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Analysis of Thermoelectric Power TTP Diagrams of Aluminum Alloy 6061

Produced by Two Different Techniques

Article · March 2012

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International Journal of Research and Reviews in Mechatronic Design and Simulation (IJRRMDS) 86
Vol. 2, No. 1, March 2012, ISSN: 2046-6234
© Science Academy Publisher, United Kingdom
www.sciacademypublisher.com

Analysis of Thermoelectric Power TTP Diagrams of Aluminum

Alloy 6061 Produced by Two Different Techniques

D. Dafir1, R. Saadani2, and A. Jamil3

1
ESTF/Mécanique, Mly Abdellah, Fes, Morocco
2
ESTM/Génie électrique, Mly Ismail, Meknès, Morocco
3
ESTF/Génie des Procédés, Mly Abdellah, Fes, Morocco
Email: dafird1@yahoo.fr, rachidsaadani@gmail.com, abdelmajid.jamil@gmail.com

Abstract – A convenient representation of the microstructural evolution of 6061 aluminum alloy in income is to draw a
diagram time, temperature, precipitations (TTP) which are worn areas of existence of each phase versus time and for each
tempering temperature.
Keywords – Aluminum, Diagram TTP, Precipitation

1. Materials and experimental procedure sample-shaped plate is tight in these blocks. The PTE on the
alloy compared to pure aluminum at temperature T and T +
1.1. Material DT / 2 is given by:
In this study we compared the evolution of the
ΔS = ΔV / DT (uV / K)
precipitation of two alloys of the same nature, but developed
in different conditions. For this purpose we have prepared: Where ΔV is the voltage produced by the Seebeck effect
An alloy based on aluminum grade 6061 (Alloy A), between the two aluminum blocks. The measurement
prepared by the technique of powder metallurgy. This alloy accuracy of ΔV is 0.2%. The absolute TEP of the sample S is
has been provided by the company Kob Steel Company. Its given by:
composition is given by the following table:
S = Sal + ΔS (1)
Eleme Si Mg Fe Cu Ni Zn Cr Ti Mn Pb
nt PTE Ltd is the absolute aluminum (-0.2 mV/K at 20 ° C).
Wt % 0,6 0,8 0,3 0,2 0,0 0,0 0,0 0,0 0,0 0,0
5 1 2 6 1 5 9 4 6 1
The selected temperatures are T = 15 ° C ± 0.1 ° C and
AT = 10 ° C ± 0.1 ° C
The other alloy is an alloy grade 6061, it was provided by The camera looks directly on the PTE of the sample. The
the company Pechiney. This material was prepared by casting duration of a measure is about one minute. The shape of the
forging. Its composition is given in the table below: sample does not matter. The only requirement is to ensure
good thermal contact to the block level. Avoid samples with
Element Si Mg Fe Cu Zn Cr Ti Mn thermal conductance is too high. In our case we used
Wt % 0,6 1,01 0,2 0,2 0,09 0,17 0,01 0,06 specimens’ parallelepiped of 70x5x1 mm.

Magnesium and silicon are the main alloying elements of
these alloys; they ensure the hardening of the alloy by the
formation of the compound Mg2Si.
The alloy used as a hardening alloy, it necessary to
subject him to a three-stage heat treatment to induce the
formation of hardening precipitates. Treatment usually done
to harden this alloy is the T6 treatment which consists of:-
Homogenization of 2 hours at 535 ° C- A water quench- An
income at 175 ° C for 8 hours
1.2. Measurement of thermoelectric power (TEP)
1.2.1. Principle:
The principle of the apparatus designed for measuring
PTE metal alloy. Two aluminum blocks a and b are
maintained at the respective temperatures T and T + DT. The
2. Characterstique thermoelectric power
aluminium and its alliaeges
The absolute TEP of a metal or alloy can be written:
S = Sd + Sg (2)
where Sd is the diffusional component of PTE associated
with a random distribution centers in thermal equilibrium
distribution of electrons, and the component of Sg photon
drag, which depends on the interaction of photons with the
electrons of the crystal and all the scattering centers the
network.
In the case of aluminum, the diffusional component is
predominant at room temperature, which is the temperature at
which it will make measurements.
D. Dafir et al. / IJRRMDS, Vol. 2, No. 1, pp. 86-91, March 2012 87

2.1. Influence of elements in solid solution

In the case of dilute alloys, the change at a given
temperature ΔSd component diffusional Sd is described by
the Gorter and Nordheim equation:
ΔSd = (ΣΔρiΔSi) / (Σ + ρ0 Δρi) (3)
ρ0 is the resistivity of the alloy without solute atoms but
possibly including an increase in resistivity due to
precipitates. Δρi is the increase in resistivity (Δρ = αici, here
and αi is the concentration and the specific resistivity of the i
solute atoms in solid solution), the PTE is ΔSi specific atoms Figure 2. Evolution of PTE 6061 A of the alloy as a function of time back to
of solute i in the pure solvent. 75 and 100 ° C.
The effect of impurity on the PTE in the case of
multicomponent alloys can be considered as an additive if
and only if ΣΔρi <<ρ0
For each element, the values of ΔSi may be inferred from
these curves and are given in the table below [1].
If the elements Mg Cu Fe Mn
ΔSi (uV / K) +2.4 +2.1 -0.74 -8 -6.8
αi (μΩ.cm /%) 0,540 0,344 1,020 2,560 2,940

2.2. Influence of precipitates

Large incoherent precipitates have a negligible effect on
the PTE if their volume fraction is very low (<10%). Figure 3. Evolution of the PTE of the alloy 6061 A function of time of
However, the GP zones or very small semi-coherent income at different temperatures between 125 ° C and 225 ° C.
precipitates may have a significant effect on the PTE [2].

2.3. Influence of dislocations

The dislocations have a very low intrinsic effect on the
PTE of pure aluminum. However they can induce large
changes in PTE due to an indirect effect (formation of
Cottrell atmosphere for example) [3].

2.4. Experimental results

We followed the evolution of PTE in income at 25 ° C
(Fig. 1) at 75 ° C and 100 ° C (Fig. 2) at 125 ° C, 150 ° C,
175 ° C, 200 ° C and 225 ° C (Fig. 3), to 225,250 ° C, 275 °
C and 300 ° C (Fig. 4) and finally to 350 ° C and 400 ° C Figure 4. Evolution of the PTE of the alloy 6061 A function of time of
income at different temperatures between 225 ° C and 300 ° C.
(fig: 5).

Figure 5. Evolution of PTE 6061 A of the alloy as a function of time back to

300 ° C and 400 ° C.
Figure 1. Evolution of PTE 6061 A of the alloy as a function of time back to
25 ° C.
Changes in PTE observed at 25 ° C and 75 ° C correspond
either to the precipitation of GP zones incomplete, or the rush
followed by the formation of precipitates coherent β ".
Between 125 ° C and 225 ° C (Fig. 3), we observe the
kinetics of evolution of PTEs regularly shifted against each
other, this shift corresponds to the thermal activation linked
to the phenomenon of precipitation. These curves show for
D. Dafir et al. / IJRRMDS, Vol. 2, No. 1, pp. 86-91, March 2012 88

aging temperatures the weak monotonic variation reflecting and (7) represent, for temperatures between 125 ° C and 225
the precipitation of one phase in the observed time scale (t ° C and between 225 ° C and 300 ° C on the other hand, the
<104 min). For higher temperatures, a minimum is obtained ratio (ΔS) / (ΔS) max function of time.
on the PET curves reflecting a phase change. Note that the
offset regular curves as a function of aging temperature
disappears between 200 ° C and 225 ° C, which likely
reflects a change in type of initial precipitation.
We can assimilate all of these curves to the precipitation
of phase β 'and β transition. "→ β'. The temperature of 225 °
C seems to be the temperature limit of stability of the β
phase. "
The maximum amplitude of variation of TEP during the
precipitation is much the same. This can be explained by the
fact that the maximum sensitivity of the element of addition
may vary in this temperature range and thus the amount of Figure 6. Evolution of the normalized curves of the alloy PTE 6061 A
metastable phase formed is always the same. Although the function of time in income between 125 ° C and 225 ° C.
precipitates have an inherent influence on the PTE, we can
estimate that this effect is the same, the volume fraction
formed is practically constant.
Between 225) C and 300 ° C (Fig. 4), we observe an
initial decrease of PTE associated with the direct
precipitation in the matrix phase β 'and then a rise again due
to the appearance of the β phase and late a bearing on aging
time corresponding to the highest stage of coalescence of this
phase. There cons by a significant decrease in the amplitude
of this variation in PTE associated with the precipitation
when the temperature increases. This decrease can be
attributed to the increase in the solubility of alloying
elements with temperature. Figure 7. Evolution of the normalized curves of the alloy PTE 6061 A
function of time in income between 225 ° C and 300 ° C.
The evolution curves at 300 ° C and 400 ° C (fig: 5) are
characterized by a rapid decrease of PTE during the first
minute of aging, amplitude lower than for lower
temperatures, followed by a plateau . These curves
correspond to direct precipitation of the β phase. Following
this is a step back from PTE which we will explain later.
To analyze our results, we proposed to use the law of
Johnson.Mehl [4], applicable in the temperature range where
only one type of precipitation is formed.
This law is expressed by the following equation:
Y = 1 - exp (-KTN) (4)
Where Y is the fraction precipitated at a given temperature, K Figure 8. Johnson-Mehl equation applied to the precipitation in the alloy A
the rate constant, and n is a coefficient characterizing the 6061.
mode of precipitation.
Assuming a linear relationship between the PTE and the The representation of LnLn (1/1-Y) gives straight lines,
precipitated fraction, Y is given by the following equation: indicating that the precipitation kinetics are consistent with a
Y = (ΔSt - ΔS0) / (ΔSM - ΔS0) law of Johnson-Mehl type. The slope of these lines represents
the coefficient n. The network of curves shown in figure (8)
= Δ (ΔS) / Δ (ΔS) / Δ (ΔS) max (5) distinguishes two families of kinetics. One includes all the
Where ΔSt. ΔS0 ΔSmax and are respectively the PTE on kinetics carried out at temperatures below 225 ° C for which
now, after quenching and end of precipitation. there is a value of n approximately equal to 1.15. According
to (Burke 68), this value of n is characteristic of a diffusion-
A - Determination of the coefficient n controlled growth. The other family consists of all the
The curves of PTE for each annealing temperature were kinetics carried out between 250 ° C and observed for these
standardized according to the relation (5) by taking into temperatures 300C.On a network of curves with an
account that the precipitation kinetics of the phase formed associated coefficient n in the range of 0.95.Selon [4] the
directly after quenching. Thus the value representing the value of n is characteristic of growth controlled by diffusion
ΔSmax PTE on the end of precipitation, is the value of ΔS and interfacial phenomena.
measured minimum of the curve of evolution when a The two different values obtained for n according to the
transition between metastable phases is observed. Figures (6) temperature range clearly confirm that a transition occurs in
the type of precipitation at a temperature of 225 ° C.
D. Dafir et al. / IJRRMDS, Vol. 2, No. 1, pp. 86-91, March 2012
B - Energy of activation
The activation energy put into play during the
precipitation is determined by two methods:
 The first is to calculate the rate constant K for each
aging temperature. The energy Ea is determined from
the slope of the Ln (K) versus 1 / T, reflecting the
relationship Arrhénus:
K = K0exp (-Ea/KB.T)
Where K0 is the frequency factor, KB the Boltzmann
constant and T the absolute temperature of aging.
 The second calculates Ea without using the empirical
law of evolution. This is to express the fractional
reaction time τ as a function of aging temperature as
follows:
τ = τ0 exp (-Ea/KBT)
Where τ is the time required for the precipitation of a fraction
Y precipitation of phase β 'β is the transition. "→ β'. It is
The drawing of curves giving Ln (τ) versus 1 / T (fig) (Y
= 0.8) also shows two distinct areas. We obtain two lines, one
in 125 ° C-225 ° C, the other in 225 ° C - 300 ° C
corresponding to two different activation energies,
respectively 21.9 kcal / mol at low temperatures and about 15
kcal / mol at high temperatures (we obtained values of
activation energy comparable to the precipitated fractions of
0.5 and 0.8).
All the results concerning the activation energy and the
value of n therefore shows clearly that the temperature of 225
° C is the temperature of transition between two types of
precipitation that, given the temperature ranges concerned
are:
 Below 225 ° C, germination and growth of the direct
phase β "from the solid solution followed by the β
transition." → β '.
 In over 225 ° C, germination and growth of the direct
phase β'à from the solid solution followed by the
transition β '. → β.
3. TTP diagram
A convenient representation of the microstructural
evolution of an alloy in income is to draw a diagram Time
Temperature Precipitation (TTP diagram) which are worn
areas of existence of each phase over time for each annealing
temperature (Fig: 9).
These areas are defined by the evolution curves as a
function of temperature, precipitation start time or transition
time. The areas defined dan these diagrams, however, can be
meaningful microstructural slightly variable. Thus, in the
case of aging at the temperature T1 (Fig: 7) where the β
phase "seed directly from the solid solution, the point A on
the edge of field (1) corresponds to a state where there is only
β phase. " The passage of the line L2, point B corresponds to
a state which coexists microstructural phase β 'phase and β'.
At higher temperature (T2), where the phase β 'seed directly
from the solid solution, the point C corresponds to a state
where there is only phase β '.
An electron microscopy study was also carried out:
 To confirm the validity of the interpretations put
forward concerning the development of PTE
89
 To compare with the times and processing temperatures
on the size of the precipitates formed.
 To clarify, for very short times of aging, the limits of
appearance of various phases.
Fig (10) represents the TTP diagram of the alloy A, aged
after homogenization of 2 hours at 535 ° C and quenching in
water, determined by measurements of PTE and electron
microscopy observations.
(6) Can be distinguished in this diagram features four
temperature ranges:
 - First domain (T <125 ° C): the precipitation starts with
the formation of GP zones, which correspond to a
collection of atoms of silicon and magnesium in
clusters.
 - Second area (125 ° C <T <225 ° C): Aging begins with
the precipitation generalized coherent precipitates β ".
(7) These precipitates are distributed homogeneously in a
matrix, their size is several nanometers. After
observed more rapidly than it moves to higher
temperatures. For example, an income of 5 hours at
200 ° C ( point 2 of the diagram TTP), appear the first
precipitated phase semi-coherent β ', obtained from a
development precipitates β ". After 24 hours of aging
at this temperature, we obtain only sticks phase β ',
whose length is about 40 nanometers. When you push
back to the treatment of 4 days, the length of the rods
can be up to 200 nm [5].
 - The third field (225 ° C <T <325 ° C): The semi-
coherent phase is formed directly without preliminary
precipitation of the β phase. "This precipitation is
heterogeneous because it is formed on the dislocations
that favor its appearance . Point 4 on the diagram
corresponding to a TTP income 10 minutes at 250 ° C,
shows the semi-coherent precipitates β 'whose length
is about 200 nm in diameter but slightly more
developed (the about 30 nm) compared with rods
obtained in income 24 hours at 200 ° C. An income of
24 hours at 250 ° C leads to precipitation of the
incoherent phase precipitated from β '. This is
illustrated by al micrograph of Fig () (item 5 on
diagram TTP). The size of the incoherent precipitates
is about 0.35 microns. At 300 ° C, one minute
revenud'une gives rise to no precipitation in the
matrix. In contrast, treatment 5 minutes at the same
temperature leads to a direct precipitation of
equilibrium phase β coxistant with the precipitates of
phase β '(item 6 on the diagram TTP).
- The precipitation of the equilibrium phase from β
microns is obtained during an income at 300 ° C for
24 hours (point 7 of TTP diagram). These precipitates
have the shape of platelets with a length of about 1μm
and diameter of 60μm.
 Fourth domain (T> 325 ° C): Phase equilibrium β
precipitates directly without preliminary precipitation
of phases β''et β '. For an income of 10 minutes at 350
° C, (point 8 of the diagram TTP) shows only
incoherent precipitates with a density much lower than
that of rods.
D. Dafir et al. / IJRRMDS, Vol. 2, No. 1, pp. 86-91, March 2012
3.1. Case of the alloy cast / wrought (alloy B)
We reported in the literature that the kinetics of
precipitation was generally faster in alloys produced by
powder metallurgy, due to the very small grain size. With
two alloy compositions close, but prepared under different
conditions, we compared their TTP diagram
Figure 9. Log (t) = f (1 / T) alloy A (Y = 0.8).
Figure 10. Diagram of the alloy TTP 6061 A.
Figure 11. Diagram of the alloy TTP 6061 B (solid line) compared to the
alloy 6061 A.
Figures (11) provide an example of the kinetics of
precipitation observed in the alloy B. The conclusions can be
drawn from the kinetic analysis and comparison with those
obtained on the alloy A are:
The fields, the apparent activation energy of precipitation
for each type of phase are fundamentally altered, as shown in
the table below.
Table: Values of n and the activation energies compared alloys A and B
Others (β'') Ea (β ') n (β'') n (β') Tc
Alloy A 21.1 15.7 1.15 0.95 200-225
Alloy B 20.4 14.2 1.10 0.95 200-225
However, the alloy produced by powder metallurgy has a
slight acceleration of precipitation kinetics compared to the
alloy prepared by conventional cast. This acceleration is
more marked as we place ourselves at temperatures higher
90
income.
 Comparison of the two TTP diagrams for alloys A and
B, shows a shift to low temperature areas of phase
stability in the case of the alloy produced by powder
metallurgy from the cast alloy / forged. This is
especially true for semi-coherent precipitates β ', the
stability domain is shifted about 10 ° C throughout the
entire diagram. This results in isothermal, reduced
time corresponding to the β transition. "→ β 'and thus
an apparent acceleration of the precipitation.
 The precipitation has a slightly different morphology.
Some electron micrographs of control illustrate this
fact. Thus, there is in the case of alloy B:
 For an aging of 10 minutes at 200 ° C, the presence of β
zones "where cons of consistency seems more marked
than in the case of A. Alliger
 For a treatment of 10 minutes at 225 ° C the presence of
precipitates β 'whose density is lower than in the case
of alloy A
 For treatment of 3 hours at 300 ° C the presence of
platelets in the β phase (Dafir, 93)
4. Conclusion
We were able to carry out a comprehensive study of
precipitation phenomena in alloys of type 6061. These alloys
are industrial type, it is interesting to compare our results
with those da literature to determine to what extent our
results may be of general character.
4.1. Area of phase stability
The temperature limit of formation of the phase coherent
β "has been the most studied. We have presented the results
concerning the solubility limit & T in Chapter IB. It should
be noted, despite the diversity of the alloys studied. (Alloys
of high purity [6], industrial alloys, alloys with or without an
excess of silicon over the composition of MgSi) a good
agreement in the results. According to the TTP diagrams we
have established, the temperature stability limit β phase
"appears to be about 220 ° C. Given the composition of our
alloys (about 1.5 wt% Mg 2 Si) our results are in good
agreement with the results of other authors (see Figure I.10)
Furthermore, these diagrams have allowed us to locate the
temperature limit of formation of the phase β'à worth about
330 ° C.
GP zones on incomplete, it appears that it are unstable
above 120) as c, from this temperature, the curves of
evolution of PTEs have only a single stage. However, only
one electron microscopy study could help define the exact
nature of the coherent precipitation.
4.2. Energy of activation
The calculation of activation energies corresponding to
the precipitation of the β phase "gives a value of 1 kcal / mol.
Studying the evolution of hardness, is a value of the
activation energy nearly identical (0 kcal / mol) energy
distribution of magnesium and silicon in aluminum (26 and
33 kcal / mol) is larger than the activation energy related to
the formation of β ". This can be explained by the fact that, in
the case of Al-MgSi alloys hardened, simulcasting of solute
atoms / gaps accelerating the diffusion and thus decreasing
D. Dafir et al. / IJRRMDS, Vol. 2, No. 1, pp. 86-91, March 2012 91

the activation energy of the precipitation phenomenon.

As for the activation energy of phase β ', the value found
(about 15 kcal / mol) consistent with the results of (Czirak
71) who studied the precipitation in an Al-1.7% Mg2Si.

4.3. TTP diagram

Comparing the two diagrams TTP showed an acceleration
of the precipitation in the composite prepared by powder
metallurgy. This phenomenon can be attributed
unequivocally to differences in microstructures resulting
from different methods of preparation. Indeed, differences in
composition between the two alloys have rather a result
opposite to that observed on the kinetics, since the alloy
produced by powder metallurgy is slightly less loaded with
magnesium.
Given these differences, we need to note that any study of
the influence of the reinforcement in a composite must be
made in comparison with the kinetics of precipitation in an
unreinforced matrix under the same conditions as the
composite.

References
[1] J.M PELLETIER, Vigier G, MERLIN J, Fouquet F. and BORRELLY
R.1984,.''effects on precipitation in Al thermopowwer Cualloy''Acta
Met. 32, 1984, pp. 1069 to 1078.
[2] PELLETIER JM 1980.''Thermoelectric power of alloys of copper and
aluminum: a study of solid solutions and the role of the precipitation of
a second phase.''Thesis LYON 1980.
[3] P. MERLE, J. MERLIN, JMPELLETIER.Validity of a lamellar model
for flow stress of alloys Containing plate-like precipitates.proc. of the
5th Int. Conf. On the Strength of Metals and Alloys-Aachen, 1979, pp.
657-662
[4] Burke, J. The kinetics of phase changes in metals. Taken: Masson et
Cie, 1968. 247p.
[5] Dafir, D; GUICHON, G. ; BORRELLY, R CARDINAL, S., Gobin, F,
MERLE, P. Study by Thermoelectric Power mesurements of the
microstructural evolution of the matrix of SiC particle-reinforced
aluminum alloy 6061, Materials Science and Engineering, vol. A144,
311-318, 1991. Dafir, D., Thesis, University of Lyon, 1993
[6] MURAKANI, Y. KOMATSU, S. and ONISHI? TAKEO. The Two-
stage aging of Al-Mg-Si alloy. Mem. Fac. Eng. Kyoto University,
1969, Vol. 31, p. 130-159

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