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Communications solubilization temperature down to room temperature are under

way, as an attempt to produce a good combination of strength


and fracture toughness. In this article, we discuss a specific
Room-Temperature Cleavage feature of fracture behavior revealed by specimens submitted
to one of the controlled cooling conditions under study.
Fracture of FeMnAlC Steels A 10-kg ingot of Fe-28Mn-8.5Al-1C steel with 1.25 pct
silicon was prepared in a vacuum induction furnace under
controlled argon ambient. It was then homogenized for 6 hours
O. ACSELRAD, J. DILLE, L.C. PEREIRA,
at 1150 °C and then hot rolled to a final thickness of 13 mm.
and J.-L. DELPLANCKE After cutting into billets, the billets were solution treated at
Alloys of the FeMnAlC system have been extensively stud- 1050 °C for 2 hours and water quenched.
ied in recent years, and perhaps their more attractive aspect is A PHILIPS* CM 20 scanning transmission electron micro-
the possibility of obtaining different combinations of mechan-
ical strength, ductility, and fracture toughness over a wide tem- *PHILIPS is a trademark of Philips Electronic Instruments Corp., Mahwah.
perature range. For structural purposes, a good combination
of mechanical strength and fracture toughness is desirable, and scope (200 kV), a MEV-ZEISS 940-A electron scanning micro-
so far the most commonly used treatment is that involving scope and a TMX 2010 Discoverer Topometrix Scanning Probe
quenching from temperatures within the austenitic field and Microscope (atomic force microscopy) were applied for
subsequent aging for 15 hours within 500 °C to 600 °C. The microstructural characterization. Fracture toughness was char-
resulting hardness and mechanical strength are high, but frac- acterized by KA, the apparent fracture toughness,[5] using con-
ture behavior may be unacceptable for critical applications. ventional Charpy 10  10 mm test specimens. The KA values
Experiments concerning controlled cooling are under way, as were determined after Charpy instrumented tests (Tinius Olsen
an attempt to produce a good combination of strength and frac- 64 equipment with Dynatup 500 instrumentation system, USA)
ture toughness. In this communication, we discuss a specific at room temperature.
feature of fracture behavior revealed by specimens submitted The controlled cooling experiments consisted of a fast cool-
to one of the processing conditions under study. ing from the solubilization temperature down to 550 °C, hold-
ing at this temperature for 7 minutes, and air cooling to room
temperature. Similar experiments were conducted at 700 °C,
and also with two successive 7-minute steps at 700 °C and
Alloys of the FeMnAlC system have been extensively 550 °C. These treatments were performed directly on the Charpy
studied in recent years, and perhaps their more attractive specimens, care being taken so that the central region (the vol-
aspect for structural application is the possibility of obtain- ume of material comprised between the lines situated at 5 mm
ing different combinations of mechanical strength, ductility, of both sides of the notch) was effectively submitted to the
and fracture toughness over a wide temperature range. Above thermal cycles, imposed by means of a Smitweld thermocycle
850 °C, alloys with 28 to 30 pct Mn, 8 to 10 pct Al and 0.8 device. For a comparative study, samples were also directly water
to 1 pct C (usual composition ranges) present a supersatu- quenched from the solubilization temperature.
rated austenitic structure. After quenching to room temper- Fracture toughness results and the hardness of differently
ature, although the austenitic structure is not fully preserved,[1] processed specimens are shown in Table I.
the resulting properties are high ductility (60 to 70 pct total According to previous results,[1] the microstructure of the
elongation) and reasonable mechanical strength (ultimate controlled cooled specimen with a 7-minute step at 550 °C
tensile strength (UTS) around 800 to 900 MPa). This consists of an austenitic matrix containing an extremely fine
austenitic phase undergoes a series of decomposition reac- distribution of -phase particles. At the very beginning, fol-
tions during isothermal holding within the temperature range lowing the initial spinodal decomposition of austenite, these
350 °C to 700 °C.[1] When aging at temperatures ranging particles are formed as cuboids with dimensions of the order
from 500 °C to 750 °C, a fine distribution of (Fe,Mn)3AlC of 2 to 3 nm, finely dispersed, coherent, and isomorphic to
carbide ( phase) appears, resulting in a significant improve- the matrix.[6] After the 7-minute step at 550 °C, they can
ment in mechanical strength.[2,3] be observed by transmission electron microscopy (TEM), as
For structural purposes, a good combination of mechanical shown in Figure 1, with particles smaller than 10 nm in a
strength and fracture toughness is desirable, and so far the most very compact distribution and partially aligned along the
commonly used treatment is that involving quenching from 001 axis of the austenitic matrix.
temperatures within the austenitic field and subsequent aging The controlled cooling procedure presents a promising
for 16 hours at 550 °C.[4] The resulting hardness and mechan- combination of hardness and toughness, but further devel-
ical strength are high (Hv of 340 and UTS around 1200 to 1400 opment demands the understanding of a particular feature
MPa), but fracture behavior may be unacceptable for critical of the fracture process revealed by the impact test. The
applications. Experiments concerning controlled cooling from fracture process of the specimen treated at 550 °C starts in
a ductile mode just after a narrow stretch zone (Figure 2)
and rapidly changes to a brittle fracture, with many trans-
O. ACSELRAD and L.C. PEREIRA, Professors, are with the Metallurgy granular cleavagelike facets containing linear markings along
and Materials Engineering Department, Federal University of Rio de Janeiro, three different directions. A better performance of these
21949-900 Rio de Janeiro, Brazil. J. DILLE, Research Engineer, and
J.-L. DELPLANCKE, Director, are with the Science des Matériaux et Elec-
alloys will only be possible once this cleavagelike fracture
trochimie, Université Libre de Bruxelles, 1050 Brussels, Belgium. is clearly understood so that an appropriate method can be
Manuscript submitted November 18, 2003. developed for suppressing such fracture behavior.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 35A, DECEMBER 2004—3863


Table I. Heat Treatments and Properties Cleavagelike fracture facets as this were already observed
on several austenitic steels fractured at cryogenic tempera-
Hardness KA
1MPa 2 m2
tures.[7–11] On the other hand, no similar observation has
Treatment (Hv)
been done before on austenitic steels at room temperature.
Solubilized and water Three different models are reported in the literature in order
quenched (austenitic) 270 330 to explain the brittle fracture of face-centered cubic alloys:
Solubilized and aged at 550 °C
for 15 h (intense -phase (1) nucleation of microcracks at intersections of deformation
precipitation) 436 84 twins, where high internal stresses are built up;[7]
Fast cooled from solubilization (2) cracking caused by the formation of epsilon martensite
temperature to 550 °C with 7 min
plates;[8] and
holding step followed by air cooling
to room temperature 335 115 (3) slipping-off of active slip planes with a high density of
Fast cooled from solubilization dislocations.[9,10,11]
temperature to 700 °C with 7 min
Thin foils parallel to the fractured surface were prepared
holding step followed by air cooling
to room temperature 325 130 right under the fracture surface. After that, they were exam-
ined by TEM. The observation reveals arrays of planar
dislocations forming slip bands and arrays of long disloca-
tions (Figure 3). These arrays are similar to those observed
by Tomota et al.[9] in high nitrogen bearing austenitic steels
fractured at 77 K. Neither mechanical twinning nor epsilon
martensite plates have been observed.
According to the model proposed by Tomota et al., the dis-
location substructure observed under the fractured surface of
our FeMnAlC alloy indicates that the primary fracture mech-
anism is slipping-off along the slip plane. Tobler and Meyn[11]
assume that this slip-band cracking is facilitated by planar
slip, and this may occur if some type of matrix hardening
process increases the difficulty of activating out secondary plane
slip. In this case, shear strain continues to accumulate in a
well-defined narrow slip band. The accumulation of dislocation-
induced defects in this band weakens it to the extent that the
component of tensile force on the band causes final separa-
tion, giving the observed cleavagelike appearance. For this alloy,
we believe that the most likely reason for matrix strengthening
is the fine precipitation of  carbides (Figure 1).
Fig. 1—Fine -phase precipitates after controlled cooling for 7 min at 550 °C, When the controlled cooling is conducted with the step at
atomic force microscopy. 700 °C, a completely different microstructural picture is estab-

(a) (b)
Fig. 2—Scanning electron micrographs obtained from the fractured surface of Charpy impact test specimen after controlled cooling experiment with a 7-min
step at 550 °C: (a) narrow stretch zone adjacent to notch root and ductile transition region; (b) detail of the ductile region; and (c) brittle fracture area, just
beyond the ductile region: cleavage facets with linear arrays and intergranular separations. (d) detail of Fig. (c).

3864—VOLUME 35A, DECEMBER 2004 METALLURGICAL AND MATERIALS TRANSACTIONS A


(c) (d)
Fig. 2—(Continued). Scanning electron micrographs obtained from the fractured surface of Charpy impact test specimen after controlled cooling experiment
with a 7-min step at 550 °C: (a) narrow stretch zone adjacent to notch root and ductile transition region; (b) detail of the ductile region; and (c) brittle fracture
area, just beyond the ductile region: cleavage facets with linear arrays and intergranular separations. (d) detail of Fig. (c).

(a) (b)
Fig. 3—(a) and (b) TEM micrographs below the fractured surface of an impact test specimen controlled cooled with a 7-min step at 550 °C.

lished, since with longer times or higher temperatures, the Therefore, as the preliminary results suggest (Hv equal to 325
size of the -phase particles increases and their composition and KA of 130 MPa 2 m ), a better performance can possi-
and lattice parameter change. A regular and periodic struc- bly be obtained in terms of fracture once possible causes for
ture begins to appear, and as seen in Figure 4, the particles cleavagelike fracture are removed or prevented. In fact, we
are no longer nearly equiaxial, but about 25 to 30 nm in did not observe in specimens treated at 700 °C for 7 minutes
their main dimension, regularly spaced along the crystallo- signs of the cleavagelike fracture we described previously.
graphic 001 directions of the austenitic matrix. It is pos-
sible that such a configuration is less severe in strengthening
the austenitic matrix than the extremely fine distribution of
-phase particles, once elastic distortions introduced in the The authors express their gratitude to Dr. P. Lienard
matrix can be at least partially relieved by the regular array (Faculte Polytechnique de Mons, Belgium) and Mr. D.L.C.
of larger particles disposed along the 001 directions.[6] Neves, for their assistance in obtaining some of the experimental

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 35A, DECEMBER 2004—3865


(a) (b)
Fig. 4—(a) and (b) TEM micrographs showing the modulated structure of the -phase precipitates after controlled cooling for 7 min at 700 °C.

results, and to CNPq (Brazil)/FNRS (Belgium), for financial 4. G.L. Kayak: Met. Sci. Heat Treatment, 1969, vol. 2, pp. 95-97.
support through International Cooperation Agreement Proc. 5. W.L. Server: J. Test. Eval., 1978, vol. 8, pp. 29-34.
6. L.D. Chumakova, I.S. Kalashnikov, and V.S. Litvinov: Phys. Met.
910105/99-5. Metallogr., 1989, vol. 67 (2), pp. 107-11.
7. P. Müllner, C. Sollenthaler, P.J. Uggowitzer, and M.O. Speidel: Acta
Metall. Mater., 1994, vol. 42, pp. 2211-17.
REFERENCES 8. J. Ishizaka, K. Orita, and K. Terao: J. Iron Steel Inst. Jpn. (Tetsu-to-
Hagané), 1992, vol. 78, p. 1846.
1. O. Acselrad, E.M. Silva, I.S. Kalashnikov, and L.C. Pereira: Metall. 9. Y. Tomota, Y. Xia, and K. Inoue: Acta Mater., 1998, vol. 46,
Mater. Trans. A, 2002, vol. 33A, pp. 3569-73. pp. 1577-87.
2. K. Sato, K. Tagawa, and Y. Inoue: Scripta Metall., 1988, vol. 22 (6), 10. Y. Tomota, Y. Xia, and K. Inoue: Acta Mater., 1998, vol. 46,
pp. 899-902. pp. 3099-3108.
3. K. Sato, K. Tagawa, and Y. Inoue: Mater. Sci. Eng., 1989, vol. A111, 11. R.L. Tobler and D. Meyn: Metall. Trans. A, 1988, vol. 19A,
pp. 45-50. pp. 1626-31.

3866—VOLUME 35A, DECEMBER 2004 METALLURGICAL AND MATERIALS TRANSACTIONS A

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