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Abstract
Fe100xNix alloys (105x590 at%) were prepared by mechanical alloying (MA) of elemental powders in a high-
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energy planetary ball mill and studied by X-ray diffractometry and Mossbauer spectroscopy. It is shown that the
concentration ranges of single-phase solid solutions of MA samples extend significantly as compared with those
obtained by conventional techniques. In our case, the BCC phase exists in the range from 0 to 20 at% Ni and FCC
phase from 30 to 100 at% Ni. Block size was 10–15 nm. Consequent annealing of MA samples resulted in further
extension of FCC single-phase concentration range to the relatively low Ni content (20 at%). This was caused by
considerable retardation of austenite–martensite transformation in MA alloys. The FCC alloys with 20–28 at% Ni were
found to be non-ferromagnetic at room temperature; only the paramagnetic component was observed in the
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corresponding Mossbauer spectra. However, the treatments of low-nickel austenite alloys like cooling in liquid nitrogen
or mechanical deformation provoked austenite–martensite transformation and led to the rise of ferromagnetic
properties. # 2001 Elsevier Science B.V. All rights reserved.
.
Keywords: Fe–Ni alloys; Mechanical alloying; Martensite transformation; Mossbauer spectroscopy
0921-4526/01/$ - see front matter # 2001 Elsevier Science B.V. All rights reserved.
PII: S 0 9 2 1 - 4 5 2 6 ( 0 1 ) 0 0 4 7 3 - 2
S.D. Kaloshkin et al. / Physica B 299 (2001) 236–241 237
will extend the FCC concentration range and the side of low nickel content (Fig. 2). One can see
narrow the BCC concentration range (Fig. 1). further stabilization of FCC phase in the annealed
As it was shown earlier [12,17,18] the MA MA alloys. The transformation of MA Fe100xNix
treatment will always cause the narrowing of two- alloys (x>10) into FCC state during the annealing
phase concentration range in the case of binary then should be followed by the FCC ! BCC phase
systems, because of the constraint of the simulta- transformation in the cooling down to the room
neous existence of several phases with different temperature. However, this non-diffusion auste-
compositions. The only one phase with the lowest nite–martensite transformation appeared to be
Gibbs energy commonly forms at low temperature significantly suppressed for the Fe–Ni alloys
MA process. The AGO-2U mill, which is used prepared by the MA technique. It is interesting
here, combines very high intensity of milling (more that the alloys with 22, 24, 26 and 28 at% of Ni
than 10 times higher than that used in Refs. [1,3]) being single-phase FCC structured after such
with relatively low temperature inside the reactive treatment were paramagnetic, and the correspond-
space due to water cooling of the vials. This creates .
ing Mossbauer spectra of these alloys include only
such milling conditions, which allowed one to ob- one paramagnetic component (single line). The
tain rather narrow two-phase concentration range formation of the non-ferromagnetic alloys seems
(8–10%) in MA Fe–Ni system, as compared with very unusual for the Fe–Ni system. Fig. 2 illus-
not only equilibrium alloys but also with that trates the reasons for such behaviour. The MA
obtained earlier by the MA technique (Fig. 1). process with consequent annealing allowed one to
Thus, the tendency to form narrow two-phase decrease the maximum concentration of Ni at
concentration ranges becomes stronger at a de- which the BCC phase still exists, down to 20 at%
crease of the temperature and an increase of the and all the alloys with a higher Ni content had
intensity of MA process. only FCC phase. However, the dependence of the
After annealing of the samples at 6508C, the Curie temperature on the concentration for the
concentration ranges of phases existence shifted to FCC phase intersects the room temperature at
about 28 at% Ni. As a result, the alloys with
22–28 at% of Ni were paramagnetic.
It is known that the temperature of austenite–
martensite transition is rather sensitive to the
structure transformations of alloy [13,14]. This
transition point should depend on the grain size,
the presence of various types of defects, etc. be-
cause of the closeness of Gibbs energies for BCC
and FCC phases. As it was mentioned before, the
grain refinement in Fe–Ni alloys at rapid quench-
ing (RQ) from melt [13] or MA treatment [1] leads
to a decrease in the temperature of martensite
formation. Therefore, a strong effect of the MA
method of samples preparation, which is used
here, on martensitic point is also expected.
The dependences of austenite-martensite trans-
formation temperature on the composition are
shown in Fig. 3 for the Fe–Ni alloys produced by
different ways: (1) as-cast and quenched from solid
state [15], (2) rapidly quenched (RQ) from melt
Fig. 2. Concentration ranges and the corresponding depen- [13], and (3) obtained by the MA technique [1].
dences of Curie temperatures of BCC and FCC phases in Fe–Ni The curve corresponding to the data of this work
alloys: as-milled and after annealing at 6508C. (4) also is plotted in Fig. 3. As one can see, the
S.D. Kaloshkin et al. / Physica B 299 (2001) 236–241 239
4. Conclusions
.
Fig. 4. X-ray patterns and Mossbauer spectra of Fe78Ni22 Fe–Ni alloys were prepared by MA technique in
alloy: (a) as-milled; (b) annealed at 7008C for 1 h; (c) cooled a high-energy planetary ball mill. MA samples
down to liquid nitrogen temperature; (d) pounded in mortar for showed a significant widening of concentration
5 min. (m) X-ray patterns of martensite, (au) X-ray patterns of
ranges of single-phase solid solutions compared
austenite.
with alloys obtained by conventional methods.
Subsequent annealing of MA samples showed
widening of FCC single-phase concentration
that the very mechanical treatment, but not range down to 22 at% Ni. It was found that the
chemical impurities, primarily affects the auste- austenite–martensite transition temperature de-
nite–martensite transformation. The mechanism of creases significantly for mechanically alloyed
this effect is not completely clear now. It seems Fe–Ni powders. MA alloys with 22–28 at% Ni
that the main cause of this transformation after annealing in austenite temperature region
suppression is the small block size in the MA have a single phase with FCC structure and are
FCC structure; however, the structure defects like not ferromagnetic at room temperature. Low-
dislocations, stacking faults and their interaction temperature treatment as well as deformation
also may play an important role. leads to partial transformation of FCC phase into
S.D. Kaloshkin et al. / Physica B 299 (2001) 236–241 241
BCC phase at 22 at% Ni. The refinement of [7] V.V. Tcherdyntsev, S.D. Kaloshkin, I.A. Tomilin,
microstructure of austenite phase is considered as E.V. Shelekhov, Yu.V. Baldokhin, Nanostruct. Mater. 12
(1999) 139.
one of the most important factors resulting in the
[8] N.S. Kohen, E. Ahlswede, J.D. Wicks, O.A. Pankhurst,
depression of martensite transformation. J. Phys: Condens. Matter 9 (1997) 3259.
[9] L. Schultz, J. Less-Common. Metals 145 (1988) 233.
[10] V.V. Tcherdyntsev, S.D. Kaloshkin, I.A. Tomilin, E.V.
Acknowledgements Shelekhov, Yu.V. Baldokhin, Z. Metallk. 90 (9) (1999)
747.
[11] S.D. Kaloshkin, I.A. Tomilin, G.A. Andrianov, U.V.
This work was supported by INTAS Project No. Baldokhin, E.V. Shelekhov, Mater. Sci. Forum 235–238
99-01741. (1997) 565.
[12] S.D. Kaloshkin, J. Metastable. Nanostuct. Mater. 8 (2000)
591.
References [13] Y. Inokite, B. Cantor, J. Mater. Sci. 12 (1977) 946.
[14] G.V. Kurdjumov, L.M. Utevskii, R.I. Entin, Transforma-
tions in Iron and Steel, Nauka, Moscow, 1977.
[1] C. Kuhrt, L. Schultz, J. Appl. Phys. 73 (1993) 1975. [15] M. Hansen, K. Anderko, Constitution of Binary Alloys,
[2] C. Kuhrt, L. Schultz, J. Appl. Phys. 73 (1993) 6588. McGraw-Hill, New York, 1985.
[3] L. Hong, B. Fultz, J. Appl. Phys. 79 (1993) 3946.
[16] K. Shimizu, T. Kakeshita, ISIJ Int. 29 (1989) 97.
[4] R.B. Scorzelli, Hyperfine Interactions 110 (1997) 143. [17] E. Ma, H.W. Sheng, J.H. He, P.H. Schilling, Mater. Sci.
[5] T.M. Lapina, V.A. Shabashov, V.V. Sagaradze, Eng. A 286 (2000) 48.
V.L. Arbuzov, Mater. Sci. Forum 294–296 (1999) 767. [18] P.J. Schiling, J.H. He, R.C. Tittsworth, E. Ma, Acta
[6] Yu.V. Baldokhin, V.V. Tcherdyntsev, S.D. Kaloshkin,
Mater. 47 (1999) 2525.
G.A. Kochetov, Yu.A. Pustov, J. Magn. Magn. Mater.
203 (1999) 313.