitative analysis was performed
been studied by Simone et al.[8] and their influence on me- on at least 500 cells. The main parameters that we investi-
chanical properties has been described by Benaouli et al.[10] gated were:
On the 3D scale, few studies have been performed and almost l Mean cell size and cell size distribution: when the cells
no quantitative analyses have been done. Qualitative studies are not closed than we closed them using morphological
have been performed on IFAM and Norsk-Hydro foams,[11,12] filters (watershed) or by using a manual process. We also
generally to characterize defects and look at deformation performed 2D granulometry on the IFAM sample. 2D
mechanisms[11,12] but this was done at a resolution of 150 lm granulometry is made by sequential closing using a
or 230 lm, and no quantitative measurements have been per- square structural element leading to an area frequency
formed. X-ray experiments have been performed on Alulight distribution.[15] This morphological operation is very use-
foams and they clearly show the presence of cracks in the cell ful when cell walls are fractured and gives a good approx-
walls. Furthermore, these data have been used to describe the imation of cell size distribution when cells are equiaxed.
foam at a mesoscale by determining the local density varia- l u estimation: this parameter was determined using mor-
tion.[13] Finally, Helfen et al.[14] studied the early stage of phological operations on segmented images: we use a 3”3
foaming formation with X-ray tomography on IFAM. It is our filter and 3 to 5 openings were performed in order to elim-
aim to present a methodology for 2D and 3D characterization inate cell walls. u was defined as the fraction of matter in
of foams, which have been processed by the three main this latter image divided by the fraction of matter in the
routes presented above. initial image. This parameter gives the fraction of solid in
the edges.
l Connectivity between pores: this parameter is defined as
C = 1-Ncc/Nic where Nic is the number of cells measured in
2. Experimental Procedure the initial image and Ncc is the number of cells when all
the cells are closed. The connectivity is 0 when all the cells
Three foams have been investigated corresponding to the
are separated and 1 when all the cells are connected. The
three routes described in the introduction: one from Alporas,
cells have been closed using a watershed filter or manu-
one from IFAM, and the last from Norsk-Hydro. The foams
ally, which leads to two values of connectivity Cw and Cm
were cut into small cubes 21”21”24 mm3. We used X-ray
respectively
microtomography at the European Synchrotron Radiation
The 3D volumes investigated in this study were
Facility (ESRF), Grenoble, to obtain volumetric information
21”21”14 mm3. Two volumes have been used for each of the
on the microstructure. The advantage of the ESRF is that we
samples and as in 2D size information has been measured on
can work with a monochromatic beam with high photon flux
cells that do not touch the border of the volume. We devel-
and therefore obtain very good quality images for 3D and 2D
oped our own 3D image analysis. Segmentation was per-
characterization. Indeed we perform 2D characterization on
formed using a simple threshold. Sometimes the threshold
slices obtained from the 3D volume. X-ray tomography at
was increased in order to avoid non-real connection between
the ESRF can be performed at various resolutions (from 1 to
cells. The parameters that we studied were:
40 micrometer). We chose an intermediate resolution of 30
l Number of cells: this gives information on connectivity
micrometer in order to resolve all the cell walls and to have
l Surface S and volume V of each cell determined using
enough cells for image analysis. Figure 1 presents the experi-
marching cube algorithms, which gives a better estimate
mental set-up for X-ray tomography. 900 projections have
of these quantities.[16] When cells are not closed we used
been taken within 180 and reference images without the
3D granulometry inpa
volume
 of 18”18”9 mm3.
3
l Sphericity SP = 6V p=S : this parameter is 1 for a sphere
z and less for every other shape.
CCD Camera l u estimation: as in 2D closing was performed in 3D to
X rays
25 keV Foam
30µm eliminate the cell walls and thus obtain an estimate of this
parameter.
l Morphological factor F: for each cell the 3D inertia matrix
Fig. 1. Experimental set up at ESRF. is determined, the eigen values are obtained and identi-

804 ADVANCED ENGINEERING MATERIALS 2002, 4, No. 10


Elmoutaouakkil et al./2D and 3D Characterization of Metal Foams Using X-ray Tomography

fied to the inertia matrix of a 3D box. We extract the larg- Table 1. 2D microstructural parameters (mean value (standard deviation)), where C is

RESEARCH NEWS
the connectivity between pores parameter and u is the fraction of solid in the edges.
est and minimum value of this box and defined F by their
ratio. The larger this ratio the more elongated the cell. The
IFAM Alporas Norsk-Hydro
mean value Fmean and maximum value Fmax are given.
r [g/cm3] = 0.37 (0.05) r [g/cm3] = 0.37 (0.04) r [g/cm3] = 0.35 (0.01)
Cw = 0.47 (0.04) Cw = 0 Cw = 0
3. 2D Quantitative Analysis Cm = 0.4 (0.04) Cm = 0 Cm = 0
u = 0.63 (0.07) u = 0.72 (0.06) u = 0.56 (0.01)
Figure 2 presents three slices (perpendicular to z-axis of
Fig. 1) extracted from the volume of the three foams studied.
The IFAM foam presents very fine structure and clearly some 0.4
cell walls are fractured. Some large cells also appear in the Alporas
0.35
structure. The curvature of the cell walls does not seem to be Norskhydro
Norsk-Hydro
very pronounced in this foam. Alporas foam presents a more 0.3 IFAM (cells closed)

Frequency (area)
regular structure and in this case cell wall curvature is higher 0.25 IFAM (granu 2D)
than in the IFAM foam. Norsk-Hydro foam also presents a typ-
0.2
ical microstructure, which consists of few large cells and many
small ones. The curvature of the cell wall seems to be higher 0.15
than in the Alporas foam. Table 1 presents the connectivity 0.1
and u estimate. Concerning the connectivity it has to be noticed
0.05
that only IFAM foam presents fractured walls and this leads to
high connectivity parameter. It seems that the automatic 0
watershed technique slightly over-estimates the connectivity:

13

20

27

33

40

47

53

60

67
1

7
the reason is that this automatic procedure sometimes consid- Area (mm2)
ers one cell as split into two. The u value of Alporas foam is Fig. 3. Cells area distribution in 2D for the different foams.
slightly larger in comparison with the two other foams.
Figure 3 presents the cells area distribution for the three
foams. In the case of IFAM foam the cells have been closed
4. 3D Quantitative Analysis
and we also plot the result obtained with 2D granulometry. It
is interesting that 2D granulometry and conventional analysis Figure 4 presents the 3D rendering of the X-ray tomogra-
give the same trend: a large peak for 7 mm2 area and a small- phy results for the three foams investigated in this study: the
er one at a larger cell size (15 mm2 when cells are closed and pixel size is 30 lm. Cuts in the volume have been done in
20 mm2 for 2D granulometry). This indicates that 2D granulo- order to better visualize the 3D features of the foams. This
metry is a good way to characterize foams when cells are not visualization allows us to look in depth into the foams and as
completely closed. The histogram of the Norsk-Hydro foam it can be seen on the Norsk-Hydro foam a large cell is present
investigated in this study shows a bimodal-like distribution in the sample. Another interesting feature is to look at serial
with a first peak around 10 mm2 and a second one around sections in the sample. This reveals that the pores observed in
70 mm2. The Alporas foam seems to be more homogenous in the Alporas foam (Fig. 2) are not large pores cut by the 2D
cell size (17 mm2), even if small pores appear in between section. As observed by Degisher et al.[13] the cell walls in the
large cells (Fig. 2). IFAM foam often seem to be ruptured. The qualitative 3D

a) b) c)

5mm 5mm 5mm


Fig. 2. a±c) 3 slices (perpendicular to z-axis of Fig. 1) extracted from the volume of the 3 foams studied. a) IFAM, b) Alporas, c) Norsk Hydro.

ADVANCED ENGINEERING MATERIALS 2002, 4, No. 10 805


Elmoutaouakkil et al./2D and 3D Characterization of Metal Foams Using X-ray Tomography
RESEARCH NEWS

Fig. 4. 3D rendering (volume size = 18”18”9 mm3). a) Alporas. b) IFAM. c) Norsk-Hydro.

Table 2. Quantitative analysis of the three foams: where C is the connectivity between tive measurements of the connectivity. What should be kept
pores parameter, F is the morphological factor, SP the cells sphericity and u is the frac-
tion solid in the edges.
in mind from these results is that IFAM foam presents a high
level of ruptured walls, which is not the case for the two other
foams.
IFAM Alporas Norsk-Hydro
C~1 C~0 C~0
Fmean and Fmax not measured Fmean = 1.6 Fmax = 2.3 Fmean = 1.7 Fmax = 5.3
4.2. Sphericity
SP not measured SP = 0.8 (0.1) SP = 0.86 (0.07)
u = 0.57 (0.05) u = 0.7 (0.05) u = 0.6 (0.02)
Values of sphericity lower than 1 are obtained for the
Norsk-Hydro and Alporas foams. This indicates that the cells
are not far from spherical shape and no real difference can be
visualization shows its limits and therefore we perform 3D
detected between these two foams. No measurement was
quantitative analysis.
possible for IFAM foam owing to the rupture of the walls.
Table 2 presents the main parameters investigated in this
The sphericity gives general information of shape but is not
study. Quantitative analysis is made after segmentation of
enough to characterize a cell. For this we need information on
the volume in gray level to obtain binary volume (cells in
morphology.
black and walls in white). This operation is not always easy
and we had to perform two kinds of segmentation: the first to
measure the connectivity and the second one to close cells in 4.3. Morphological Factor
order to obtain information about the cells. The first segmen-
tation has been chosen taking care not to close cells that are The morphological factor has not been determined for
not closed and also making sure not to create ªartificial rup- IFAM foams since cells are connected and it was not possible
turesº. The second segmentation has been done to close as to close them properly in 3D. However, this morphological
many cells as possible but without loosing small cells. There- parameter was measured on the two other foams and it
fore, absolute values may change with these segmentations shows that the cells are elongated (Fmean > 1) and that Norsk-
but we think that the results are relevant as we compare the Hydro foam can present highly elongated cells (Fmax = 5.3),
various foams. which is less the case for Alporas foam (Fmax = 2.3).

4.1. Connectivity 4.4. Cell Size Distribution

The connectivity parameter C of IFAM foam has been In order to compare the three foams we chose to use the
found to be 1 since, within the volume analyzed, the counting granulometry method, presented in 2D, and extended here in
procedure detected only one object: this means that all the 3D. This allows us to obtain the cell size distribution of the
cells are connected in 3D. It has to be noticed here that it was IFAM foam and compare it to the other two foams. This anal-
not possible to draw such conclusion with the 2D analysis ysis can be compared to the classical one (measurement of
since the connectivity parameter was found to be lower than volumes) when cells are closed (case of Alporas and Norsk-
0.5. In the case of Alporas and Norsk-Hydro, no connected Hydro). We found that this comparison is as good as the one
cells were found in the 2D analysis. As mentioned earlier, the we made in 2D for IFAM in Figure 3. Figure 5 presents the
segmentation procedure is very important to obtain quantita- results obtained by the 3D granulometry.

806 ADVANCED ENGINEERING MATERIALS 2002, 4, No. 10


Elmoutaouakkil et al./2D and 3D Characterization of Metal Foams Using X-ray Tomography

in Norsk-Hydro and Alporas foam nearly all the cells have

RESEARCH NEWS
0.09
Alporas
been found to be closed. X-ray tomography analysis at 30 mi-
0.08
crometer pixel size allowed us to investigate in a non-destruc-
0.07 IFAM tive manner the microstructure of foam (cells and walls). In
frequency (volume)

0.06 Norskhydro
Norsk-Hydro this study, we have presented results concerning the entire
cells and future work will be done on cell walls. Furthermore,
0.05
we shall perform in-situ compression of these foams and
0.04 results are under analysis.
0.03
0.02
0.01 ±
0 [1] J. Baumeister, J. Banhart, M. Weber, Powder Met. Interna-
0.0 50.0 100.0 150.0 200.0 tional 1993, 25, 182.
cells volume (mm3) [2] P. Asholt, Metal Foams and Porous Metal Structures (Eds:
Fig. 5. Cell volume distribution obtained from 3D granulometry. J. Banhart, M. F. Ashby, N. A. Fleck) Verlag MIT Pub-
lishing, Bremen 1999, p. 133.
[3] T. Miyoshi, M. Itoh , S. Akiyama, A. Kitahara, Metal
Norsk-Hydro presents a bimodal distribution centered on
Foames and Porous Metal Structures 1999, p. 125.
20 mm3 for the first peak and 125 mm3 for the second one.
[4] V. Gergely, B. Clyne, Adv. Eng. Mater. 2000, 2, 175.
However, it must be noticed that the volume frequency ob-
[5] Y. Sugimura, J. Meyer, Y. He, H. Bart-Smith, J. Gre-
tained for the larger ones is small, which indicates that the
nested, A. G. Evans, Acta Mater. 1997, 45, 5245.
number of large cells is small as it can be seen in Figure 4. To
[6] L. Gibson, M. Ashby, Cellular Solids, Cambridge Univer-
a lesser extent the same conclusion can be drawn for IFAM
sity Press, Cambridge 1997.
foams: a first sharp peak at very low volumes (around
[7] M. Valente, M. Parisi, F. Nanni, Adv. Eng. Mater., 2000,
2 mm3) and a less important second peak at 50 mm3 are
2, 748.
found. It seems that only the Alporas foam presents mono-
[8] A. E. Simone, L. J. Gibson, Acta Mater. 1998, 46, 3109.
modal distribution (the last peak around 180 mm3 does not
[9] F. Simancik, N. Minarikova, S. Culak, J. Kovacik, Metal
seem to be relevant). What is interesting to note is that
Foams and Porous Metal Structures (Eds: J. Banhart, M. F.
Table 2 shows the same trend as Figure 3, which means that
Ashby, N. A. Fleck), Verlag MIT Pub., Bremen 1999,
in this case a 2D analysis captures the cell size distribution.
p. 105.
[10] A. E. Markaki, T. W. Clyne, Acta Mater. 2001, 49,
p. 1677.
5. Conclusion and Future Efforts
[11] A. H. Benaouli, L. Froyen, M. Wevers, X-ray Tomography
We performed 2D and 3D quantitative analysis on three in Material Science, Hermes Science 2000, p. 139.
different foams. These foams have been scanned at a resolu- [12] E. Maire, F. Wattebled, J. Y. Buffiere, G. Peix. Proc of the
tion of 30 lm at the ESRF in order to retrieve the volume: 2D Euromat 99, (Eds: Clyne, Simancik), vol. 5, Wiley-VCH
analysis has then been carried out on 2D slices from the vol- 1999, pp. 68±73.
ume obtained by tomography. We focused our interest on cell [13] H. P. Degischer, A. Kottar, Metal Foams and Porous Metal
size distribution, fraction of solid in the edges (u estimation), Structures, (Eds: J. Banhart, M. F. Ashby, N. A. Fleck)
connectivity of the cells and morphology of the cells. We de- Verlag MIT Publishing, Bremen 1999, pp. 213±220.
veloped tools for 3D analysis and when cells are not closed [14] L. Helfen, T. Baumbach, H. Stanzick, J. Banhart, A. El-
we used a special morphological operation (granulometry) to moutaouakkil, P. Cloetens, K. Schladitz, Cellular Metals
retrieve the cell size distribution. We found that IFAM and and Metal Foaming Technology, (Eds: J. Banhart, M. F.
Norsk-Hydro foam present bimodal cell size distributions Ashby, N. A. Fleck) Verlag MIT Publishing, Bremen
(with a low fraction of large cells), whereas Alporas exhibits a 2001, pp. 239±244.
monomodal distribution. It seems that Alporas foam has less [15] J. L. Chermant, M. Coster, PrØcis d'Analyse d'Image, Edi-
aluminum in its cell walls than the two other foams. Norsk- tion du CNRS, 1985.
Hydro foam has more elongated cells than Alporas foam and [16] W. E. Lorensen, H. E. Clyne, Computer Graph. 1992, 21,
finally in the IFAM material all the cells are connected while p. 163.

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ADVANCED ENGINEERING MATERIALS 2002, 4, No. 10 807

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