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The formation of (Al8Fe2Si, Al13Fe4) phases from Al-Fe-Si system by TE mode

Conference Paper · March 2015

DOI: 10.1063/1.4914214

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 The formation of (Al8Fe2Si, Al13Fe4) phases from Al-Fe-Si system by TE mode
A. Boulouma, A. Drici, A. Benaldjia, M. Guerioune, and D. Vrel

Citation: AIP Conference Proceedings 1653, 020023 (2015); doi: 10.1063/1.4914214

View online: http://dx.doi.org/10.1063/1.4914214
View Table of Contents: http://scitation.aip.org/content/aip/proceeding/aipcp/1653?ver=pdfcov
Published by the AIP Publishing

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 The Formation Of (Al8Fe2Si, Al13Fe4) Phases From
Al-Fe-Si System By TE Mode
A.Boulouma1, 2, A.Drici2, A. Benaldjia2, M.Guerioune2, D.Vrel3

1- EPST -Annaba-, Algeria.

2- LEREC Laboratory, physics department, University of Annaba- Algeria.
3- LSPM Laboratory, University of Paris 13, France.

Abstract. This work prepared Al8Fe2Si, Al13Fe4mixed sample by ball milling and thermal explosion techniques
applying Al, Fe and Si powders as precursors. Thermal combustion of powder mixes of composition 24, 37 Al+ 50, 36
Fe + 25, 27 Si in mass reveals production of several binary and ternary intermetallic phases such: A113Fe4 and Al8Fe2Si..
Synthesis conditions were optimized to fabricate these phases having many potential applications.
Keywords: Al8Fe2Si, J-Al9FeSi3, A113Fe4, Al-Fe-Si system, thermal explosion.
PACS : 61.66.DK

INTRODUCTION
The Al-Fe-Si system contains many technologically important alloys, such as foil and
sheet products for food packaging, capacitors, lithographic printing sheets, magnetic alloys
for transformer. Furthermore, iron and silicon, originating from bauxite ore and anode
material, are present in nearly all industrial Al-alloys. Metallurgical grade silicon also
contains, among others, aluminium and iron as impurities. Due to these reasons, there are
numerous experimental studies on the phase equilibria of the ternary system, the results of
which have been reviewed from time to time [1-7].
Intermetallic compounds are produced by conventional manufacturing methods.
However, the method based on the principle of self-propagating high temperature
synthesis (SHS) and thermal explosion appears to be promising for ease of production [8].
Aluminium based intermetallic compounds that have been investigated by SHS
production techniques are; NiAl, TiAl, FeAl, NbAl, TaAl, CuAl, CoAl and RuAl [8- 11].
Ternary Al-Fe-Si compounds have been investigated in Al–Si alloy castings containing
iron as an impurity element. Several compounds have been identified and named as D-
Fe2SiAl8,E-FeSiAl5, J-FeSiAl3 and dG-FeSi3 Al9 phases [12]. Production of these AlFeSi
intermetallic compounds by TE method has not been studied in detail so far. A113Fe4,
Al8Fe2Si phases have many technologically and metallurgical applications and influence
on phases formation in the Al-Fe-Si system [13-15].

EXPERIMENTAL PROCEDURE
One powder mix of compositions in weight percentage 24.37Al+ 50.36Fe+25.27Si
(mix A) was made, from fine and high purity elemental powders (5–50 Pm particle size,

4th International Congress in Advances in Applied Physics and Materials Science (APMAS 2014)
AIP Conf. Proc. 1653, 020023-1–020023-7; doi: 10.1063/1.4914214
© 2015 AIP Publishing LLC 978-0-7354-1295-8/$30.00

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 99.9%) of aluminium, iron, silicon. Four samples from (mix A) were ball milled for 30,
120, 210, 300 minutes at a ball to powder ratio of 10:1 at 300 RPM speed.
Pellets of diameter 20 mm and weight approximately 4 g were cold pressed to 70% of
relative density.
In our work the ignition mode is based on the application of high density current at the
cylindrical sample (l=2cm, I=10mm). In the same time a mechanical pressure was applied
(Fig1). All of samples were exposed to a current intensity of 1000 A° under argon
atmosphere.

FIGURE 1, the ignition mode scheme

Shimadzu X-ray Diffractometer 6000 was used to study the crystal structures in the
reflection mode using copper KD X-rays.

RESULTS AND DISCUSSION

* * Fe
+ Al
0 Si
++ Al6Fe2
0
Intensity

++

+
0 +
0 *
+ 0

20 40 60 80 100 120
2T, degrees

FIGURE 2a, X-ray powder diffraction pattern of mix (A) ball-milled 300 min

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 **
* Al8Fe2Si
** Al13Fe4
+ Al5Fe2
++ G-Al9FeSi3
0 Al0.5Fe3Si0.5
00 Al0.3Fe3Si0.7
Intensity

00
*

++

FeSi2
Fe5Si3
++
+

00
0

20 40 60 80 100 120
2T in degrees

FIGURE 2b, X-ray powder diffraction pattern of the reacted mix (A) ball-milled for 30 min

* Al8Fe2Si
**

** Al13Fe4
+ Al5Fe2
++ G-Al9FeSi3
0 Al0.5Fe3Si0.5
00 Al0.3Fe3Si0.7
++
Intensity

+
*

00
++

Fe5Si3

FeSi2

00

0
20 40 60 80 100 120
2T in degrees

FIGURE 2c, X-ray powder diffraction pattern of the reacted mix (A) ball-milled for 120 min

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 * Al8Fe2Si

**
** Al13Fe4
+ Al5Fe2
++ G-Al9FeSi3
0 Al0.5Fe3Si0.5
00 Al0.3Fe3Si0.7
Intensity

*
0

FeSi

00
++

FeSi2
**

Fe5Si3
0

00
20 40 60 80 100 120
2T in degrees

FIGURE 2d, X-ray powder diffraction pattern of the reacted mix (A) ball-milled for 210 min
**

* Al8Fe2Si
** Al13Fe4
+ Al5Fe2
++ G-Al9FeSi3
0 Al0.5Fe3Si0.5
Intensity

00 Al0.3Fe3Si0.7
*

+
*

00
++

FeSi2
Fe5Si3

00
**

20 40 60 80 100 120
2T in degrees

FIGURE 2e, X-ray powder diffraction pattern of the reacted mix (A) ball-milled for 300 min

Figure 2a shows that ball-milled mix A before reaction gives an additional intermetallic
phase Al6Fe2, therefore all post-reacted samples shows almost the same phases such as
Al8Fe2Si, J-Al9 FeSi3, and A113Fe4. Offbeat patterns mean the influence of ball-milled time
on cell parameters of some phases.

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 Figures 2(b,c,d,e) show X-ray powder diffraction patterns of the reacted mix (A) ball-
milled during different times; the formation of Al13Fe4 phase was observed, this binary
phase is reported to dissolve 0.8 mass% Si [16], 0.2 mass% Si [17], 1.0 mass% Si [18], 2.9
mass% Si [19], up to 6.0 mass% Si at 600°C [20], and 4 at.% Si at 550°C [21]. This is
associated with an increase in the a-lattice parameter and a decrease in the b-lattice
parameter; whereas no significant changes in the c-lattice parameter and E were detected
[20].
The composition dependence of a- and b-lattice parameters in Fe4Al13 is expressed by
[20] as:
a (in pm) = 1505.0+1.14*WFe-0.41*WSi
b (in pm) = 862.8-1.41*WFe-1.3*WSi
Where WFe and WSi are the mass % of Fe and Si respectively.

TABLE 1, Crystal structure of Al13Fe4 phase

Phase/Temperature Range Pearson Lattice parameters References/Comments
[°C] Symbol/ [pm]
Space Group/
Prototype
Al13Fe4 mC102 a = 1552.7 to 1548.7 [15], 74.16 to 76.7 at. %
d1160 C2/m b = 803.5 to 808.4 Al solid solubility ranges
Al13Fe4 c = 1244.9 to 1248.8 from 74.5 to 75.5 at.% Al
E= 107.7 to 107.99°
a = 1549.2 [15], at 76.0 at.% Al.
b = 807.8 Also denoted FeAl3 or
c = 1247.1 Fe2Al7
E = 107.69°
A detailed crystallographic analysis of the Al13 Fe4 phase, by means of convergent
beam electron diffraction and high resolution electron microscopy, has been performed by
[14]. Lattice images revealed that the Al13Fe4 crystals are divided into tiny domains (few
thousand pm) which are separated by lattice displacements such as stacking faults [22,
14].This phase was also identified as an active and selective semi-hydrogenation catalyst
[23].
Other ternary phases were observed, such as Al8Fe2Si, J-Al9 FeSi3, Al0.5Fe3Si0.5 and
Al0.5Fe3Si0.5 and Al0.5Fe3Si0.5 The intermetallic Al8Fe2Si is reported when concentration of
Si is between 2 and 12.6 wt%, Fe between 0.05 and 0.5 wt% and solidification rates of 0.1,
1, 5 and 50 K.s-1 in Al–Si–Fe hypoeutectic casting alloy system. this phase evolves at all
levels of the parameters during solidification and subsequently transforms into the
Al9Fe2Si2 through a peritectic reaction when promoted by certain combinations of
solidification parameters such as higher Fe level, lower Si level and slower solidification
rates. Further, it is also hypothesized from experimental evidences that the Al13 Fe4 binary
phase precludes the evolution of Al8 Fe2Si during solidification and subsequently
transforms into the Al9Fe2Si2 phase during solidification. These observations are
anomalous to the publications as prior art and simulation predictions of thermodynamic
phase diagrams of these alloys, wherein, only one intermetallic phase Al9 Fe2Si2 is
predicted to evolve and be retained as the terminal phase at the end of solidification [24].
Binary phases are also observed, such as Al5 Fe2, FeSi, Fe5Si3, and FeSi2

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 CONCLUSION
This work allows using TE mode as a low cost and simple mode to produce advanced
material, as so far as the system Al-Fe-Si which has very important applications in
metallurgical and physics fields. This system is the key to understand transformation
phases at Al/Fe/Si corners. This study put in evidence of using TE mode to produce
Al8Fe2Si, J-Al9 FeSi3, and A113Fe4 phases; we demonstrated that the activation step has an
effect on parameter cells of each phase produced by TE, the activation influences also on
samples activated mechanically by giving some binary phases under what we call
mechanical activation.

REFERENCES
1. Rivlin, V.G., “Assessment of Phase Equilibria in Ternary Alloys of Iron”, J. Less-Common Met., 114,
111-121 (1985) (Equi. Diagram, Review, #, *, 4)
2. Prince, A., “Comment on Intermetallic Phases in the Al-side of the AlFeSi-Alloy System”,J. Mater.
Sci. Lett., 6, 1364 (1987) (Equi. Diagram, Theory, #, 1)
3. Raynor, G.V., Rivlin, V.G., “Al-Fe-Si”, in “Phase Equilibria in Iron Ternary Alloys”, 122-139 (1988)
(Equi. Diagram, 39)
4. Ghosh, G., “Aluminium-Iron-Silicon”, MSIT Ternary Evaluation Program, in MSIT Workplace,
Effenberg, G. (Ed.), MSI, Materials Science International Services GmbH, Stuttgart; Document ID:
10.14596.1.20, (1992) (Crys. Structure, Equi. Diagram, Assessment, 134)
5. Zakharov, A.M., Guldin, I.T., Arnold, A.A., Matsenko, Yu.A., “Phase Equilibria in Multicomponent
Aluminum Systems with Copper, Iron, Silicon, Manganese and Titanium”,Metalloved. Obrab. Tsv.
Splavov, RAN. Inst. Metallurgii. M, 6-17 (1992) (Experimental, Equi. Diagram, 14)
6. Raghavan, V., “The Al-Fe-Si System”, J. Phase Equilib., 15(4), 414-416 (1994) (Equi. Diagram,
Review, 27)
7. Raghavan, V., “Al-Fe-Si (Aluminium-Iron-Silicon)”, J. Phase Equilib., 25(4), 107-112 (2002) (Equi.
Diagram, Review,24)
8. Munir ZA. Ceram Bull (1988);67(2):342.
9. Rabin BH, Wright RN. Metall Trans (1991);A22:277.
10. Yi HC, Moore JJ. J Mater Sci (1990);25:1159.
11. Joslin DL, Easton DS, Liu CT, David SA. Mater Sci Eng (1995);A192/193:544.
12. Mondolfo LF. Aluminum alloys: structure and properties. London:Butterworths; (1979). p. 282 and
534.
13. Korchef.A et al. / Journal of Alloys and Compounds 427 (2007) 176–182
14. Skjerpe, P., “An Electron Microscopy Study on the Phase Al3Fe”, J. Microsc., 148, 33-50(1987)
(Crys. Structure, Experimental, Theory, 12)
15. Miyazaki. S et al. / Materials Science and Engineering A 400–401 (2005) 294–299
16. Armand, M., “Liquation and Equilibrium Diagram: Applications to the Diagram of Aluminium-Iron-
Silicon Alloys” (in French), International Congress of aluminium, Paris. 1954, Revue de l'Aluminium, 1,
305-327 (1955) (Crys. Structure, Experimental, *, 9)
17. Sun, C.Y., Mondolfo, L.F., “A Clarification of the Phases Occuring in Al-Rich Al-Fe-Si Alloys”, J.
Inst. Met., 95, 384 (1967) (Crys. Structure, Experimental, *, 2)
18. Dons, A.L., “AlFeSi-Particles in Commercial Pure Aluminium”, Z. Metallkd., 75, 170-174 (1984)
(Equi. Diagram, Experimental, #, *, 10)
19. Skjerpe, P., “Intermetallic Phases Formed during DC-Casting of an Al-0.25 wt.% Fe-0.13wt.% Si
Alloy”, Metall. Trans. A, 18A, 189-200 (1987) (Crys. Structure, Experimental, 35)
20. Stefaniay, V., Griger, A., Turmezey, T., “Intermetallic Phases in the Aluminum-Side Cornerof the
AlFeSi-Alloy System”, J. Mater. Sci., 22, 539-546 (1987) (Crys. Structure, Equi Diagram, Experimental,
#, *, 13)

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Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions IP: 181.215.134.209 On: Thu, 28 Apr 2016 07:28:51
 21.Krendelsberger N., “Constitution of the Systems Aluminium-Manganese-Silicon, Aluminium-Iron-
Silicon, und Aluminium-Iron-Manganese-Silicon”, Tezisy Inst. Phys.Chem. Univ., Vienna, (2001)
(Crys. Structure, Equi. Diagram, Experimental, #, *, 83)
22.Skjerpe, P., Gjonnes, J., “Solidification Structure and Primary Al-Fe-Si Particles in Direct-Chilled-
Cast Aluminum Alloys”, Ultramicroscopy, 22, 239-250 (1987) (Crys.Structure, Experimental, 21)
23.Armbrüster. M et Al, Al13Fe4 as a low-cost alternative for palladium in heterogeneous
hydrogenation, Nature Materials 11, 690–693 (2012) doi:10.1038/nmat3347
24.Gorny.A et al. / Journal of Alloys and Compounds 577 (2013) 103–124.

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