Materials Science & Engineering A 689 (2017) 4852

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

A novel cryogenic treatment for reduction of residual stresses in 2024 MARK

aluminum alloy

M. Araghchia, , H. Mansouria, R. Vafaeia, Yina Guob
a
Department of Materials Engineering, Malek Ashtar University of Technology, Isfahan, Iran
b
Bernal Institute, University of Limerick, Limerick, Ireland

A R T I C L E I N F O A BS T RAC T

Keywords: Residual stresses induced during quenching of aluminum alloys cause distortion and have a negative eect on
2024 aluminum alloy their properties. The purpose of this study is to reduce the residual stresses and improve mechanical properties
Residual stresses by using a novel cryogenic treatment. Water quenched samples were cooled down by immersion in liquid
Cryogenic treatment nitrogen at 196 C, following by rapid heating in hot oil at 180 C and nally they were articially aged.
Residual stresses was measured by the hole drilling strain gauge method. The mechanical properties and
microstructure of a heat treated samples were investigated by means of hardness measurements, tensile tests
and transmission electron microscopy. The results showed that this treatment can relieve up to 71% of the
residual stresses compared to 29% related to the traditional cryogenic treatment that used boiling water as the
reheating medium. In addition, there is a considerable increase of about 75 MPa in the ultimate tensile strength
in comparison to the T6 heat-treated alloy. TEM observations revealed that the S precipitates were ne and
uniformly distributed in the microstructure due to deformation during reheating in hot oil.

1. Introduction
The essential step in creating the high strengths in precipitation
hardened aluminum alloys is the rapid cooling from the solution heat
treatment temperature [1]. When cooling is fast enough, it will lead to
higher strength. However, another undesirable eect of rapid cooling is
the generation of residual stresses [2].
However, residual stresses have a negative eects on parts proper-
ties due to distortion and dimensional variation and it may cause
premature failure [3]. Therefore, it is necessary to decrease the residual
stresses generated by rapid quenching to improve the dimensional
accuracy of the components.
Extensive studies have been carried out with the aim of reduction of
residual stresses induced by quenching in aluminum alloys. Some
researchers have changed the quench conditions such as quench
medium and the temperature, which the required strength to be
achieved [46]. In some other studies, the eect of size and geometry
have been researched on the stress distribution [7]. A methods can be
used after quenching to reduce residual stresses for instance the
application of cold working [8], low frequency magnetic elds [9],
electro-pulsing [10] and cryogenic treatment [11], or a combination of
the above.
Cryogenic treatment is the most widely used method to reduce the
residual stresses of aluminum alloys and can be utilized to parts with a
complex shape. This treatment is also known as uphill quenching or
thermo-mechanical method. During conventional cryogenic treatment,
water quenched parts are cooled down by immersion in liquid nitrogen
at 196 C, followed by rapid heating in boiling water or high velocity
steam. Researchers are reported that the residual stresses due to water
quenching can be relieved by up to 80% by using high velocity steam in
cryogenic treatment [1214]. However, this process is associated with
some problems. One of the major disadvantages of conventional
cryogenic treatment is that it is a relatively expensive process that is
often considered too dicult. Moreover, it requires the use of a special
steam nozzle and all surfaces should not receive such a similar thermal
input [15].
The aim of this research is to redesign the conventional cryogenic
treatment to reduce the problems associated with the current methods
and to make it more applicable and cheaper to use. Also the changes
shall be able to improve the mechanical properties.
2. Experimental procedures
In this work, samples with dimensions of 552525 mm3 in size were
cut from a 2024-T3 industrial extruded prole with the chemical
compositions given in Table 1. The samples were solution treated by

Corresponding author.
E-mail addresses: M.Araghchi@ma.iut.ac.ir, M.Araghchi@gmail.com (M. Araghchi).

http://dx.doi.org/10.1016/j.msea.2017.01.095
Received 3 December 2016; Received in revised form 27 January 2017; Accepted 28 January 2017
Available online 31 January 2017
0921-5093/ 2017 Elsevier B.V. All rights reserved.
M. Araghchi et al. Materials Science & Engineering A 689 (2017) 4852

Table 1
Chemical compositions of 2024 aluminum alloy (wt%).

Element Cu Mg Mn Si Fe Cr Zn Ti Al

Nominal 3.84.9 1.21.8 0.30.9 < 0.5 < 0.5 < 0.1 < 0.25 < 0.15 Bal.
In this study 4.37 1.29 0.6 0.3 0.4 0.052 0.075 0.009 Bal.

Table 2
Sample solution heat treatment, quenched media and their corresponding condition.

sample name Solution heat treatment Quenched Media Immersion in liquid nitrogen Reheating Medium Aging

QWNA(T4) 2 h 495 C water 20 C Natural Aging 30 day

QWAA(T6) 12 h 190 C
QWCA1 1h Oil 180 C
QWCA24 24 h Oil 180 C
QWBW24 24 h Boiling Water

Q: Quench, W: Water, N: Natural, C: Cryogenic, B: Boiling for example QWCA24 means quenched
in water at 20 C, immersion in liquid nitrogen for 24 h and followed by articial aged at 190 C for 12 h

procedure provided by TML Measurements Group Ltd. [16]. The hole

was drilled to a depth of 2 mm from the surface. All measurements
were recorded at the same location on the samples center. Multiple
(repeatability) hole drilling measurements allowed an estimation of
one standard deviation of random uncertainties as 25 MPa.

2.2. Mechanical properties measurement

Fig. 1. Heat treatment cycle for new cryogenic treatment by hot oil.
heating to 495 5 , holding for 2 h and then quenched in water at
20 C. Subsequently, the samples were prepared at dierent cryogenic and
reheating treatments and nally were aged at room temperature for 30
days or at 190 6 for 12 h. The detailed description along with samples
labels are given in Table 2 and the temperature proles for solid solution
treatment, cryogenic treatment and articial aging are shown Fig. 1.
Flat tensile specimens were cut from the samples using the electron
discharge machining (EDM) method as described in the standard
technique ASTM E8 with a gauge length of 9 mm and 2.5 mm in width.
Uniaxial tensile tests were carried out with a 500 kN servo-hydraulic
utilizing a laser extensometer at room temperature. Uncertainties in
the 0.2% yield stress and tensile strength were 4% and 2% respec-
tively. Three samples were tested for each condition and the average
was reported.
The measurement of the Rockwell B hardness was carried out in
accordance with ASTM E18-13. For each sample, at least 5 points were
measured to obtain an average value with a typical uncertainty of 1%.
2.3. Microstructure characterizations

2.1. Residual stresses determination A eld-emission transmission electron microscope (JEM-2100F

Residual stresses were measured using the hole-drilling strain-
gauge method according to ASTM E837-01. The RS200 milling guide
was used to generate a hole in the samples. FRS-323 Type A strain-
gauge rosette (Fig. 2a,b) was attached to the samples as stated by the
TEM) was used to characterize the microstructure of the samples.
The TEM specimens were prepared by mechanical grinding and
punching into discs of 3 mm, followed by twin-jet polishing using a
solution of 25% nitric acid +75% methanol at a temperature main-
tained between 40 and 30 C at 20 V.

Fig. 2. Strain gauge rosetta type A (a) Schematic (b) FRS-323(TML Production).

49
M. Araghchi et al. Materials Science & Engineering A 689 (2017) 4852

Fig. 4. The engineering stressstrain curves of 2024 aluminum alloys in dierent

conditions.

Table 4
Hardness and tensile properties of the samples in different conditions.

sample name Hardness 0.2% Ultimate Elongation to

(HRB) yield tensile failure (%)
stress strength
(Mpa) (Mpa)

QWNA(T4) 74.6 0.8 317 12 453 9 16.3 0.7

QWAA(T6) 79.2 0.8 358 14 506 10 11.6 0.4
QWCA1 83.3 0.8 407 16 557 11 10.7 0.4
Fig. 3. (a) Results of measured residual stresses magnitudes by Hole drilling method, (b) QWCA24 86.7 0.9 423 17 581 12 9.8 0.3
Relative reduction in residual stresses compared to water quenched sample and natural QWBW24 81.1 0.9 367 14 540 11 11.4 0.4
aging (QWNA-T4).

3. Results and Discussion
The measured residual stresses are shown in Fig. 3(a), indicating
compressive stress at the surface. The residual stress in QWNA (T4)
sample is as much as 140160 MPa, the highest as compared to the
others. Godlewski et.al. [17] have shown that natural aging has no
eects on residual stresses. Therefore, sample was quenched in water
at 20 C result in the largest residual stress magnitude.
The residual stress magnitudes obtained for the samples quenched
in water and articially aged (QWAA-T6) were 130145 MPa. It was
seen that articial aging treatment (12 h at 190 C) resulted in a 10
20 MPa (about 10%) decrease in residual stress compared to natural
aging. The percentage of reduction of residual stress compared to the
sample naturally aged are represented in Fig. 3(b). It is concluded from
studies on dierent alloys [18] that depending on alloy type, aging time
and temperature, articial aging treatment, causes between 10 to 35%
reduction in residual stresses that ts well with the results in this study.
The residual stresses of the QWCA1 and QWCA24 samples are
about 5070 MPa and 4050 MPa respectively. Using a novel cryo-
genic treatment led to reduction of residual stress from 140 MPa to
40 MPa. It is about 71% lower than that of the sample naturally aged.
Table 3 presents residual stresses of the cryogenic sample in compar-
ison with the results of some published works on aluminum alloys. It
can be seen that as compared to other investigation which used high
velocity steam for reheating medium, new cryogenic treatment is more
ecient to reduce residual stresses. Moreover, holding time in liquid
nitrogen (1h and 24h) has a minor eect on relieving residual stress.
The use of boiling water for the reheating medium results in
reduction in residual stress as much as only 29% in the QWBW24
sample and it reaches to about 100115 MPa.
The use of oil medium at a temperature of 180 C as a heating
medium has some advantages compared to high velocity superheated
steam and boiling water. The oil and liquid nitrogen provide tempera-
tures of 180 C and 196 C, respectively which are higher than that of
steam and boiling water. Higher temperature of heating medium
causes an increase in dierences in the temperature of the surface

Table 3
The result of reduction in residual stresses by the use of conventional cryogenic treatment presented by other researchers.

Alloy Sample dimension Measurement Reheating Maximum compressive as Maximum compressive after Residual stress Reference
(mm) technique medium quenched stress (MPa) cryogenic treatment (Mpa) reduction (%)

2014 50150300 Saw cut High velocity 96 20 79 [12]

7075 50150300 steam 138 28 80
7050 76150300 Crack compliance High velocity 220 45 80 [13]
steam
2014 178 X ray diffraction High velocity 290 41 86 [19]
7049 38 steam 131 28 77
6061 200 h200t10 Saw cut Boiling water 43.4 30.9 28 [20]
6061 50h50 X ray diffraction Boiling water 70.1 40.3 42 [21]
7050 40110220 X ray diffraction High velocity 315 91 75 [22]
steam
2024 252550 Hole drilling Hot oil 140 40 71 Present study

50
M. Araghchi et al.
Fig. 5. TEM images of 2024 aluminum alloy after dierent heat treatments, T6 heat treated sample, showing large, needle-like S precipitates, New cryogenic treatment used by hot oil,
showing small S precipitates (S precipitates are shown by black arrows).
and the core of the aluminum samples and this issue creates more
thermal strain on the surface. Hill et al. [12] have shown that the
greater dierence in temperature of surface and core results in more
reduction of residual stress. The high temperature of oil provides a high
temperature at the surface of the sample and cause decreases yield
strength and the elastic modulus. Hence plastic deformation initiates at
lower stresses and more strains will be induced.
Hot oil as a liquid medium can provide uniform heating for the
immersed sample. Hot oil makes all surfaces uniformly exposed to high
temperatures and all surfaces deform plastically. Another advantage of
the hot oil is its ease of application so that it requires no xtures and
special equipment. Moreover, the use of oil results in the reduction of
the time between bringing out the sample from the cooling to the
heating medium. So the process can be carried out faster compared to
high velocity steam and provides a higher temperature dierence.
Fig. 4 presents the engineering stressstrain curves of the samples
treated in cryogenic medium, hot oil and boiling water. For compar-
ison, the curves of QWNA (T4) and QWAA (T6) heat-treated samples
are given as well. Table 4 shows the mechanical properties of the
samples.
It has been seen that ultimate tensile strength (UTS) of the QWAA
(T6) sample is 506 MPa. It has increased by 10% and 15% and reaches
557 MPa and 581 MPa in the QWCA1 and QWCA24 sample, respec-
tively. Furthermore, the yield strength (YS) of the QWCA1 and
QWCA24 is 13.7% and 15.6% higher than that of QWAA (T6) sample,
respectively.
During cryogenic treatment, immersion in the heating medium
enhances plastic deformation in the sample. Subsequently, dislocation
density increases. In articial aging, precipitate nucleation mostly
occurs in dislocations, and it is heterogeneous [23,24]. Since, plastic
deformation provides more nucleation sites for precipitates, they are
ne and dispersed.
The use of boiling water as a reheating medium, cant cause the
dierence in temperature in the samples as much as hot oil. So, plastic
deformation is not the case. This is why the UTS of the QWBW24
sample has increased slightly as compared to the QWAA (T6) one. It
should be mentioned that in comparison with QWAA (T6), the
elongation of the QWCA24 sample is slightly reduce by only about
1.8%, indicating that the sample which undergo cryogenic treatment
process good combination of strength and ductility.
The hardness of heat treated sample given in Table 4. It shows that
the hardness of the QWNA (T4) is 74.6 HRB. Tis gure for articial
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Materials Science & Engineering A 689 (2017) 4852
aging one is 79.2 HRB. It increases to 83.3 HRB and 86.7 HRB for the
QWCA1 and QWCA24 samples, respectively. Using hot oil with a
temperature close to the aging temperature leads to an increase of
hardness from 79.2HRB to 86.7 HRB. Based on a previous study [25],
increasing the density of dislocations before articial aging enhances
the heterogeneous nucleation sites. Dislocations generate a dierent
path for the formation of the precipitates. The hardness of the sample
heat treated in boiling water is 81.1 HRB which shows no signicant.
Fig. 5(a) shows the QWAA (T6) heat-treated 2024 aluminum alloy,
showing that large needle-like S precipitates. Bagaryatsky [26] and
Silcock [27] have shown the following orientation relationship between
the precipitates and the aluminum matrix:
[100Al //[100]S(S); [021Al //[010]S(S); [012Al //[001]S(S).
They are considered to be non-shearable [28,29], and have a signicant
role in strength of QWAA (T6). The S phase is believed to preferen-
tially precipitate on dislocations. Therefore, it becomes ner distrib-
uted after cryogenic treatment, as shown in Fig. 5(b). The TEM
micrograph of the cryogenic treated sample indicates that the size of
S precipitates is smaller than that of the QWAA (T6) sample.
4. Conclusion
In the present work, a novel cryogenic treatment was used to reduce
the residual stresses in a 2024 aluminum alloy. In this context,
mechanical properties and microstructure of the heat treated samples
were studied as well. It was shown that:
(1) The use of hot oil in the novel cryogenic treatment compared to
high velocity steam can cause the process to be done without
special equipment and more applicable.
(2) This novel cryogenic treatment can reduce 71% of the residual
stress, higher than the traditional cryogenic treatment (uphill
quenching) in boiling water and similar to high velocity steam.
(3) The strength of the cryogenic treated sample increased about
75 MPa compared with T6 sample. So, this method not only
resulted in reduction of residual stresses, but also improved the
mechanical properties.
(4) Deformation during reheating in cryogenic treatment increased the
density of dislocation and subsequently provided preferential sites
for nucleation of S precipitates. Meanwhile, the S precipitates
were well distributed in the microstructure and their average size
was reduced.
M. Araghchi et al.
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