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DOI: 10.1002/adem.201100126MM
UNI
Martensitic Phase Transformation in TRIP-Steel/Mg-PSZHoneycomb Composite Materials on Mechanical Load**
CATIO
By Christian Weigelt,* Christos G. Aneziris, Harry Berek, David Ehinger and Ulrich MartinN
Composite materials have been in focus of scientific studies since decades. Metal-matrix compositeshave received extensive attention in the last years. The combination of a metastable austeniticTRIP-steel with magnesia partially stabilized zirconia is presented in this study. The stress inducedmartensitic phase transformation in both components leads to advantageous mechanical behavior.Raised compression strength as well as increased specific energy absorption on plastic deformationoffers a range of structural and crash-absorption applications. Samples with zirconia additions arereinforced by volume increase during tetragonal-monoclinic phase transformation at compressivestrains below 35%. The microstructure and phase evolution of partially stabilized zirconia as well assteel has been investigated by EBSD with purpose to correlate mechanical properties with phaseevolution.
Composite materials have been in focus of scientific
researches since decades. The advantageous combination of
two or more different materials offers a range of micro- and
macrostructure designs according to their crashworthi-
ness.[1–3] Crashworthiness is concerned with the absorption
of energy through controlled failure mechanisms and modes
that enable a defined load profile during deformation.[4]
Cellular materials, such as metal foams and honeycomb
structures, are materials which stand out for the combination
of physical and mechanical properties, e.g., crash box
applications in automobile and train structures. Specific
energy absorption per unit mass and specific energy
absorption per unit volume are the key features for
crashworthiness, respectively.
[*] C. Weigelt, Prof. C. G. Aneziris, Dr. H. BerekInstitute of Ceramic, Glass and Construction Materials,Technische Universitat Bergakademie Freiberg, Agricolastraße17, 09596 Freiberg, (Germany)E-mail: [email protected]
D. Ehinger, Prof. U. MartinInstitute of Materials Science, Technische UniversitatBergakademie Freiberg, Agricolastraße 17, 09596 Freiberg,(Germany)
[**] This scientific work was supported by the German ResearchFoundation (DFG) in terms of the Collaborative ResearchCentre ‘‘TRIP-Matrix Composites’’ (CRC 799). The authorsalso acknowledge the support of Dr. B. Ullrich withSEM-analysis.
ADVANCED ENGINEERING MATERIALS 2012, 14, No. 1-2 � 2012 WILEY-VCH
Several groups have produced cellular structures by using
hollow spheres made of different steel compositions. These
materials exhibit a plateau stress of 5 and 23MPa with a
specific energy absorption of 2 and 10MJ �m�3, respectively,
up to 50% strain.[5,6] Rabiei and O’Neill[7] presented a new
composite material based on steel hollow spheres packed into
a dense arrangement by filling free space with casting
aluminum. The compressive strength of this material was
given at averaged 67MPa in the region of 10–50% strain with
an energy absorption of 30MJ �m�3 after 50% compressive
strain.
The combination of a ductile metal matrix with brittle
ceramic additions leads to failure tolerant metal-matrix
composites (MMC). TRansformation induced plasticity
(TRIP)-steels offer a matrix material with outstanding strain
associated with slight strain hardening. These properties
originate from a martensitic phase transformation from
austenite to martensite on mechanical load. Similar transfor-
mations can be observed for zirconia (ZrO2) ceramics. ZrO2
appears in three modifications: between melting and 2 370 8Cthe cubic phase (c-ZrO2) is stable. Further cooling leads to
transformation into the tetragonal phase (t-ZrO2) and below
1 170 8C highly distorted monoclinic ZrO2 (m-ZrO2) is
thermodynamically preferred. The phase composition can
be affected by stabilizer additions as well as heat treatment.
Particularly the t$m transformation is of technological
interest. In general this transformation appears with a volume
change of 3–5% exceeding the critical fracture length in
ceramics. Whilst this effect eliminates pure zirconia applica-
tions the transformation can be used for reinforcing a second
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C. Weigelt et al./Martensitic Phase Transformation in TRIP-Steel/Mg-PSZ . . .
Table 1. Chemical composition of TRIP-steel powder AISI 304 in wt%.
Fe Cr Ni Mn Si C
Bal. 18.40 9.30 1.13 0.67 0.01
Table 2. Chemical composition of Mg-PSZ zirconia powder in wt%.
ZrO2 MgO SiO2 HfO2 Al2O3 TiO2
Bal. 3.4 2.4 1.7 0.6 0.1
material. Guo et al.[8] achieved samples with strength of 1400
up to 2 100MPa for dynamic high-rate deformation. They
combined a low-alloyed steel with up to 35 vol% yttria
stabilized zirconia. Recent publications of Aneziris et al. [9,10]
presented cellular composite materials based on TRIP-steel
with magnesia partially stabilized zirconia (Mg-PSZ).
The standard route for the production of cellular
honeycomb specimens is the extrusion of plastic pastes. Since
decades filters and catalyst carriers are produced in close
related geometry. This method offers the ability of homo-
geneous mixtures of steel and ceramic particles in the range of
some mm. To achieve the properties for extrusion usually
organic additions, e.g., plasticizers, are necessary. After
drying and thermal debinding, a sintering step takes place
to achieve the final properties.
Within the present work the extrusion of austenitic
stainless steel matrix composites with Mg-PSZ particles at
room temperature was performed. After sintering the samples
were tested under uniaxial compressive load. The main topic
is the relation between mechanical properties and the
EBSD-observed phase evolution in both components. The
stress-induced martensitic transformation of single partially
stabilized zirconia particles and the identification of the
corresponding state of deformation are in focus. The key to
advantageous mechanical properties of the presented com-
posite material is the ability of both phases for the martensitic
phase transformation due to mechanical stresses. The
amounts of metastable austenite in steel as well as the
metastable tetragonal phase in partially stabilized zirconia
are important. Several interactions during sample production
and heat treatment may influence the phase proportion in
comparison to starting material. But the success of the
presented composite material is related to phase relations.
Experimental
The honeycomb square cell composites have been pro-
duced with the well-established ceramic extrusion technique.
Table 1 presents the chemical composition of the as-received
steel powder typeAISI 304 (German grade X5CrNi 18-10) with
an average particle size of 14mm. The percentage of 92%
Table 3. Composition of mixtures for paste preparation.
Raw materials
Material Type
Austenitic steel 1.4301, d50¼ 14mm Womet, Ger
ZrO2 PMG 3.4, d50¼ 1.3mm Saint-Gobain
Plasticizer flour Coarse grained flour Dresdener M
Plasticizer cellulose Methocel F4M DOW Wolff
Dispersant Castament FS60 Degussa, Ge
Surfactant Denk Mit Henkel, Ger
Sum
Plus additional water
Water Deionized
54 http://www.aem-journal.com � 2012 WILEY-VCH Verlag GmbH & Co.
metastable austenitic phase was calculated based on the
amount of ferrite measured by the aid of X-ray diffraction
(XRD). The ceramic phase consists of magnesia partially
stabilized zirconia (see Table 2) with 3.4wt% MgO (Saint
Gobain, USA) at an average particle size of 1.3mm. Referring
to XRD the starting powder consists of 10% monoclinic, 36%
tetragonal, and 53% cubic phase. The compositions of the
presented samples can be seen in Table 3.
Before extrusion the inorganic powder materials were
mixed within 30min in a tumble drum with yttria stabilized
zirconia balls. In a second step the plasticizers and binders
were added and the material was further mixed in a
conventional mixer (Toni Technik, Germany) for 5min.
Finally, water was added and the recipes were kneaded until
a homogeneous and plastic paste was achieved. Due to a
combined de-airing single screw extruder with vacuum
chamber and sigma kneader type LK III 2A (LINDEN,
Germany) honeycomb structures were extruded with a
square shape of 25� 25mm2 and a honeycomb structure
of 14� 14 channels (200 cpsi-channels per square inch). The
wall thickness differs between 350mm (inner walls) and
400mm (exterior wall). After extrusion the specimens were
dried stepwise at 40–80–110 8C in an air-circulated dryer
within 12 h at each temperature and decreasing humidity
from 80 to 20%. Afterward cubic samples of 25mm length
were cut and placed on alumina tiling. The debinding step
took place at 350 8C for 90min in air atmosphere with a
Recipe [wt%]
Supplier 0Z 5Z 10Z
many 96.72 93.11 89.43
, USA 0.00 3.60 7.29
uhlen, Germany 1.81 1.82 1.81
Cellulosics, Germany 0.94 0.93 0.91
rmany 0.14 0.14 0.16
many 0.39 0.40 0.40
100 100 100
5.91 6.02 5.88
KGaA, Weinheim ADVANCED ENGINEERING MATERIALS 2012, 14, No. 1-2
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Table 4. Lattice parameter used in the EBSD phase analysis.
Phase ICDD no. Crystal system Lattice parameter
a [A] b [A] c [A] a [8] b [8] g [8]
ZrO2 0780047 Monoclinic 5.15 5.20 5.32 90 99.20 90
ZrO2 0140534 Tetragonal 5.09 5.09 5.18 90 90 90
ZrO2 0707304 Tetragonal 3.58 3.58 5.16 90 90 90
ZrO2 0270997 Cubic 5.09 5.09 5.09 90 90 90
Mg0.38 Mn0.62 SiO3 0832282 Trigonal 9.65 10.39 12.11 108.65 102.32 82.95
(Mg,Mn)Al2O4 0011154 Cubic 8.03 8.03 8.03 90 90 90
Austenite fcc 3.66 3.66 3.66 90 90 90
a0-Martensite bcc 2.87 2.87 2.87 90 90 90
Table 5. Density and shrinkage of the sintered honeycomb structures.
0Z 5Z 10Z
Density [g � cm�3] 6.77 6.62 6.61
Open porosity [%] 7.71 9.28 8.80
Linear shrinkage [%] 11.88 12.67 12.70
heating rate of 1 K �min�1. To prevent oxidation effects during
further heat treatment the honeycombswere placedwith stock
in graphite crucibles after debinding. Finally the samples were
sintered pressure less in a 99.999% argon atmosphere using an
electrical furnace typeHT 1600GTVac (LINN, Germany) with
oxidic furnace lining and MoSi2 heating elements. After
heating with 5 K �min�1 the temperature of 1 350 8C was kept
constant for 120min followed by cooling with 10 K �min�1 to
room temperature. Open porosity and bulk density were
determined based on Archimedes principle and DIN EN 1389
with toluol as immersion fluid.
The compressive tests were performed on bilateral
polished samples with a 500 kN servo hydraulic testing
machineMTS 880 (MTS, Germany)with a displacement rate of
0.022mmmin�1 at room temperature. In order to analyze the
Fig. 1. Honeycomb structure based on recipe 5Z as-sintered: (a) profile view, (b) top view.
Fig. 2. SEM image of a typical fracture surface region of 5Z before compression test, (a) magnification 1 000�,(b) magnification 3 000�.
crashworthiness stress–strain-curves were
recorded. To clarify the correlation between
mechanical properties and phase evolution
of metal and ceramic components deforma-
tion tests were stopped after 2, 5, 10, 20, and
30% compressive strain, respectively, on
different samples. Additionally, compression
tests were carried out up to deformation
degrees of 35 and 50% in order to identify
the material failure and structural damage of
the multi-cell columns. The specific energy
absorption was calculated according to
Equations (1a) and (1b). SEAV is defined as
specific energy absorption per volume (V)
unit, SEAm refers to mass (m) unit, respec-
tively.
SEA ¼ W
Vor SEA ¼ W
m(1a)
where
W ¼ZSb
0
PdS (1b)
W is the total energy absorbed during sample
deformation, P the load, S the displacement,
ADVANCED ENGINEERING MATERIALS 2012, 14, No. 1-2 � 2012 WILEY-VCH Ve
and Sb is the strain at end of experiment according to Jacob
et al. [4].
Microstructure characterization was conducted using
scanning electron microscopy (SEM), energy dispersive
X-ray microanalysis (EDX) as well as electron backscatter
diffraction (EBSD). Mechanically tested as well as non-
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C. Weigelt et al./Martensitic Phase Transformation in TRIP-Steel/Mg-PSZ . . .
Fig. 3. (a) Stress–strain curves of the compositions 0Z, 5Z, and 10Z, (b) Specific energy absorption as a functionof engineering strain applying a quasi-static compressive load in OOP-direction.
Fig. 4. Collapse patterns of the honeycomb specimen reinforced by 10 vol% Mg-PSZ after interruptedcompression at 35% strain: (a) view of the outer skin, (b) view of the longitudinal section.
Table 6. Specific energy absorption after compressive deformation test, average of 5samples.
Recipe Strain SEA
[%] [kJ � kg�1] [MJ �m�3]
0Z 2 0.47� 0.03 1.47� 0.09
5Z 2 0.64� 0.08 2.04� 0.25
10Z 2 0.72� 0.07 2.25� 0.24
0Z 5 1.55� 0.04 4.89� 0.06
5Z 5 2.05� 0.12 6.48� 0.33
10Z 5 2.36� 0.15 7.40� 0.53
0Z 10 4.06� 0.06 12.79� 0.07
5Z 10 5.18� 0.13 16.37� 0.27
10Z 10 5.92� 0.31 18.55� 1.18
0Z 20 11.95� 0.24 37.65� 0.33
5Z 20 14.42� 0.05 45.62� 0.52
10Z 20 16.18� 0.83 50.76� 3.49
0Z 30 23.60� 0.65 74.34� 1.15
5Z 30 26.96� 0.64 85.26� 2.69
10Z 30 28.18� 1.22 87.80� 5.34
0Z 50 49.49� 2.06 157.63� 7.26
5Z 50 53.17� 4.77 169.10� 5.52
10Z 50 46.49� 1.14 145.84� 0.93
Fig. 5. XRD pattern of recipe 10Z after sintering at 1 350 8C for 2 h in argonatmosphere.
deformed specimens were prepared for analysis. Overviews
regarding the EBSD method are given in several contribu-
tions.[11,12] The incident electron beam is inelastically scattered
within the sample. A part of the backscattered electrons can
escape the sample. In their way they are reflected on lattice
planes. The electron backscatter patterns (EBSP) are a result of
interference following Bragg’s role. EBSP contain all informa-
56 http://www.aem-journal.com � 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
tion about the lattice symmetry within the
excited sample volume and thus can be used
for phase analysis. They consist of parallel
lines for each reflecting lattice plane. The
angles between these lines in the so called
Kikuchi pattern or EBSP exactly correspond
to the angles in the lattice structure. The
analysis is realized by comparing the
measured angles with those of candidate
lattice structures. Some knowledge about
possible phases and their lattice structures is
necessary. The decision can be taken on the
base of medium angle differences. There is a
possibility to determine lattice spacing’s too.
But under normal conditions for ceramic
materials the accuracy is not acceptable. The
investigation was carried out in a conven-
tional scanning electron microscope Philips
XL30 equipped with an EBSD system TSL
(Edax/Ametek, Germany). In the case of
ceramic materials a conductive coating is
necessary. One also should keep in mind
that as a result of sample preparation a
disturbed region might occur. These effects
strongly reduce the quality of EBSP.
Phase determination can be carried out
for single spots or for defined scans. There
are two preconditions for a successful EBSD phase mapping.
First of all undisturbed and electrically conducting sample
surfaces are needed. Sample preparation thus is of great
importance especially in the case of multi-crystalline ceramic
materials which contain a high number of cracks. The sample
preparation was realized by vibration polishing in a
BUEHLER VibroMet2. All samples were coated with Pt-layers
in the nm range using a conventional EDWARDS sputter
coater. For each sample ten randomly spread regions with
zirconia agglomerate and surrounding metal phase were
analyzed. The second problem to be solved is a set of lattice
parameters of phases which really are involved in the given
sample. For this purpose an ICDD data base was used.[13] By
ADVANCED ENGINEERING MATERIALS 2012, 14, No. 1-2
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comparing the EBSD results with XRD a set of possible crystal
structures was defined. The results for the given PSZmaterials
and additional major phases for composite material are given
in Table 4. XRD measurements were done using a Philips
diffractometer with Cu Ka radiation scanning 2u angular
region from 5 to 808. Phase identification and quantification
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Fig. 6. Cross-section of zirconia agglomerate in the as sintered state, 5Z. (a) SEI, (b) EDX Zr map, (c) EDX Omap, (d) EDX Mg map, (e) EDX Mn map, (f) EDX Si map, (g) EBSD quality map, (h) EBSD phase mapshowing t/c-ZrO2 (black), and m-ZrO2 (gray).
have been done with aid of X’Pert Highscore
Plus analysis software (Panalytical, Nether-
lands).
Results and Discussion
The determined properties density, open
porosity and shrinkage are listed in Table 5.
The addition ofMg-PSZ powder has negligible
effects on the presented properties showing
differences only in the range of standard
deviation (average of five samples with a
deviation of less than 4%). Thus differences in
mechanical behavior at compressive strength
tests cannot be explained by differences in
porosity, Figure 1 shows a sintered sample of
recipe 5Z before deformation test.
During sintering and densification the
honeycomb sample structure changes from
200 cpsi after drying to �260–280 cpsi with a
cubic structure with length of 22mm in each
dimension. The thickness of inner walls can be
determined to 300mm whereas the exterior
walls Exhibit 350mm. Figure 2 presents the
microstructure of a typical sample fracture
surface of recipe 5Z after sintering. A dense
structure of TRIP-steel matrix with well
dispersed zirconia particles can be seen.
Usually ceramic additions appear as agglom-
erates. According to EDX-analysis three dif-
ferent regions can be identified. On the one
hand the composition of metal phases approx-
imate correlates with starting chemical com-
position of Table 1. On the other hand ceramic
regions with dominating zirconia content can
be observed. Beyond these particles with
elevated concentrations of e.g., manganese,
magnesium, and silicon are detectable.
Various interactions between TRIP-steel and
Mg-PSZ will be discussed later.
The results of the mechanical tests are
presented below. Figure 3 displays the
mechanical responses of the three material
conditions (0Z, 5Z, 10Z) under uniaxial
compressive loading in out-of-plane direction
(OOP, parallel to the extrusion axis denoted by
X3) with respect to the engineering stress
[Figure 3(a)] and the specific energy absorp-
tion per unit mass [Figure 3(b)] as a function of
strain. As has already been mentioned in
ADVANCED ENGINEERING MATERIALS 2012, 14, No. 1-2 � 2012 WILEY-VCH Ve
previous publications[14–16] the stress–strain curves of all
recipes start with a linear-elastic regime. Rising load is
associated with an interval of strain hardening with a
transition to a maximum compression stress peak of about
428� 22MPa. These phenomena are caused by a combined
mechanism of structural collapse and material damage. The
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C. Weigelt et al./Martensitic Phase Transformation in TRIP-Steel/Mg-PSZ . . .
mechanical behavior of the pure metal samples is different
from the zirconia toughened specimens. Increasing additions
of Mg-PSZ lead to enhanced compressive flow stresses related
with lower critical failure strains in contrast to the unrein-
Fig. 7. Cross-section of zirconia agglomerate after 20% compressive strain, 5Z. (a) SEI, (b) EDX Zrmap, (c) EDX O map, (d) EDX Mg map, (e) EDX Mn map, (f) EDX Si map, (g) EBSD quality map,(h) EBSD phase map showing t/c-ZrO2 (black), and m-ZrO2 (gray).
forced TRIP-steel condition. The reasons for these
early failures are the formation of cracks and cell
wall displacements as results of the global column
buckling mode as well as reduced ductility caused
by a lower amount of deformation-induced mar-
tensite in sample volume.[14,16] In Figure 4 the cell
wall buckling dominated by the formation and
cross-shaped arrangement of plastic hinges and the
crack initiation in the outer skin and the honey-
comb core are demonstrated for the specimen
reinforced by 10 vol% zirconia and deformed up to
35% compressive strain. As shown in the diagram
in Figure 3(b), the effect of particulate reinforce-
ment by 5 vol% of Mg-PSZ results in a higher
capacity of absorbed energy up to the applied
deformation degree of 50%. The distinctive failure
behavior of the recipe 10Z involves a decrease
of specific energy absorption above 35% strain.
The values for mass- and volume-specific energy
absorption calculated by Equations (1) and (2) are
presented in Table 6. In comparison to other
cellular crash-absorbing materials[1,17–19] the pre-
sented zirconia toughened TRIP-steel composite
honeycomb structures (recipes 5Z and 10Z) offer
excellent energy dissipation amounting to values
between 53.2 and 46.5 kJ � kg�1 (cf. 169.1 and
145.8MJ �m�3) after 50% compressive deformation.
Knowing the phase composition of the compo-
site material is of great importance for the under-
standing of the mechanical behavior and micro-
structure mechanisms during compressive
deformation tests. XRD are state-of-the-art for
qualitative and quantitative analysis in metal and
ceramic materials. Figure 5 presents a diffraction
pattern of recipe 10Z after sintering 2 h at 1 350 8Cin argon atmosphere. As already known from
literature the quantitative phase analysis in zirco-
nia demands XRD at high angles.[20] The amount of
ceramic phase in the composite material is limited
to 10 vol% regardingmechanical properties. Due to
this restriction of the volume ratio the intensities of
zirconia peaks and subsequently the validity of the
interesting peaks is poor. Hence, changes in phase
composition during compressive deformation tests
are hardly detectable by XRD and the demand of an
advanced phase analysis method becomes clear.
In contrast, EBSD measurements enable phase
identification of small particles and clusters,
respectively.[11] Lumpy sample surface even after
polishing, e.g., pores, as well as inhomogeneity in
crystal structure are restricting factors for analyses.
Grain boundaries and highly distorted crystal
58 http://www.aem-journal.com � 2012 WILEY-VCH Verlag GmbH & Co.
lattice or chemical reactions forming new compounds during
sintering, respectively, limit results. Not only microstructure,
but also mechanical properties are shifted by interactions. As
already known from[21] several interactions between zirconia
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Fig. 9. Volume fraction of fcc-austenite, bcc-martensite, and hdp-martensite afterdifferent compressive deformation rates measured by EBSD, 5Z.
and TRIP-steel occur during temperature treatment. Diffusion
of magnesium and alloying elements results in destabilization
of reinforcing ceramic particles during sintering.
Figure 6 presents the steps of EBSD-phase analysis of
non-deformed recipe 5Z starting with SEM image
[Figure 6(a)], EDX mapping [Figure 6(b–f)], EBSD quality
map [Figure 6(g)] and the resulting EBSD phase map
[Figure 6(h)]. The same procedure after 20% compressive
strain is presented in Figure 7. Both spots show zirconia
agglomerates embedded in TRIP-steel matrix. The EDX maps
Figure 6(b) and 7(b) clarify the edge between metal and
ceramic phase enabling separated phase analysis. In case of
the as-fired specimen the EBSD image quality for zirconia
particles is lower in comparison to steel. After plastic
deformation both phases appear with nearly the same validity
due to distorted crystal lattices. The dominating amount of
non-metastable monoclinic phase after sintering is obviously.
Nevertheless, the m-ZrO2 quantity is increased after com-
pressive deformation.
Figure 8 shows the calculated phase evolution of ceramic
particles in 5Z samples as a function of compressive
deformation. The first transformation in zirconia takes place
during sintering with a significant increase of non-
transformable monoclinic regions to 80.5� 4.5%. In reverse
the amount of metastable tetragonal (16.0� 4.0%) and cubic
(3.8� 1.6%) decreases. To keep in mind the as-delivered
powder possesses an m-ZrO2 quantity of 10%. The quantity
increases during deformation test to values of 90.3� 5.8% after
10% compressive strain. As expected the value of metastable
tetragonal phase decreases to 7.7� 4.7%. This is the result of
the stress induced phase transformation. Further compression
does not influence the phase composition significantly. The
scatter of the values is caused by lattice distortions and due to
the restrictions of a statistic method. The cubic phase is almost
completely destabilized during thermal treatment. Hence, in
the present paper only a negligible change from 3.8� 1.6%
after firing to 1.3� 0.7% after 30% deformation is detectable.
The possibility of phase transformation toughening in zirconia
ceramics is already known.[22] However, the influence of cubic
Fig. 8. Volume fraction of monoclinic, tetragonal and cubic phase in zirconia particlesafter different compressive strain measured by EBSD, 5Z.
ADVANCED ENGINEERING MATERIALS 2012, 14, No. 1-2 � 2012 WILEY-VCH Ve
zirconia for toughening effects during mechanical or thermal
treatment is not yet uniformly clarified.
The small amount of metastable tetragonal phase of the
as-fired specimens results from temperature treatment.
Sintering pure Mg-PSZ in the temperature field of
1 300–1 400 8C leads to a distinct increase of monoclinic phase
due to thermal destabilization.[21] Besides this, in the presence
of manganese, silica and alumina interdiffusion, and chemical
interactions occur. As can be seen in EDXmaps Figure 6 and 7
the concentration of these elements and magnesium, respec-
tively, is increased at grain boundaries. With the aid of EBSD
analysis these regions can be identified as Mg0.38Mn0.62SiO3
and (Mg,Mn)Al2O4. As a consequence themagnesia content in
zirconia lattice is reduced resulting in t!m transformation.
The most limitation factor for continuing advances in
TRIP-steel/Mg-PSZ composite materials can be seen as the
interactions during processing.
Figure 9 presents the corresponding volume fractions in
metal phases during compressive deformation of samples 5Z.
As expected the quantity of austenite (g) decreases with
increasing strain. At low strain particular the g ! e transfor-mation is triggered by deformation. Further compression
leads to e!a0 and g! e!a0 transformations, respectively.
The formation of martensite can also be observed by
deformation bands in Figure 7(g).
Conclusions
The ceramic plastic extrusion route at room temperature
has been applied in order to produce honeycomb macro-
structures based on austenitic stainless TRIP-steel and
TRIP-steel/magnesia partially stabilized zirconia composite
materials, respectively. It can be resumed that the reinforcing
mechanism of additions of ceramic particles enables compo-
site materials with superior mechanical properties. Advan-
tages have been achieved in terms of higher compressive
stresses as well as energy absorption during deformation. The
martensitic transformation in both phases was proven by
EBSD measurements resulting in a strain dependent phase
evolution.
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Three main conclusions after sample producing and
compressive deformation test can be drawn.
(i) H60
eat treatment of the composite material leads to diffu-
sion and several chemical reactions between alloying
elements and zirconia stabilizing agent resulting in high
amount of non-transformable monoclinic zirconia even
before mechanical testing.
(ii) T he stress induced phase transformation in metastablezirconia particles occurs at compressive deformations
below 10%. Furthermechanical load does not significantly
trigger the phase destabilization. Nevertheless, improve-
ments of strength at compressive strain below 35% are
significant.
(iii) T he deformation-induced austenite-to-martensite trans-formation in TRIP-steel matrix is equivalent to strain,
even up to 30%.
In future work the phase composition of the partially
stabilized zirconia particles after sintering has to be changed
regarding higher amounts of metastable tetragonal and cubic
phase. A high potential of reinforcing effects of ceramic
particles can be expected when degreasing the amount of
non-transformable monoclinic zirconia before mechanical
load. Furthermore the mechanism of chemical interactions
between TRIP-steel matrix and zirconia during sintering has
to be investigated.
Received: April 27, 2011
Final Version: June 1, 2011
Published online: July 21, 2011
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