Three-dimensionaI Reconstruction of the Porosity of PeIIets of Iron

Oxide and CoaI Powders by SeriaI Sectioning

ROCHA E.P.
1,a
, CASTRO J.A.
1,b
, FONSECA G.S.
1,c


1
EEMVR- Universidade Federal Fluminense
Av. dos Trabalhadores 420, Vila Santa Ceclia, Volta Redonda RJ BRAZL
a
elisa_procha@yahoo.com.br,
b
adilson@metal.eeimvr.uff.br,
c
glaucio@metal.eeimvr.uff.br

Key words: ultrafine powder, characterization, porosity, tortuosity.

Abstract. The selI-reducing agglomerates produced Irom powders generated within the
electric arc Iurnace and LD converters is oI special interest in process oI recycling due to the
amount oI iron and other metals oI high economical value. However, the reducibility and
inner pore structures play important role on the processing technology oI these materials.
Aiming at investigating the inIluence oI the agglomerate structure, some two-dimensional
metallographic techniques have been used to evaluate the porosity in clusters with inaccurate
results, essentially due its three-dimensional Ieatures. From the processing technological
point oI view, the shape and distribution oI inner porosity oI the powders agglomerates are oI
Iundamental importance due to their eIIects on the reaction rates involving the present phases
taking place into the reduction stage. In this study a 3D serial sectioning imaging
reconstruction is proposed to determine local inner porosities and detailed measurements oI
parameters oI pores connections and tortuosities. The averaged porosities results are
discussed and compared with traditional measurements based on pycnometry method.

3troductio3

In general, the characterization oI materials is perIormed by the metallographic

traditional technique by two-dimensional analysis. However, some microstructural
parameters, such as the geometric distribution oI particles, porosity and pore connectivity
show inaccurate values when characterized by two-dimensional sections |1|. Some
techniques allow the structural three-dimensional visualization, such as X-ray computed
tomography, magnetic resonance imaging and serial sectioning. |2|. The serial sectioning
technique consists oI three-dimensional reconstruction oI the microstructure removing thin
suIaces sections and obtaining consecutive images using the optical microscope |1,2,3|. This
technique includes the sequential steps Iollowing: mechanical or chemical polishing oI the
sample surIace; Vickers microhardness; two-dimensional images acquisition in optical
microscope; images alignment and three-dimensional reconstruction and visualization oI the
2-D plans |4|. For each polishing step, it is removed the same amount oI material, reducing
the indentation area and then, it is perIormed another microhardness |2,3|. In this work the
serial sectioning technique is used and the three-dimensional image reconstruction oI planar
sections oI the selI-reducing pellets oI EAF dust was carried out to analyze the inner structure
oI the pores present in the agglomerate oI selI reducing pellets. The importance oI porosity
within this material on the kinetics reduction can be explained not only by the interIacial
adsorption oI the gaseous reducing agent with the solid metal oxides present in the structure
but mainly due to the heat transIer within the pores coupled with gas Ilows |5|. This work
aims to analyze the internal distribution oI the main present phases in the selI-reducing pellet
and its porosity and quantiIy the parameters that aIIect the reduction kinetics, such as the
tortuosity oI the pores and shape Iactor oI the particles by using the serial sectioning
technique and three-dimensional image reconstruction. The importance oI the parameters
accuracy is to improve a kinetic model Ior the oxides present in the selI-reducing pellet and
determine optimum conditions Ior the Iormation and removal oI undesirable impurities
present such as lead, zinc, cadmium and chromium.

%0ory

The pellet were polished in order to obtain Ilat surIaces Ior optical microscope
analysis with good resolution, Iollowing three superIicial Iields oI the sample were chosen Ior
observation oI the porosity distribution in these areas. The Vickers indentation marks were
made in a Shmadzer model binocular microscope composed by lens 0.65M 40x and Vickers
microhardness. The penetration time was 15 seconds and the hardness required was 0.3 Hv.
AIter make the Iirst indentation, the Iirst image was obtained with the optical microscope
Nikon Eclipse LV150. The sequential images were always obtained aIter the removal oI thin
slices by 4000 grain sandpaper Ior a speciIied and constant time oI 3 minutes and 30 seconds.
This process was accomplished until a considerable reduction in the microhardness diagonal
penetration and then, a new microhardness near oI the last Iield is carried out. From the
diIIerence between mean values oI Vickers diagonals beIore and aIter polishing (D1 D2), it
is possible to calculate the height oI each removed surIace slices, according to Eq. 1.

A =
(1-2)
2tung

2
. (1)

The amount oI material removed aIter each polishing cycle is about 2.06 m. Thirty
2-D plans were aligned and visualized three-dimensionally in a volume oI 182.4 m x 182.4
m x 14.25 m. The 3-D serial section reconstruction microscopy studies were carried out
according to the Iollowing steps: I) sequential two-dimensional images data acquisition oI the
studied Iield, II) alignment oI the digital images; III) rendering and visualization oI porous
structure observed.
The soItware used Ior the three-dimensional reconstruction was the NIH Image J.
Some available plugins were important to distinguish the pixels diIIerences between the
phases in the pellet, with the segmentation oI the images, such as shown in the Fig. 1.

a) Original image b) Pixels selected c) Pores selection

Figure 1. Image segmentation showing the present porous at the surIace pellet.

According to Fig. 2, it is possible to observe that the microhardness (marked by a red

circle) is larger than the pores. This is due to the analyzed material is very soIt which requires
low penetration load.



Figure 2. DiIIerence between the size oI porous and Vickers Microhardness.

The magniIication oI 5X was used to the acquisition oI the digital images to obtain
enough amount oI porous in the same image. AIter the segmentation oI 2-D images, it was
built a stack (stack oI sequential images) and so, to perIorm the alignment oI cells with the
StackReg plugin, developed by Philippe Thevenaz, Irom the Biomedical Imaging Group,
Ecole Polytechnique Federale oI Lausanne |6|. The alignment oI the images allows
recognizing the continuity oI the pore and tortuosity visualization. This alignment can be
visualized in the Fig.3.



Figure 3. Alignment process to carry out the next step, the 3-D image reconstruction.

The images renderization aIter the alignment allows a more 'solid visualization oI
the volume. To perIorm the renderization oI the volume, it was used the plugin Volume
Viewer developed by K. U. Barthel |7|.
It is also possible to control the opacity oI the volume using a tool oI transparency
controller, allowing the visualization oI the structure oI the porous, as can be observed in the
Fig.4 and 5. In these Iigures the white pixels are the porous images selected in the samples.



Figure 4. 3-D image reconstruction oI the microstructure oI the pellet showing the pore
structure. The black color is set to the other phases.



Figure 5. 3-D image reconstruction oI some pores identiIied in the pellet agglomerate.

From the 3D image reconstruction it was observed that the porous do not have a
homogeneous structure with small and larger pores, spherical and shapeless presenting
connectivity oI clusters. It is worthy to mention that to the subsequent metallurgical process
unit the connectivity oI the porous in the selI-reducing pellets plays important role, because
the reducing gas has to be in contact with the oxides in order to get high reaction rates oI
reduction and promoting short residence time which can lead to higher process productivity.
However, these connectivity structure must be strictly controlled to attain suitable mechanical
strength oI the pellet. The tortuosity oI the pore can be obtained using the Eq. 2, where L is
the real size oI the pore and orthogonal length.

t =
L
h
(2)

Table 1 shows diIIerent values oI L and h parameters Ior Iour pores chosen to analyze
the tortuosity.

Table 1. Tortuosity Ior Iour diIIerent pores.

!or0 1 !or0 2 !or0 3 !or0 4
L m] 26.7957 27.3600 15.0594 14.9625
m] 25.1085 27.3600 9.1200 14.8314
x 1.0672 1.0000 1.6512 1.0088

The porosity material was calculated using the average oI the porous Iound in these
areas and so the result was conIronted with the pycnometric method. The porosity obtained
by the technique reconstruction three-dimensional in serial sectioning was perIormed in the
soItware Image J, resulting in a porous Iraction oI 47.5. The pycnometric technique is a
method that compares the relative densities oI the solid and liquid. It is a simple, eIIective,
accurate and cheaper method |8|. This method is based on ASTM B 311-93 standard and it is
valid Ior metallic materials containing less than 2 porosity. As the pellet has porosity
greater than 2, its surIace was surrounded by a thin polymeric Iilm to prevent that the liquid
came in the pores, because iI this happened, the apparent weight obtained would be an
inaccurate value. According the Eq. 3 and 4, it is possible to estimate the density and porosity
oI the pellet, respectively.

I =
u
u-E
. (3)

[^[_ =
pt-pa
pt
(4)

Where,
Pa: weight oI dry sample (kg.m/s2);
Pa
'
: apparent weight oI the sample (kg.m/s2);
pl: liquid density (g/m3);
pt: theoretical density (g/m3) and;
pa: apparent density (g/m3).

The theoretical density oI the sample was calculated with the volume oI the phases in
the pellet using X-ray analysis |9|. The liquid used was water. Table 2 shows the results oI
the theoretical density, apparent density and pore Iraction Ior three pellets analyzed. The
average porosity determined in pycnometry method was compared with the result obtained in
3-D image reconstruction and presented good agreement.

Table 2. Density and porosity oI the pellet calculated Ior picnometry.

$ampl0s
%0or0tical
D03sity g/cm
3
]
Appar03t
D03sity g/cm
3
]
!or0s ]
(pic3om0try)
!0ll0t 1 3.9920 2.2230 44.31
!0ll0t 2 3.9920 2.3151 42.01
!0ll0t 3 3.9920 2.1562 45.98

The area Iraction was evaluated by using the soItware Image J within 5 diIIerent Iields
and the average results oI 44.1 and 47.5, respectively were obtained Ior both techniques. It is
observed a diIIerence oI around 7 oI the values obtained by these methodologies, however
the 3D image reconstruction allows the evaluation oI additional quantities such as shape and
tortuosities oI the pores analyzed. ThereIore the 3D image reconstruction was judged a better
methodology to study the agglomerates structure oI the selI-reducing pellets.

Co3clusio3s

In this work is conIirmed that the 3D image reconstruction by serial sectioning technique is a
suitable methodology to investigate pores structures oI selI-reducing pellets and gives
important additional inIormation regarding to the kinetics parameters oI reactions in the
subsequent process oI reduction and elimination oI impurities. Some diIIiculties were
observed during the metallographic characterization due to the soItness oI the agglomerate
that can cause inaccurate results, however with careIul control in the polishing step this
shortcoming could be avoided and good images were obtained aIter continuous reIinement oI
the data image processing. By observing the Iinal reconstruction images it was observed that
the tortuosities values oI the average Iields were close to unit and the pores are closely to
cylindrical shape with small interconnectivity among them.

Ack3owl0dg0m03ts

The authors thank the Iinancial support oI CNPq, FAPERJ and CAPES.

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