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Characterization of Material Properties of 2xxx

Series Al-Alloys by Non Destructive Testing
Techniques

Article in Journal of Nondestructive Evaluation · March 2011

DOI: 10.1007/s10921-011-0117-5

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J Nondestruct Eval
DOI 10.1007/s10921-011-0117-5

Characterization of Material Properties of 2xxx Series Al-Alloys

by Non Destructive Testing Techniques
Fawad Tariq · Nausheen Naz · Rasheed Ahmed Baloch ·
Faisal

Received: 28 March 2011 / Accepted: 18 October 2011

© Springer Science+Business Media, LLC 2011

Abstract 2xxx series Al-alloys are widely employed in
structural applications due to their good mechanical proper-
ties. During heat treatment of these alloys, solution treated
parts sometimes mixed with age hardened parts during han-
dling. This result in difficulty in distinguishing between so-
lution treated and aged parts of various grades. Moreover,
it is also necessary to separate improper aged parts from
properly treated parts. The traditional methods of charac-
terization of different heat treated parts are hardness, ten-
sion testing and microscopy, however these are destructive
in nature and sometimes not desired particularly for finished
products. The main purpose of this paper is characteriza-
tion of material properties of 2xxx series Al-alloys by eddy
current and ultrasonic NDE techniques so that the inspec-
tion can be carried out effectively in the shortest possible
time. Three wrought Al-alloys of 2xxx series (AA 2014,
AA 2024 and AA 2219) were homogenized followed by so-
lution heat treatment and age hardening treatments at spe-
cific temperatures for 1–16 h. The changes in hardness and
microstructure during heat treatments were determined by
traditional material characterization methods and then cor-
related with electrical conductivity, sound velocity and at-
tenuation coefficient obtained through Nondestructive Eval-
uation (NDE) techniques. Results demonstrated an excellent
correlation between hardness and sound velocity, whereas
extend of aging can be easily predicted by electrical con-
ductivity, and attenuation coefficient measurement. Investi-
gation suggested a way towards the non-destructive detec-
F. Tariq () · N. Naz · R.A. Baloch · Faisal
Materials Research and Testing Laboratory, Pakistan Space and
Upper Atmosphere Research Commission (SUPARCO),
Karachi 75270, Pakistan
e-mail: t_fawad@hotmail.com
tion and characterization of material properties when con-
ventional testing methods are not applicable.
Keywords AA 2024 · AA 2014 · AA 2219 · Aluminum
alloys · Precipitation hardening · Ultrasonic testing · Eddy
current testing
1 Introduction
Heat treatable aluminum alloys of 2xxx series (Al–Cu type)
are widely used for structural applications (particularly in
aerospace and automotive industry) at moderate service tem-
peratures due to their good strength-to-weight ratio and fa-
tigue resistance. The mechanical properties of such alloys
are obtained through precipitation (or more often called age
hardening) hardening phenomena wherein strength is in-
creased because of existence of an ordered precipitate struc-
ture. In solid solution, the alloying elements are completely
dissolved and the material behaves like a single-phase ma-
terial having low strength and hardness. During aging, the
alloying elements cluster and start forming different types
of small precipitates, depending on the aging temperature.
The precipitation sequence in Al–Cu–Mg–Si alloys is ex-
tensively studied by different researchers [1–6].
Theses alloys are usually used in peak hardened condi-
tion (i.e. mostly in T6 condition—solution heat treatment
followed by artificially aging). Mechanical properties and
microstructures obtained as a result of solution treatment
and aging are generally characterized and qualified by con-
ventional testing techniques like micro-hardness, tension
testing, optical or scanning electron microscopy, etc. How-
ever, these evaluation techniques are destructive in nature,
costly and time consuming. Furthermore, these tests are
usually carried out on ‘coupon samples’ assuming that the

coupon is the true representative of the component that will
go into service. The conventional ‘coupon based’ approach
of determining material properties may not be good enough
as there may be variation in the heat treatment seen by the
coupon and the component itself. Hence the results of de-
structive tests on coupons may not truly apply to the compo-
nent to be used in service. Also in service, when these alloys
are employed at temperatures in the range 130–170°C near
to those of the artificial aging treatment, aging processes
proceed causing over-aging of material (coarsening of pre-
cipitates) and deteriorating its mechanical properties such as
hardness and tensile strength [3]. Field characterization and
performance evaluation is also not possible using destructive
testing techniques. Therefore, there exists need for alternate
techniques such as nondestructive techniques for rapid and
cost-effective characterization and qualification of material
properties during production as well as in service.
Nondestructive evaluation (NDE) methods are most com-
monly employed for detection and characterization of de-
fects in the component; however they hold good poten-
tial to characterize mechanical properties and microstruc-
tures in materials [7–14]. In the past few decades numer-
ous attempts have been made by researchers to characterize
(i) metallurgical properties (like grain size [15–17], precip-
itation hardening reactions [18–20], phase change [21–23],
porosity [24, 25], weld microstructure, and defects [26, 27],
etc.), (ii) mechanical properties (like hardness, strength, im-
pact strength, fracture toughness, etc.) [28–33], (iii) thermo-
mechanical treatments during fabrication (like cold rolling,
hot deformation, etc.) [34–36] and (iv) service-induced
damage on components (like fatigue, creep, stress corrosion
cracking, hydrogen attack, etc.) [37–42], by conventional
testing techniques and correlate these with the parameters
(like electrical conductivity, sound velocity, sound attenua-
tion, etc.) obtained by NDE techniques (eddy current testing,
ultrasonic testing, acoustic emission testing, etc.).
Among many available Nondestructive Evaluation (NDE)
techniques, ultrasonic testing (UT) and eddy current testing
(ECT) are the most preferred, widely studied and employed
techniques for characterizing material properties. Both non-
destructive evaluation techniques offer distinct advantage in
that the material properties can be verified on actual com-
ponents of engineering structures. Moreover, being volu-
metric in nature, examination can give an idea about the
bulk material properties. Non-destructive evaluation by UT
is one promising method which has gained much interest
during recent years. Ultrasonic parameters (sound veloc-
ity and attenuation) are significantly affected by changes
in microstructural features or mechanical properties of ma-
terials [43]. Eddy current testing is another important non-
destructive evaluation technique used to quickly character-
ize materials, because eddy currents are influenced by mi-
crostructural alterations due to precipitates, cold work, de-
formation, etc. and the coil impedance or induced voltage in
J Nondestruct Eval
pick-up coil changes accordingly. The magnitude and phase
of induced voltage or impedance change are used to corre-
late with the microstructures and mechanical properties.
Extensive amount of work has been conducted on charac-
terizing properties of different Al-alloy grades non-destruc-
tively by UT and ECT [43–53]. However, there is little
published data available in literature on the relationship be-
tween the material properties and ECT and UT responses of
2xxx series Al-alloys as a result of aging treatments. Since
Al-alloys of 2xxx series are the most widely used alloys for
structural applications therefore the full potential of nonde-
structive evaluation techniques in these alloys is yet to be
realized. Therefore, in the present study an attempt is made
to establish a correlation between hardness and microstruc-
tures of wrought 2xxx series Al-alloys (AA 2014, AA 2024
and AA 2219) with electrical conductivity and acoustic pa-
rameters (velocity and attenuation) obtained through ECT
and UT respectively. It is envisaged that data present in this
study could be used to determine nondestructively, the hard-
ness (or strength) of the 2xxx series Al-alloy grades as well
as the unknown thermal history of a given component before
putting the component to service.
2 Experimental Work
2.1 Material
The materials used in this research work were wrought heat
treatable 2xxx series Al-alloys. Three grades were selected
for investigation: (i) AA 2014 (Al–Cu–Si), (ii) AA 2024
(Al–Cu) and (iii) AA 2219 (Al–Cu–Mn). Spectroscopic
analysis of all grades was carried out using optical arc emis-
sion spectrometer and the elemental composition is given in
Table 1.
2.2 Heat Treatment
All the grades were initially in the form of plates and forged
bars. Square samples of about 25 × 25 × 20 mm size and
round samples of about 50 mm diameter and 25 mm thick-
ness were cut perpendicular to the rolling direction from
plates and bars respectively. Samples of all three grades
were homogenized at particular temperature and time (heat
treatment schedule is listed in Table 2) and slowly cooled
in furnace to obtain a uniform reference microstructure.
Samples were then solution heat treated (SHT) to dissolve
all precipitates followed by quenching in water at ambient
temperature to obtain supersaturated solid solution (see Ta-
ble 2). Following the SHT, the samples were artificially aged
at specified temperature (corresponding to T6 temper) of
each grade for different duration ranging from 1–16 h and
water quenched to cease further aging reaction. The aged
J Nondestruct Eval

Table 1 Average elemental

composition of 2xxx series Grade Cu Si Zn Mg Mn Fe Cr Al
Al-alloy grades used in this
study AA 2014 3.95 0.62 0.089 0.48 0.80 0.20 – Bal.
AA 2024 3.50 0.35 0.041 0.55 0.54 0.35 0.035 Bal.
AA 2219 5.35 0.20 0.022 0.006 0.25 0.40 0.003 Bal.

Table 2 Heat treatment cycle

conducted on 2xxx series Grade Homogenization → Solution heat treatment → Age hardening → water
Al-alloy grades furnace cooled water quenched quenched
Temperature Time Temperature Time Temperature Time
(°C) (h) (°C) (h) (°C) (h)

AA 2014 497 8 500 2 165 1–16

AA 2024 490 8 490 2 190 1–16
AA 2219 525 8 530 2 185 1–16

specimens were kept at −5°C in refrigerator to inhibit fur-
ther aging. Homogenization and SHT was done in electric
resistance-type heat treatment furnace and age hardening
treatments were done in heating oven. The temperature vari-
ation was kept within ±3°C.
2.3 Macrohardness
Hardness measurement was performed on flat, prepared sur-
face by Macro-Vicker hardness tester at 10 kg load and 10 s
dwell time. At least five measurements were taken for each
condition and average result is quoted in this work. The
maximum scatter in the hardness measurements was found
to be less than ±3 HV.
2.4 Microstructural Examination
Metallographic samples of all three grades in solution
treated and aged conditions were prepared by adopting stan-
dard grinding and polishing techniques. Observations were
made after etching with modified HF solution (10 ml HF +
90 ml H2 O + adding MoO3 up to saturation). Microstruc-
tural examinations were carried out using optical micro-
scope incorporated with image analyzing software and scan-
ning electron microscope equipped with energy dispersive
spectrometer (EDS).
2.5 Electrical Conductivity Measurement
Eddy current testing technique was used for calculation of
electrical conductivity of the materials in all heat treated
conditions. Electrical conductivity was measured on ground
and polished samples as per ASTM standard E 1004-94
using portable Locater 3s eddy current equipment capa-
ble of operation in frequency range of 10 Hz to 10 MHz.
500 kHz electrical conductivity measuring probe (5/16 inch
diameter, suitable for non-ferrous metals and alloys) was
used for all measurements. Change in electrical conductivity
was measured at room temperature in terms of percentage
of international annealed copper standard (%IACS). Before
conducting electrical conductivity test, equipment was cal-
ibrated on standards of known conductivity. The measured
values were considered to be accurate within ±0.5%IACS.
Five readings were taken of each sample and then average
value was used for plotting the graph of electrical conduc-
tivity verses aging temperature.
2.6 Sound Velocity Measurement
Longitudinal sound velocity was measured by using
Krautkramer USM-25S LEMO ultrasonic flaw detector as
per ASTM standard E 494-99. The calibration standard
block V1 was used for calibration of equipment. The sound
velocity was calculated by Pulse-echo method. Both 2 MHz
and 4 MHz longitudinal beam probes were used to measure
sound velocity. Filtered machine oil was used as the cou-
plant for the longitudinal wave probes and a constant force
was applied on the probes to obtain a stable thickness of the
coupling film. For achieving the highest possible accuracy,
the specimens were carefully machined and polished to have
smooth, flat and parallel surfaces. The plane parallelism be-
tween the two opposite faces of the sample was checked
using a surface plate and a dial gauge. The thickness of spec-
imens was measured with an error of ±0.001 mm and the
scatter in ultrasonic velocities was within ±3 m/s. The accu-
racy of the measurement is largely depends on the accuracy
with which the thickness of the component is measured.
Moreover, temperature also affects the velocity of sound;
therefore all the measurements were carried out at almost
same temperature. The mean values for the velocities were
obtained by averaging the five independent measurements.
In addition to sound velocity, attenuation co-efficient (α)

Fig. 1 Graphs of (a) hardness, (b) electrical conductivity, (c) longitudinal sound velocity, and (d) attenuation coefficient with respect to aging
time at 165°C for AA 2014 grade
was also calculated by finding the amplitude difference (dB)
between the two back-surface signals and then dividing it
by the total path traveled (thickness of sample in this case).
Attenuation co-efficient (α) is expressed in terms of dB/mm.
3 Analysis of Results and Discussion
3.1 AA 2014 (Al–Cu–Mg–Mn)
Response of age hardening treatments on hardness, elec-
trical conductivity, longitudinal sound velocity and attenu-
ation coefficient are plotted on graph as shown in Fig. 1.
The variation in hardness with aging time exhibited different
peaks corresponding to the precipitation of different phases,
as shown in Fig. 1a. The existence of typical precipitation
sequence is evident in aging curve (Fig. 1a). Sudden rise in
J Nondestruct Eval
hardness (from solution treated condition i.e. 105 HV) was
seen upon artificial aging up to 4 h which was attributed to
the formation of GP I zone (coherent with the matrix). Fur-
ther aging between 4–12 h resulted in more hardness incre-
ment and peak hardness of about 150 HV was approached
in 12 h. Precipitation of second phase θ  (GP II zone) and
θ  particles (metastable) having definite crystal structure are
responsible for peak hardness in this alloy. Aging for longer
time periods i.e. above 12 h have resulted in gradual decline
in hardness curve due to over-aging. Material gets soft be-
cause of either precipitation of in-coherent stable precipi-
tates (equilibrium θ phase formed and coherency strain is
lost) or coarsening of already precipitated particles. With
continued aging at any given temperature, there is tendency
for the small particles to dissolve and the resultant solute to
precipitate on larger particles causing them to grow, thereby
J Nondestruct Eval
lowering the total interfacial energy. This process is termed
as particle-coarsening or sometimes Ostwald ripening.
The actual concurrent sequence of precipitation in 2xxx
series Al–Cu–(Mg–Mn) alloys strongly depends on rela-
tive amount of alloying elements, history of the material in-
cluding production methods (rolling, forging, etc.), quench-
ing conditions, natural aging and further heat treatments.
Various authors have discussed the possible sequences of
precipitation in Al–Cu, Al–Cu–Mg and Al–Cu–Mg–Mn al-
loys [1–6].
(1) α ss → GPZ (Cu-rich phase) → θ  (metastable) → θ 
(metastable with definite crystal structure) → θ (CuAl2 -
stable)
(2) α ss → GPZ (Cu-rich phase) → GPZ II (Cu-rich phase)
or S (metastable) → S (metastable) → S (CuMgAl2 -
stable)
(3) α ss → GPZ (Cu-rich phase) → Q (metastable) → Q
(Cu2 Mg8 Si6 Al5 or Al4 Cu2 Mg8 Si7 -stable )
The change in electrical conductivity (in terms of %
IACS) in response to artificial aging is presented in Fig. 1b.
The variation in the electrical conductivity with aging is
complex and results from a number of contributions includ-
ing changes in the scattering of electrons. The change was
not perfectly linear i.e. electrical conductivity increases with
increasing aging time but the curve does not highlights dif-
ferent precipitation stages, which are clearly visible in hard-
ness curve (Fig. 1a). Electrical conductivity decreases af-
ter 12 h aging which reflects the onset of over-aging. Elec-
trical conductivity measurements cannot, in principle, dif-
ferentiate between GP zones since changes in conductivity
are determined more by the number and size of the scatter-
ing centers than by their crystal structure or degree of co-
herency with Al-matrix. Same phenomenon was observed
here that the GP zones are not revealed by the electrical con-
ductivity measurement however the formation of intermedi-
ate phases (coherent θ  and semi-coherent θ  phases) are de-
tected (Fig. 1b). The increase in conductivity with increasing
aging time was thought to be the result of purification of the
matrix by means of segregation of the solute atoms and for-
mation of semi-coherent metastable phases. As the rate of
precipitation was accelerated, the foreign atoms that act as
scattering centers of electrons segregate from the aluminum
matrix at an enhanced rate. Electrical conductivity level be-
comes lower when the concentration of solute atoms in solid
solution increases, while it becomes higher when the alloy-
ing elements are precipitated out. The electrical conductivity
is therefore largely influenced by the amount of alloying el-
ements in the solid solution (Al matrix) and the amount and
nature of precipitates. Equilibrium θ precipitates are coarser
and their size increases as aging proceeds above 12 h, thus
minimizing their scattering effect. Therefore, reduction in
electrical conductivity in over-aged samples was recorded.
The relationship observed between electrical conductivity
and aging treatments was in agreement with the previous
work on Al–Cu alloys [44, 54].
Figure 1c depicts the change in longitudinal sound veloc-
ity as a function of aging time. The plot shows that the sound
velocity (measured by both 2 MHz and 4 MHz probes) in-
creases non-monotonically in the same way as hardness in-
creases. Moreover, the precipitation of different phase can
be distinguished by different peaks in sound velocity values.
Increase in velocity during initial stages of aging was at-
tributed to the increase in the elastic modulus of the matrix
due to the depletion of solute element (Cu) from the matrix
during precipitation of θ  and θ  phases. Maximum velocity
was detected for 12 h aged samples. This value corresponds
to the peak hardness condition. The decrease in velocity val-
ues above 12 h aging was attributed to loss of coherency
strain and precipitates coarsening i.e. over-aging. The re-
sults illustrated a quite good correlation between hardness
and longitudinal sound velocity with degree of age harden-
ing. The observations of results also suggest that the sound
velocity obtained from 4 MHz probe could be more reliable
than 2 MHz probe. Same trend of sound velocity with age
hardening treatments (i.e. increase in sound with hardness)
was also quoted earlier by other authors [18, 19]. The sound
wave velocity in solids is in fact related to elastic modu-
lus of the material, which in turns change with age hard-
ening because of change in matrix composition and pre-
cipitation of different phases. The increase in the sound
velocity with aging is attributed to the increased volume
fraction of precipitates (which results in reduction in the
distortion in the crystal lattice), which contribute to the in-
creased elastic modulus and hardness of the aged speci-
men [18]. However, in overaged condition (i.e. incoherent
matrix-precipitate interface exists); the loss of coherency
strain leads to decrease in the elastic modulus of the inter-
face and therefore reduces the effective ultrasonic velocity
of the material. Hence the ultrasonic velocity monitored dur-
ing age hardening process would provide insight into the ki-
netics of precipitate formation and their growth/dissolution.
These ultrasonic velocity observations have been substanti-
ated with micro-examination results discussed in upcoming
paragraphs.
The variation in attenuation coefficient (α) with increas-
ing aging duration is illustrated graphically in Fig. 1d. It is
observed that the attenuation measured with 4 MHz probe
increases linearly with increasing time of aging. Attenua-
tion in longitudinal sound waves followed the same trend as
that of hardness in response to aging. Moreover, attenuation
coefficient measured with 4 MHz probe leads better results
than 2 MHz probe. This is because the ultrasonic waves at
high frequencies have relatively shorter wavelengths, and
hence, the ultrasonic waves become sensitive to fine pre-
cipitates and are expected to interact more strongly with

Fig. 2 Showing correlation of hardness with (a) electrical conductivity, (b) longitudinal sound velocity (from 4 MHz probe), and (c) attenuation
coefficient (from 4 MHz probe)
them. Ultrasonic energy is attenuated as the wave propagates
through a material due to scattering and absorption. Absorp-
tion, which is caused by microstructural defects such as dis-
location and point defect, takes only small part of the mea-
sured attenuation in metallic materials and usually assumed
to be negligible [55]. The increase of ultrasonic attenuation
with aging seems to be related to the precipitation of various
phases (which act as scattering points) in the microstructure.
The precipitation of second phase particles from the ma-
trix and coarsening of second phase particles with different
acoustic impedance from the matrix is reported to increase
ultrasonic scattering [56, 57]. As aging proceeds, the forma-
tion of precipitates (having different impedance than matrix)
J Nondestruct Eval
occurs which acts as source of scattering in path of propagat-
ing sound waves. Coarsening of precipitates in the overaged
condition also increases scattering of waves so the attenua-
tion values further increased. It is known that the attenuation
depends upon the size of the substructure of the grains (like
martensite platelets in hardened steel) divisions [58]. Hence
the increase in particle size during over-aging will appar-
ently increase attenuation in sound waves.
Hardness values (up to peak hardness condition i.e. 12 h
aging) were correlated with electrical conductivity, longitu-
dinal sound velocity and attenuation coefficient in Fig. 2.
The solid line in Fig. 2 represents the least square best-fit
line to the data. Figure 2a shows good relationship between
J Nondestruct Eval
Fig. 3 Optical micrographs of
AA 2014 in (a) solution treated
condition and (b) after 8 h aging
Fig. 4 SEM photos of AA 2014
taken after (a) 5 h aging and
(b) 12 h aging
hardness and electrical conductivity with a correlation coef-
ficient, R 2 of about 0.97 calculated using 2nd order polyno-
mial fit. Graph between hardness and sound velocity showed
a remarkable linear relationship with correlation coefficient
of about 0.98 (Fig. 2b). This indicates that an excellent cor-
relation is existed between hardness and velocity, and hard-
ness could be predicted more accurately by measuring sound
velocity. However, the graph between hardness and atten-
uation coefficient was non-linear and the polynomial line
is best fitted with the R 2 value of 0.83 which depicts pro-
nounced scatter in values, as shown in Fig. 2c.
The changes in microstructure from SHT condition to
peak hardened condition in response to aging time can be
seen in Fig. 3. The micrograph of SHT sample (Fig. 3a)
shows fine re-crystallized grain structure of AA 2014 grade
of Al-alloy consisting of α matrix (Al-rich) within which
black insoluble coarse particles of AlMgCu and AlMnCu-
types (also containing Fe as determined by energy disper-
sive spectroscopy) are present. These intermetallic particles
were elongated in the flow direction and were not soluble at
solution treatment temperature. Undissolved CuAl2 precip-
itates (white, outlined) are also visible in the structure. Dur-
ing quenching from SHT temperature, GP zones are formed
in Al–Cu type alloys which are so fine that they could not
be resolved by optical microscope. The large black particles
are rosette formed by eutectic melting above the solution an-
nealing temperature. The strain lines are also seen in Fig. 3a.
No significant precipitation was observed in the structure
upon artificial aging at 165°C for 5 h. However, less vol-
ume of CuAl2 intergranular particles was present. Precipi-
tates were also found on grain boundaries. Figure 3b shows
the micrograph of sample aged for 8 h consisting primarily
of re-crystallized grains with intergranular and intragranu-
lar precipitation of coherent θ  or semi-coherent θ  phases.
Strain line and grain contrast was also evident in the struc-
ture. High density of fine precipitates (probably θ  and θ  )
uniformly dispersed throughout the structure was observed
in the 12 h aged sample. The fine dispersion of strength-
ening precipitates (coherent and semi-coherent) is responsi-
ble for higher hardness of the material. In alloys such as the
AA 2014, the high copper content (about 4% by wt.) assures
the presence of θ precipitation sequence, generally observed
for Cu greater than 0.2–0.5 wt.%. Aging above 12 h caused
formation of equilibrium θ (CuAl2 ) phase which was inco-
herent with the matrix and over-aging occurred.
Figure 4 presents the selected high magnification SEM
pictures of the AA 2014 samples. Microstructure of 5 h aged
sample did not reveal any appreciable precipitation; only in-
soluble particles were found at grain boundaries, as shown
in Fig. 4a. The almost clear grains showed that the zones
were dissolved and replaced by coherent fine strengthening
precipitates (mostly θ  and relatively low amount of θ  ) dis-
tributed evenly in the matrix. Although significant hardness
was achieved after 5 h aging, but the precipitates were rather
so fine that they were not resolved by SEM. Figure 4b cor-
responds to the high magnification micrograph of 12 h aged
sample that was artificially aged to peak hardness. Fine pre-
cipitates (shown with arrow in Fig. 4b) found to be evenly
distributed throughout the structure; both within grains and
at grain boundaries.
3.2 AA 2024 (Al–Cu)
Variation in hardness, electrical conductivity, longitudinal
sound velocity and attenuation coefficient for AA 2024

Fig. 5 Graphs of (a) hardness, (b) electrical conductivity, (c) longitudinal sound velocity, and (d) attenuation coefficient with respect to aging
time at 190°C for AA 2024 grade
grade as a function of aging time is presented in Fig. 5.
A little dissimilar trend in hardness increment was found in
AA 2024 grade upon aging which was primarily due to dif-
ferent chemical composition than AA 2014 grade and sec-
ondary due to higher aging temperature (i.e. 190°C as com-
pared to 165°C for AA 2014 grade) employed. It is well
known that when the Cu content is high and the aging tem-
perature low, the sequence of stages followed is GP I zone,
GP II zone, θ  and θ (CuAl2 ). On aging at higher tempera-
tures, however, one or more of these intermediate stages may
be surpassed. In Fig. 5a typical non-monotonic increase in
hardness was observed with increasing aging duration. From
83 HV in SHT condition, hardness rapidly rises to 105 HV
within 2 h and then becomes steady in between 2–4 h, as
J Nondestruct Eval
seen in Fig. 5a. Hardness then continuously increased with
increasing aging time up to 8 h and then becomes almost
constant. Peak hardness of about 144 HV was achieved af-
ter 13 h of aging. Aging above 13 h caused decline in curve
which reflects over-aging. Preliminary increase in hardness
up to 2 h was attributed to precipitation of GP zones. Straight
region between 2–4 h, in which hardness was almost stable,
was thought to be due to dissolution of GP zones and for-
mation of intermediate phases. Further increase in hardness
up to peak condition was because of precipitation of tran-
sition metastable phases. These transition phases are either
fully or partially coherent with the matrix and are actually
responsible for hardening. Aging above 13 h resulted in re-
duction in hardness due to precipitation of in-coherent equi-
J Nondestruct Eval
librium precipitates (i.e. over-aging occurred), as shown in
Fig. 5a.
Figure 5b shows graph of electrical conductivity with ag-
ing time, presenting a continuous rise in conductivity with
aging time up to 14 h and then drops above it. Similar behav-
ior was observed in hardness with aging duration. However,
an interesting feature about electrical conductivity curve was
the presence of different peaks which corresponds to differ-
ent stages of precipitations. All these stages were not being
detected in hardness curve as shown in Fig. 5a. Similar trend
in electrical conductivity with aging treatments was also re-
ported earlier [44, 54, 59]. It was thus observed that progress
of aging and precipitation sequence can be monitored with
electrical conductivity measurements.
Figure 5c shows variation in sound velocity (from both
2 MHz and 4 MHz longitudinal wave probes) with aging
time. Similar trend in velocity was noticed as that for elec-
trical conductivity. Both sound wave velocity and hardness
increase to a certain peak value and then decrease on over-
aging. For any given aging time, it was observed that the
ultrasonic velocity at 4 MHz was higher than that at 2 MHz.
Furthermore, the peak velocity was observed at 12 h aging
(Fig. 5c). Existence of various peaks in sound velocity curve
confirmed the concurrent precipitation of different phases.
Moreover, the velocities curve showed that the actual onset
of over-aging was at 12 h, wherein coherent precipitates be-
gin losing their coherencies and coarsening of precipitates
started. The differences in sound velocity during aging arise
primarily from the differences in the elastic modulus of the
phases and precipitate/matrix interface which are in turn af-
fected by the degree of lattice distortion caused by the pre-
cipitate. The variation in velocity values with aging treat-
ments were very well correlated with hardness and electrical
conductivity and are in close agreement with the findings of
other researchers [19, 57].
Results of attenuation coefficient measurement showed
linear relationship with aging time i.e. attenuation in sound
waves increases with aging time up to 16 h (Fig. 5d). Atten-
uation kept increasing without any drop; even in overaged
condition. Similar behavior in attenuation coefficient was
also found in AA 2014 grade, as shown in Fig. 1d. The rea-
son for this was already discussed in preceding paragraphs.
It was also noted that the high frequency probe leads better
results than low frequency probe. The occurrence of con-
temporaneous peaks in both hardness and ultrasonic attenu-
ation provides the experimental evidence of the suitability of
using ultrasonic testing for characterizing precipitation pro-
cesses in Al–Cu alloys. However, the occurrence of peaks
in attenuation coefficient curve depends also on the type,
volume fraction and average distribution of the precipitate
size in the structure. From the results, it was cleared that
the onset of over-aging can not be detected by the attenua-
tion coefficient measurement for most cases. This continu-
ous increase in attenuation with aging of Al–Li and Al–Cu
alloys was also pointed out by others [50, 60]. Sound ve-
locity seems to be more reliable parameter and could eas-
ily predict all stages of precipitation including over-aging.
But accurate sound velocity measurement demands highly
prepared polished surface. It was observed that the slight
changes in test temperature, surface preparation/conditions,
thickness variation in sample, and coupling conditions could
lead to large scatter in the results.
Figure 6 illustrates the relationship of hardness with elec-
trical conductivity, sound velocity and attenuation coeffi-
cient. Linear relationship of hardness (up to peak hardness
condition i.e. 14 h aging) with correlation coefficient of 0.97
was calculated for longitudinal sound velocity (Fig. 6b).
Whereas, hardness data was correlated with electrical con-
ductivity and attenuation coefficient by least square best-
fit method using 2nd order polynomial function, shown in
Figs. 6a and 6c. It was observed that sound velocity corre-
lated more perfectly than any other parameter and could be
used for hardness prediction with reasonable accuracy and
high confidence level.
Figure 7 shows the microstructural changes in AA 2024
grade in response to aging treatments. Solution treated struc-
ture mainly consisted of Al-rich matrix having equiaxed
grains with intergranular and intragranular spehoidized in-
soluble intermetallics, as seen in Fig. 7a. These large black
particles were found to be CuMgAl2 , Cu2 MnAl20 and
CuFeAl7 by energy dispersive spectroscopic analysis. Pre-
cipitation of CuAl2 particles was less because of proper so-
lution treatment; Cu was mostly dissolved in solid solution.
Slight change in structure was seen in 4 h aged samples.
Structure consisted of uniform distribution of precipitates
throughout the matrix; however individual precipitates were
on very fine scale and therefore not resolved by optical mi-
croscope. After 4 h aging, GP zones were thought to be
completely dissolved and replaced by intermediate phases of
definite crystal structure. High density of precipitation was
observed in the spotted structure after 12 h of aging; respon-
sible for high hardness. Fine coherent and semi-coherent
precipitates were uniformly distributed throughout the ma-
trix. Figure 7b corresponds to the microstructure after 14 h
aging. Precipitates were relatively coarser; this illustrated
the onset of over-aging. The fine precipitates dissolved (to
lower total interfacial energy) in favor of coarse equilibrium
precipitates. These equilibrium precipitates are incoherent
with the matrix and their formation always leads to soften-
ing (also confirmed from hardness, electrical conductivity
and sound velocity results), since coherency strains disap-
pear. Precipitation free zones (PFZ) were also observed in
the structure (Fig. 7b). These zones were formed as a con-
sequence of solute atom (Cu) depletion from the adjoining
areas of the grain boundaries.
Detailed microstructural analysis by SEM also con-
firmed the various stages of precipitation during aging. SEM
 J Nondestruct Eval

Fig. 6 Showing correlation of hardness with (a) electrical conductivity, (b) longitudinal sound velocity (from 4 MHz probe), and (c) attenuation
coefficient (from 4 MHz probe)

Fig. 7 Optical micrographs of

AA 2024 in (a) solution treated
condition and (b) after 14 h
aging
J Nondestruct Eval
Fig. 8 SEM photos of AA 2024
taken after (a) 9 h aging and
(b) 14 h aging (rectangular box
in picture shows magnified
view)
Pictures of only few selected samples are presented here
(Fig. 8). Microstructure of 9 h aged sample is shown in
Fig. 8a. Even dispersion of fine precipitates (black dots
shown with arrow) is visible in the structure. Microstruc-
ture of sample aged for 14 h is shown in Fig. 8b. It was
viewed that the precipitates grew on longer aging times i.e.
over-aging had occurred. Coarse precipitates (indicated with
arrow) were evident in the magnified view of the selected re-
gion in Fig. 8b.
Microstructural changes and occurrence of different pre-
cipitation stages during aging were confirmed from both
optical and scanning electron microscope results and these
changes were very well correlated with the hardness, elec-
trical conductivity and ultrasonic parameters.
3.3 AA 2219 (Al–Cu–Mn)
The effect of artificial aging time up to 16 h at fixed temper-
ature (i.e. 185°C) on hardness, electrical conductivity and
ultrasonic parameters of AA 2219 grade are graphically de-
picted in Fig. 9. Increase in hardness was observed with in-
creasing aging time, as seen in Fig. 9a. Hardness increment
with aging time in AA 2219 grade was almost similar to that
observed in AA 2024 grade (Fig. 5a) because both grades
were very close in chemical composition except Cu con-
tent (about 5.35% in AA 2219 grade as compare to 3.50%
in AA 2024 grade). Initially, aging up to 4–5 h resulted in
marked rise in hardness up to 128 HV. The hardness was al-
most stable in between 5–12 h and then again increase upon
aging to 12–14 h. Peak hardness of about 138 HV was at-
tained after 14 h of aging. Decline in hardness curve was
registered for aging above 14 h owing to overaging.
Electrical conductivity results showed continuous in-
crease in conductivity with increasing aging duration up to
14 h and then drops on further aging (Fig. 9b). It was ob-
served that electrical conductivity values were not stable in
between 5–12 h aging as in hardness curve; instead they
keep increasing and this trend was attributed to continu-
ous depletion of solute elements from the Al matrix with
subsequent formation of precipitates. This causes purifica-
tion of Al-rich matrix. It is well known fact that all metallic
additions to Al reduce its electrical conductivity, and elec-
trical conductivity increases when these elements precipi-
tate out of the solution. Moreover, continuous change in lat-
tice distortion due to matrix/precipitate interface, precipitate
sizes, morphology and distribution within the matrix also
cause change in conductivity. Steps in conductivity curve
exhibited the stages of precipitation (i.e. formation and dis-
solution of GP zones, precipitation of metastable transition
phases, and precipitation of equilibrium particles and their
coarsening). Similar electrical conductivity response with
aging time was also observed in AA 2024 grade (Fig. 5b).
Figure 9c shows prominent variations in longitudinal
sound wave velocity with aging treatments and it was ob-
served that the sound velocity varies in the same manner
as the hardness upon aging. Different stages of precipita-
tion were distinguished from different peaks in sound veloc-
ity curve. Similar dependence of sound velocity on elastic
modulus and hardness (which in turns depends upon precip-
itation process) during aging of AA 2219 grade was stated
by other researchers [20]. It was thus confirmed that good
correlation exists between hardness and longitudinal sound
velocity for AA 2219 grade.
Changes evolved during aging of AA 2219 grade were
also monitored in terms of attenuation coefficient as shown
in Fig. 9d. It was observed in Fig. 9d that attenuation co-
efficient measured with 4 MHz probe varied linearly with
aging time. Similar tendency in attenuation coefficient (i.e.
increase with increasing aging time) was already seen in
Fig. 5d for AA 2024 grade. However, results obtained from
2 MHz probe showed large scatter in the readings and were
therefore not meaningful.
Relationship of hardness data with electrical conductiv-
ity, sound velocity and attenuation coefficient was plotted
and linear as well as 2nd order polynomial regression was
calculated using least square fit method, as shown in Fig. 10.
From Fig. 10a, it was clearly seen that the data was quite
scattered and relatively weak relationship existed among
hardness and electrical conductivity (R 2 of about 0.73). It
was observed that towards the highest values of hardness,
the electrical conductivity shows rapid increase without any
appreciable increase in hardness. This trend was obvious in
all three alloys (Figs. 2a and 6a). This is in the regime where
the incoherent precipitates are forming. Precipitates of such
phases do not increase the hardness but increase the elec-
trical conductivity. Distinct positive correlation was existed

Fig. 9 Graphs of (a) hardness, (b) electrical conductivity, (c) longitudinal sound velocity, and (d) attenuation coefficient with respect to aging
time at 185°C for AA 2219 grade
(R 2 of 0.96) between the hardness and longitudinal sound
velocity (Fig. 10b). Correlation coefficient R 2 of about 0.85
was obtained between hardness and attenuation coefficient
through 2nd order polynomial fit, as seen in Fig. 10c. The
analysis of results suggested a rational correlation between
hardness and ultrasound velocity, whereas other parameters
are weakly related with hardness.
Figure 11 shows the optical micrographs of AA 2219
grade taken after different thermal treatments. The basic
trend in microstructural evolution during aging treatments
was almost same as that observed in AA 2024 grade. Fig-
ure 11a shows typical structure in solution treated condi-
tion containing large amount of insoluble intermetallics dis-
tributed all over the matrix. Grain boundaries were not re-
vealed in the micrograph (Fig. 11a). Significant alteration in
microstructure was observed in 5 h aged sample (Fig. 11b).
Darkish mottled appearance was indicative of precipitations
J Nondestruct Eval
of transition phases. Precipitation of transition phases was
also confirmed from hardness value i.e. 128 HV. Moreover,
precipitates were seen segregated at various locations. Sol-
uble CuAl2 particles (white outlined) were also visible in
Fig. 11b. Prolonged aging (up to 16 h) resulted in over-aging
of the structure; precipitates become incoherent and coarse.
Scanning electron micrographs of AA 2219 grade sam-
ples in aged conditions are displayed in Fig. 12. Change
in microstructure after 5 h of aging is shown in Fig. 12a.
This change in structure was attributed to precipitation of
intermediate phases responsible for significant increase in
hardness. High magnification micrograph of 13 h aged sam-
ple revealed high density of precipitates evenly distributed
throughout the matrix, as shown in Fig. 12b. This struc-
ture corresponds to peak hardness condition (138 HV). Rela-
tively large volume fraction of precipitates (probably coher-
ent θ  and mostly semi-coherent θ  , shown with arrow) in
J Nondestruct Eval

Fig. 10 Showing correlation of hardness with (a) electrical conductivity, (b) longitudinal sound velocity (from 4 MHz probe), and (c) attenuation
coefficient (from 4 MHz probe)

Fig. 11 Optical micrographs of

AA 2219 in (a) solution treated
condition and (b) after 5 h aging
 J Nondestruct Eval

Fig. 12 SEM photos of AA 2219 taken after (a) 5 h aging, (b) 13 h aging and (c) 16 h aging (rectangular box in picture shows magnified view)

Table 3 Showing the

consolidated list of different Test parameters AA 2014 AA 2024 AA 2219
parameters for the investigated
three Al-alloy grades Peak hardness (HV) 150 144 138
Aging time to achieve peak hardness (h) 12 13 14
Electrical conductivity (%IACS) (at peak hardness) 35.85 37.85 41.60
Longitudinal sound velocity (m/s) at 4 MHz (at peak 6422 6400 6354
hardness)
Attenuation coefficient (db/mm) at 4 MHz (at peak 0.055 0.0639 0.046
hardness)
Correlation between hardness and electrical 0.97 0.94 0.73
conductivity (R 2 )
Correlation between hardness and sound velocity (R 2 ) 0.98 0.97 0.96
Correlation between hardness and attenuation 0.83 0.95 0.85
coefficient (R 2 )

the structure was the outcome of higher aging temperature.
Aging above 14 h caused particle growth and coarsening
with subsequent decrease in hardness (about 127 HV in 16 h
aged sample), as seen in Fig. 12c. Coarse precipitates (prob-
ably semi-coherent θ  and equilibrium θ ) are clearly visible
(shown with arrow) in magnified view in Fig. 12c. The mi-
crostructural modifications during aging examined by mi-
croscopy are in conformance with the results of hardness
measurements, electrical conductivity and ultrasonic param-
eters.
Analysis of results and discussion firmly suggested that
excellent correlation existed between hardness and longi-
tudinal sound velocity obtained from 4 MHz probe for all
the three grades of 2xxx series investigated and the linear
fit obtained show good promise in identifying any particu-
lar microstructure for a given ultrasonic velocity/hardness
(Table 3). Quite good relationship (using polynomial fit)
was found between hardness and electrical conductivity for
AA 2014 and AA 2024 grades. However, relatively weak
relationship was existed between hardness and attenuation
coefficient for AA 2014 and AA 2219. But, electrical con-
ductivity and attenuation coefficient could be helpful in pre-
dicting microstructural evolution during aging treatments;
since they can reveal different stages of precipitation. Fur-
thermore, ultrasonic velocity was found to be more effective
measure of hardness than attenuation coefficient because on-
set of over-aging could not be detected from attenuation
change. The change in hardness with aging time was also
confirmed from microstructural examination. Thus, progress
of aging treatments and resulting material properties (mainly
hardness) could be successfully and non-destructively mon-
itored and assessed by simultaneous combination of eddy
current and ultrasonic nondestructive evaluation techniques.
4 Conclusions
The possibility and effectiveness of characterizing material
properties of 2xxx series Al-alloys as a result of age harden-
ing treatments, by eddy current and ultrasonic nondestruc-
tive evaluation techniques, was evaluated in this study. The
results and discussion of this work can be summarized as
follows:
1. Samples of three Al–Cu alloy grades were homogenized
and solution treated followed by artificial aging at known
fixed temperature for varying time durations (1–16 h) to
disclose different stages of precipitation.
2. Hardness measurements showed continuous, non-mono-
tonic increase in hardness in response to aging treatments
for all three Al-alloys. Upon initial aging, sudden rise in
J Nondestruct Eval
hardness was observed which was attributed to the for-
mation of GP zones coherent with the matrix. Slight de-
crease in hardness after few 2–4 h of aging was due to
dissolution of GP zones. Hardness kept increasing till a
peak value was attained at certain aging time. The peak
hardness condition is known to be due to precipitation of
coherent and semi-coherent metastable precipitates. Ag-
ing for longer times above 12–14 h resulted in decrease in
hardness due to dissolution and formation of incoherent
precipitates and their coarsening.
3. Electrical conductivity measurement results of all three
Al-alloys exhibited a linear trend that is conductivity
increased with aging time up to peak hardness condi-
tion. Further aging above peak hardness resulted in de-
crease in conductivity which proved the over-aging of
the structure. Moreover, in most cases the multi-step pre-
cipitation sequence can be easily detected by monitoring
various steps in electrical conductivity values. Hence, it
was demonstrated that a good correlation exists between
progress of aging and electrical conductivity.
4. Longitudinal sound velocity and attenuation coefficient
was measured in all aged samples by 2 MHz and 4 MHz
probes. Sound velocity and attenuation coefficient was
found increasing with increasing aging duration and fol-
lows the same trend as that of hardness. The different
stages of precipitation were also clearly revealed by dif-
ferent steps in sound velocities and attenuation. Ultra-
sonic velocity decreases with decrease in hardness upon
over-aging; but attenuation coefficient value keep in-
creasing. Hence onset of over-aging can only be detected
by sound velocity. Better relationship was observed be-
tween ultrasonic parameters, hardness and microstruc-
tural change when the velocity and attenuation were mea-
sured by high frequency (4 MHz) probe. Study carried
out to correlate ultrasonic parameters (velocity and at-
tenuation coefficient) with the degree of age hardening in
2xxx series Al-alloys has shown excellent results. More-
over the results were in good agreement with the pre-
vious work of other researchers. It was established that
both sound velocity and attenuation coefficient could be
used to characterized precipitation hardening processes
in 2xxx Al-alloys, which in contrast to traditional meth-
ods, is fast, non-destructive and cost-effective means of
testing.
5. Microstructural changes during aging treatments of all
three Al-alloys were monitored by optical and scanning
electron microscopy. The existence of precipitation se-
quence and various phases along with over-aging stage
was confirmed by microscopy and the results were dis-
cussed and correlated well with the variation in hardness,
electrical conductivity and ultrasonic parameters.
6. It was therefore concluded that the combination of eddy
current and ultrasonic nondestructive evaluation tech-
niques could yield better, more reliable, comprehensive
and realistic results than any single technique for non-
destructive detection and characterization of microstruc-
tures and material properties of 2xxx series Al-alloys
when conventional testing techniques are difficult or not
suitable.
Acknowledgements The authors wish to thank Mr. Muhammad
Saraf (Deputy Chief Manager) and Dr. Sajid Mirza (Senior Chief Man-
ager) for their valuable suggestions and guidance and Mr. Ahmed Bilal
(Chairman SUPARCO) for their approval and provision of facilities.
Authors also like to acknowledge the technical assistance and mean-
ingful discussions made by Mr. Badar-ul-Hassan (Technical Officer),
Mr. Arsala Khan for his assistance and cooperation in ultrasonic test-
ing, Mr. Sajid Ali Asghar for providing eddy current testing facility,
and Mr. Yousuf Khan for SEM-EDS facility.
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