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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 tion and characterization of material properties when con-
structural applications due to their good mechanical proper- ventional testing methods are not applicable.
ties. During heat treatment of these alloys, solution treated
parts sometimes mixed with age hardened parts during han- Keywords AA 2024 · AA 2014 · AA 2219 · Aluminum
dling. This result in difficulty in distinguishing between so- alloys · Precipitation hardening · Ultrasonic testing · Eddy
lution treated and aged parts of various grades. Moreover, current testing
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- 1 Introduction
sion testing and microscopy, however these are destructive
in nature and sometimes not desired particularly for finished Heat treatable aluminum alloys of 2xxx series (Al–Cu type)
products. The main purpose of this paper is characteriza- are widely used for structural applications (particularly in
tion of material properties of 2xxx series Al-alloys by eddy aerospace and automotive industry) at moderate service tem-
current and ultrasonic NDE techniques so that the inspec- peratures due to their good strength-to-weight ratio and fa-
tion can be carried out effectively in the shortest possible tigue resistance. The mechanical properties of such alloys
time. Three wrought Al-alloys of 2xxx series (AA 2014, are obtained through precipitation (or more often called age
AA 2024 and AA 2219) were homogenized followed by so- hardening) hardening phenomena wherein strength is in-
creased because of existence of an ordered precipitate struc-
lution heat treatment and age hardening treatments at spe-
ture. In solid solution, the alloying elements are completely
cific temperatures for 1–16 h. The changes in hardness and
dissolved and the material behaves like a single-phase ma-
microstructure during heat treatments were determined by
terial having low strength and hardness. During aging, the
traditional material characterization methods and then cor-
alloying elements cluster and start forming different types
related with electrical conductivity, sound velocity and at-
of small precipitates, depending on the aging temperature.
tenuation coefficient obtained through Nondestructive Eval-
The precipitation sequence in Al–Cu–Mg–Si alloys is ex-
uation (NDE) techniques. Results demonstrated an excellent
tensively studied by different researchers [1–6].
correlation between hardness and sound velocity, whereas
Theses alloys are usually used in peak hardened condi-
extend of aging can be easily predicted by electrical con- tion (i.e. mostly in T6 condition—solution heat treatment
ductivity, and attenuation coefficient measurement. Investi- followed by artificially aging). Mechanical properties and
gation suggested a way towards the non-destructive detec- microstructures obtained as a result of solution treatment
and aging are generally characterized and qualified by con-
ventional testing techniques like micro-hardness, tension
F. Tariq () · N. Naz · R.A. Baloch · Faisal testing, optical or scanning electron microscopy, etc. How-
Materials Research and Testing Laboratory, Pakistan Space and ever, these evaluation techniques are destructive in nature,
Upper Atmosphere Research Commission (SUPARCO),
Karachi 75270, Pakistan costly and time consuming. Furthermore, these tests are
e-mail: t_fawad@hotmail.com usually carried out on ‘coupon samples’ assuming that the
J Nondestruct Eval

coupon is the true representative of the component that will pick-up coil changes accordingly. The magnitude and phase
go into service. The conventional ‘coupon based’ approach of induced voltage or impedance change are used to corre-
of determining material properties may not be good enough late with the microstructures and mechanical properties.
as there may be variation in the heat treatment seen by the Extensive amount of work has been conducted on charac-
coupon and the component itself. Hence the results of de- terizing properties of different Al-alloy grades non-destruc-
structive tests on coupons may not truly apply to the compo- tively by UT and ECT [43–53]. However, there is little
nent to be used in service. Also in service, when these alloys published data available in literature on the relationship be-
are employed at temperatures in the range 130–170°C near tween the material properties and ECT and UT responses of
to those of the artificial aging treatment, aging processes 2xxx series Al-alloys as a result of aging treatments. Since
proceed causing over-aging of material (coarsening of pre- Al-alloys of 2xxx series are the most widely used alloys for
cipitates) and deteriorating its mechanical properties such as structural applications therefore the full potential of nonde-
hardness and tensile strength [3]. Field characterization and structive evaluation techniques in these alloys is yet to be
performance evaluation is also not possible using destructive realized. Therefore, in the present study an attempt is made
testing techniques. Therefore, there exists need for alternate to establish a correlation between hardness and microstruc-
techniques such as nondestructive techniques for rapid and tures of wrought 2xxx series Al-alloys (AA 2014, AA 2024
cost-effective characterization and qualification of material and AA 2219) with electrical conductivity and acoustic pa-
properties during production as well as in service. rameters (velocity and attenuation) obtained through ECT
Nondestructive evaluation (NDE) methods are most com- and UT respectively. It is envisaged that data present in this
monly employed for detection and characterization of de- study could be used to determine nondestructively, the hard-
fects in the component; however they hold good poten- ness (or strength) of the 2xxx series Al-alloy grades as well
tial to characterize mechanical properties and microstruc- as the unknown thermal history of a given component before
tures in materials [7–14]. In the past few decades numer- putting the component to service.
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],
2 Experimental Work
porosity [24, 25], weld microstructure, and defects [26, 27],
etc.), (ii) mechanical properties (like hardness, strength, im-
2.1 Material
pact strength, fracture toughness, etc.) [28–33], (iii) thermo-
mechanical treatments during fabrication (like cold rolling,
The materials used in this research work were wrought heat
hot deformation, etc.) [34–36] and (iv) service-induced
treatable 2xxx series Al-alloys. Three grades were selected
damage on components (like fatigue, creep, stress corrosion
for investigation: (i) AA 2014 (Al–Cu–Si), (ii) AA 2024
cracking, hydrogen attack, etc.) [37–42], by conventional
testing techniques and correlate these with the parameters (Al–Cu) and (iii) AA 2219 (Al–Cu–Mn). Spectroscopic
(like electrical conductivity, sound velocity, sound attenua- analysis of all grades was carried out using optical arc emis-
tion, etc.) obtained by NDE techniques (eddy current testing, sion spectrometer and the elemental composition is given in
ultrasonic testing, acoustic emission testing, etc.). Table 1.
Among many available Nondestructive Evaluation (NDE)
techniques, ultrasonic testing (UT) and eddy current testing 2.2 Heat Treatment
(ECT) are the most preferred, widely studied and employed
techniques for characterizing material properties. Both non- All the grades were initially in the form of plates and forged
destructive evaluation techniques offer distinct advantage in bars. Square samples of about 25 × 25 × 20 mm size and
that the material properties can be verified on actual com- round samples of about 50 mm diameter and 25 mm thick-
ponents of engineering structures. Moreover, being volu- ness were cut perpendicular to the rolling direction from
metric in nature, examination can give an idea about the plates and bars respectively. Samples of all three grades
bulk material properties. Non-destructive evaluation by UT were homogenized at particular temperature and time (heat
is one promising method which has gained much interest treatment schedule is listed in Table 2) and slowly cooled
during recent years. Ultrasonic parameters (sound veloc- in furnace to obtain a uniform reference microstructure.
ity and attenuation) are significantly affected by changes Samples were then solution heat treated (SHT) to dissolve
in microstructural features or mechanical properties of ma- all precipitates followed by quenching in water at ambient
terials [43]. Eddy current testing is another important non- temperature to obtain supersaturated solid solution (see Ta-
destructive evaluation technique used to quickly character- ble 2). Following the SHT, the samples were artificially aged
ize materials, because eddy currents are influenced by mi- at specified temperature (corresponding to T6 temper) of
crostructural alterations due to precipitates, cold work, de- each grade for different duration ranging from 1–16 h and
formation, etc. and the coil impedance or induced voltage in 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- diameter, suitable for non-ferrous metals and alloys) was
ther aging. Homogenization and SHT was done in electric used for all measurements. Change in electrical conductivity
resistance-type heat treatment furnace and age hardening was measured at room temperature in terms of percentage
treatments were done in heating oven. The temperature vari- of international annealed copper standard (%IACS). Before
ation was kept within ±3°C. conducting electrical conductivity test, equipment was cal-
ibrated on standards of known conductivity. The measured
2.3 Macrohardness values were considered to be accurate within ±0.5%IACS.
Five readings were taken of each sample and then average
Hardness measurement was performed on flat, prepared sur- value was used for plotting the graph of electrical conduc-
face by Macro-Vicker hardness tester at 10 kg load and 10 s tivity verses aging temperature.
dwell time. At least five measurements were taken for each
condition and average result is quoted in this work. The 2.6 Sound Velocity Measurement
maximum scatter in the hardness measurements was found
to be less than ±3 HV. Longitudinal sound velocity was measured by using
Krautkramer USM-25S LEMO ultrasonic flaw detector as
2.4 Microstructural Examination per ASTM standard E 494-99. The calibration standard
block V1 was used for calibration of equipment. The sound
Metallographic samples of all three grades in solution velocity was calculated by Pulse-echo method. Both 2 MHz
treated and aged conditions were prepared by adopting stan- and 4 MHz longitudinal beam probes were used to measure
dard grinding and polishing techniques. Observations were sound velocity. Filtered machine oil was used as the cou-
made after etching with modified HF solution (10 ml HF + plant for the longitudinal wave probes and a constant force
90 ml H2 O + adding MoO3 up to saturation). Microstruc- was applied on the probes to obtain a stable thickness of the
tural examinations were carried out using optical micro- coupling film. For achieving the highest possible accuracy,
scope incorporated with image analyzing software and scan- the specimens were carefully machined and polished to have
ning electron microscope equipped with energy dispersive smooth, flat and parallel surfaces. The plane parallelism be-
spectrometer (EDS). tween the two opposite faces of the sample was checked
using a surface plate and a dial gauge. The thickness of spec-
2.5 Electrical Conductivity Measurement imens was measured with an error of ±0.001 mm and the
scatter in ultrasonic velocities was within ±3 m/s. The accu-
Eddy current testing technique was used for calculation of racy of the measurement is largely depends on the accuracy
electrical conductivity of the materials in all heat treated with which the thickness of the component is measured.
conditions. Electrical conductivity was measured on ground Moreover, temperature also affects the velocity of sound;
and polished samples as per ASTM standard E 1004-94 therefore all the measurements were carried out at almost
using portable Locater 3s eddy current equipment capa- same temperature. The mean values for the velocities were
ble of operation in frequency range of 10 Hz to 10 MHz. obtained by averaging the five independent measurements.
500 kHz electrical conductivity measuring probe (5/16 inch In addition to sound velocity, attenuation co-efficient (α)
J Nondestruct Eval

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) hardness (from solution treated condition i.e. 105 HV) was
between the two back-surface signals and then dividing it seen upon artificial aging up to 4 h which was attributed to
by the total path traveled (thickness of sample in this case). the formation of GP I zone (coherent with the matrix). Fur-
Attenuation co-efficient (α) is expressed in terms of dB/mm. 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
3 Analysis of Results and Discussion θ  particles (metastable) having definite crystal structure are
responsible for peak hardness in this alloy. Aging for longer
3.1 AA 2014 (Al–Cu–Mg–Mn)
time periods i.e. above 12 h have resulted in gradual decline
Response of age hardening treatments on hardness, elec- in hardness curve due to over-aging. Material gets soft be-
trical conductivity, longitudinal sound velocity and attenu- cause of either precipitation of in-coherent stable precipi-
ation coefficient are plotted on graph as shown in Fig. 1. tates (equilibrium θ phase formed and coherency strain is
The variation in hardness with aging time exhibited different lost) or coarsening of already precipitated particles. With
peaks corresponding to the precipitation of different phases, continued aging at any given temperature, there is tendency
as shown in Fig. 1a. The existence of typical precipitation for the small particles to dissolve and the resultant solute to
sequence is evident in aging curve (Fig. 1a). Sudden rise in precipitate on larger particles causing them to grow, thereby
J Nondestruct Eval

lowering the total interfacial energy. This process is termed The relationship observed between electrical conductivity
as particle-coarsening or sometimes Ostwald ripening. and aging treatments was in agreement with the previous
The actual concurrent sequence of precipitation in 2xxx work on Al–Cu alloys [44, 54].
series Al–Cu–(Mg–Mn) alloys strongly depends on rela- Figure 1c depicts the change in longitudinal sound veloc-
tive amount of alloying elements, history of the material in- ity as a function of aging time. The plot shows that the sound
cluding production methods (rolling, forging, etc.), quench- velocity (measured by both 2 MHz and 4 MHz probes) in-
ing conditions, natural aging and further heat treatments. creases non-monotonically in the same way as hardness in-
Various authors have discussed the possible sequences of creases. Moreover, the precipitation of different phase can
precipitation in Al–Cu, Al–Cu–Mg and Al–Cu–Mg–Mn al- be distinguished by different peaks in sound velocity values.
loys [1–6]. Increase in velocity during initial stages of aging was at-
tributed to the increase in the elastic modulus of the matrix
(1) α ss → GPZ (Cu-rich phase) → θ  (metastable) → θ 
due to the depletion of solute element (Cu) from the matrix
(metastable with definite crystal structure) → θ (CuAl2 -
during precipitation of θ  and θ  phases. Maximum velocity
stable)
was detected for 12 h aged samples. This value corresponds
(2) α ss → GPZ (Cu-rich phase) → GPZ II (Cu-rich phase)
to the peak hardness condition. The decrease in velocity val-
or S (metastable) → S (metastable) → S (CuMgAl2 -
ues above 12 h aging was attributed to loss of coherency
stable)
strain and precipitates coarsening i.e. over-aging. The re-
(3) α ss → GPZ (Cu-rich phase) → Q (metastable) → Q
sults illustrated a quite good correlation between hardness
(Cu2 Mg8 Si6 Al5 or Al4 Cu2 Mg8 Si7 -stable )
and longitudinal sound velocity with degree of age harden-
The change in electrical conductivity (in terms of % ing. The observations of results also suggest that the sound
IACS) in response to artificial aging is presented in Fig. 1b. velocity obtained from 4 MHz probe could be more reliable
The variation in the electrical conductivity with aging is than 2 MHz probe. Same trend of sound velocity with age
complex and results from a number of contributions includ- hardening treatments (i.e. increase in sound with hardness)
ing changes in the scattering of electrons. The change was was also quoted earlier by other authors [18, 19]. The sound
not perfectly linear i.e. electrical conductivity increases with wave velocity in solids is in fact related to elastic modu-
increasing aging time but the curve does not highlights dif- lus of the material, which in turns change with age hard-
ferent precipitation stages, which are clearly visible in hard- ening because of change in matrix composition and pre-
ness curve (Fig. 1a). Electrical conductivity decreases af- cipitation of different phases. The increase in the sound
ter 12 h aging which reflects the onset of over-aging. Elec- velocity with aging is attributed to the increased volume
trical conductivity measurements cannot, in principle, dif- fraction of precipitates (which results in reduction in the
ferentiate between GP zones since changes in conductivity distortion in the crystal lattice), which contribute to the in-
are determined more by the number and size of the scatter- creased elastic modulus and hardness of the aged speci-
ing centers than by their crystal structure or degree of co- men [18]. However, in overaged condition (i.e. incoherent
herency with Al-matrix. Same phenomenon was observed matrix-precipitate interface exists); the loss of coherency
here that the GP zones are not revealed by the electrical con- strain leads to decrease in the elastic modulus of the inter-
ductivity measurement however the formation of intermedi- face and therefore reduces the effective ultrasonic velocity
ate phases (coherent θ  and semi-coherent θ  phases) are de- of the material. Hence the ultrasonic velocity monitored dur-
tected (Fig. 1b). The increase in conductivity with increasing ing age hardening process would provide insight into the ki-
aging time was thought to be the result of purification of the netics of precipitate formation and their growth/dissolution.
matrix by means of segregation of the solute atoms and for- These ultrasonic velocity observations have been substanti-
mation of semi-coherent metastable phases. As the rate of ated with micro-examination results discussed in upcoming
precipitation was accelerated, the foreign atoms that act as paragraphs.
scattering centers of electrons segregate from the aluminum The variation in attenuation coefficient (α) with increas-
matrix at an enhanced rate. Electrical conductivity level be- ing aging duration is illustrated graphically in Fig. 1d. It is
comes lower when the concentration of solute atoms in solid observed that the attenuation measured with 4 MHz probe
solution increases, while it becomes higher when the alloy- increases linearly with increasing time of aging. Attenua-
ing elements are precipitated out. The electrical conductivity tion in longitudinal sound waves followed the same trend as
is therefore largely influenced by the amount of alloying el- that of hardness in response to aging. Moreover, attenuation
ements in the solid solution (Al matrix) and the amount and coefficient measured with 4 MHz probe leads better results
nature of precipitates. Equilibrium θ precipitates are coarser than 2 MHz probe. This is because the ultrasonic waves at
and their size increases as aging proceeds above 12 h, thus high frequencies have relatively shorter wavelengths, and
minimizing their scattering effect. Therefore, reduction in hence, the ultrasonic waves become sensitive to fine pre-
electrical conductivity in over-aged samples was recorded. cipitates and are expected to interact more strongly with
J Nondestruct Eval

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 occurs which acts as source of scattering in path of propagat-
through a material due to scattering and absorption. Absorp- ing sound waves. Coarsening of precipitates in the overaged
tion, which is caused by microstructural defects such as dis- condition also increases scattering of waves so the attenua-
location and point defect, takes only small part of the mea- tion values further increased. It is known that the attenuation
sured attenuation in metallic materials and usually assumed depends upon the size of the substructure of the grains (like
to be negligible [55]. The increase of ultrasonic attenuation martensite platelets in hardened steel) divisions [58]. Hence
with aging seems to be related to the precipitation of various the increase in particle size during over-aging will appar-
phases (which act as scattering points) in the microstructure. ently increase attenuation in sound waves.
The precipitation of second phase particles from the ma- Hardness values (up to peak hardness condition i.e. 12 h
trix and coarsening of second phase particles with different aging) were correlated with electrical conductivity, longitu-
acoustic impedance from the matrix is reported to increase dinal sound velocity and attenuation coefficient in Fig. 2.
ultrasonic scattering [56, 57]. As aging proceeds, the forma- The solid line in Fig. 2 represents the least square best-fit
tion of precipitates (having different impedance than matrix) 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- of re-crystallized grains with intergranular and intragranu-
ficient, R 2 of about 0.97 calculated using 2nd order polyno- lar precipitation of coherent θ  or semi-coherent θ  phases.
mial fit. Graph between hardness and sound velocity showed Strain line and grain contrast was also evident in the struc-
a remarkable linear relationship with correlation coefficient ture. High density of fine precipitates (probably θ  and θ  )
of about 0.98 (Fig. 2b). This indicates that an excellent cor- uniformly dispersed throughout the structure was observed
relation is existed between hardness and velocity, and hard- in the 12 h aged sample. The fine dispersion of strength-
ness could be predicted more accurately by measuring sound ening precipitates (coherent and semi-coherent) is responsi-
velocity. However, the graph between hardness and atten- ble for higher hardness of the material. In alloys such as the
uation coefficient was non-linear and the polynomial line AA 2014, the high copper content (about 4% by wt.) assures
is best fitted with the R 2 value of 0.83 which depicts pro- the presence of θ precipitation sequence, generally observed
nounced scatter in values, as shown in Fig. 2c. for Cu greater than 0.2–0.5 wt.%. Aging above 12 h caused
The changes in microstructure from SHT condition to formation of equilibrium θ (CuAl2 ) phase which was inco-
peak hardened condition in response to aging time can be herent with the matrix and over-aging occurred.
seen in Fig. 3. The micrograph of SHT sample (Fig. 3a) Figure 4 presents the selected high magnification SEM
shows fine re-crystallized grain structure of AA 2014 grade pictures of the AA 2014 samples. Microstructure of 5 h aged
of Al-alloy consisting of α matrix (Al-rich) within which sample did not reveal any appreciable precipitation; only in-
black insoluble coarse particles of AlMgCu and AlMnCu- soluble particles were found at grain boundaries, as shown
in Fig. 4a. The almost clear grains showed that the zones
types (also containing Fe as determined by energy disper-
were dissolved and replaced by coherent fine strengthening
sive spectroscopy) are present. These intermetallic particles
precipitates (mostly θ  and relatively low amount of θ  ) dis-
were elongated in the flow direction and were not soluble at
tributed evenly in the matrix. Although significant hardness
solution treatment temperature. Undissolved CuAl2 precip-
was achieved after 5 h aging, but the precipitates were rather
itates (white, outlined) are also visible in the structure. Dur-
so fine that they were not resolved by SEM. Figure 4b cor-
ing quenching from SHT temperature, GP zones are formed
responds to the high magnification micrograph of 12 h aged
in Al–Cu type alloys which are so fine that they could not
sample that was artificially aged to peak hardness. Fine pre-
be resolved by optical microscope. The large black particles
cipitates (shown with arrow in Fig. 4b) found to be evenly
are rosette formed by eutectic melting above the solution an- distributed throughout the structure; both within grains and
nealing temperature. The strain lines are also seen in Fig. 3a. at grain boundaries.
No significant precipitation was observed in the structure
upon artificial aging at 165°C for 5 h. However, less vol- 3.2 AA 2024 (Al–Cu)
ume of CuAl2 intergranular particles was present. Precipi-
tates were also found on grain boundaries. Figure 3b shows Variation in hardness, electrical conductivity, longitudinal
the micrograph of sample aged for 8 h consisting primarily sound velocity and attenuation coefficient for AA 2024
J Nondestruct Eval

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. seen in Fig. 5a. Hardness then continuously increased with
A little dissimilar trend in hardness increment was found in increasing aging time up to 8 h and then becomes almost
AA 2024 grade upon aging which was primarily due to dif- constant. Peak hardness of about 144 HV was achieved af-
ferent chemical composition than AA 2014 grade and sec- ter 13 h of aging. Aging above 13 h caused decline in curve
ondary due to higher aging temperature (i.e. 190°C as com- which reflects over-aging. Preliminary increase in hardness
pared to 165°C for AA 2014 grade) employed. It is well up to 2 h was attributed to precipitation of GP zones. Straight
known that when the Cu content is high and the aging tem- region between 2–4 h, in which hardness was almost stable,
perature low, the sequence of stages followed is GP I zone, was thought to be due to dissolution of GP zones and for-
GP II zone, θ  and θ (CuAl2 ). On aging at higher tempera- mation of intermediate phases. Further increase in hardness
tures, however, one or more of these intermediate stages may up to peak condition was because of precipitation of tran-
be surpassed. In Fig. 5a typical non-monotonic increase in sition metastable phases. These transition phases are either
hardness was observed with increasing aging duration. From fully or partially coherent with the matrix and are actually
83 HV in SHT condition, hardness rapidly rises to 105 HV responsible for hardening. Aging above 13 h resulted in re-
within 2 h and then becomes steady in between 2–4 h, as duction in hardness due to precipitation of in-coherent equi-
J Nondestruct Eval

librium precipitates (i.e. over-aging occurred), as shown in alloys was also pointed out by others [50, 60]. Sound ve-
Fig. 5a. locity seems to be more reliable parameter and could eas-
Figure 5b shows graph of electrical conductivity with ag- ily predict all stages of precipitation including over-aging.
ing time, presenting a continuous rise in conductivity with But accurate sound velocity measurement demands highly
aging time up to 14 h and then drops above it. Similar behav- prepared polished surface. It was observed that the slight
ior was observed in hardness with aging duration. However, changes in test temperature, surface preparation/conditions,
an interesting feature about electrical conductivity curve was thickness variation in sample, and coupling conditions could
the presence of different peaks which corresponds to differ- lead to large scatter in the results.
ent stages of precipitations. All these stages were not being Figure 6 illustrates the relationship of hardness with elec-
detected in hardness curve as shown in Fig. 5a. Similar trend trical conductivity, sound velocity and attenuation coeffi-
in electrical conductivity with aging treatments was also re- cient. Linear relationship of hardness (up to peak hardness
ported earlier [44, 54, 59]. It was thus observed that progress condition i.e. 14 h aging) with correlation coefficient of 0.97
of aging and precipitation sequence can be monitored with was calculated for longitudinal sound velocity (Fig. 6b).
electrical conductivity measurements. Whereas, hardness data was correlated with electrical con-
Figure 5c shows variation in sound velocity (from both ductivity and attenuation coefficient by least square best-
2 MHz and 4 MHz longitudinal wave probes) with aging fit method using 2nd order polynomial function, shown in
time. Similar trend in velocity was noticed as that for elec- Figs. 6a and 6c. It was observed that sound velocity corre-
trical conductivity. Both sound wave velocity and hardness lated more perfectly than any other parameter and could be
increase to a certain peak value and then decrease on over- used for hardness prediction with reasonable accuracy and
aging. For any given aging time, it was observed that the high confidence level.
ultrasonic velocity at 4 MHz was higher than that at 2 MHz. Figure 7 shows the microstructural changes in AA 2024
Furthermore, the peak velocity was observed at 12 h aging grade in response to aging treatments. Solution treated struc-
(Fig. 5c). Existence of various peaks in sound velocity curve
ture mainly consisted of Al-rich matrix having equiaxed
confirmed the concurrent precipitation of different phases.
grains with intergranular and intragranular spehoidized in-
Moreover, the velocities curve showed that the actual onset
soluble intermetallics, as seen in Fig. 7a. These large black
of over-aging was at 12 h, wherein coherent precipitates be-
particles were found to be CuMgAl2 , Cu2 MnAl20 and
gin losing their coherencies and coarsening of precipitates
CuFeAl7 by energy dispersive spectroscopic analysis. Pre-
started. The differences in sound velocity during aging arise
cipitation of CuAl2 particles was less because of proper so-
primarily from the differences in the elastic modulus of the
lution treatment; Cu was mostly dissolved in solid solution.
phases and precipitate/matrix interface which are in turn af-
Slight change in structure was seen in 4 h aged samples.
fected by the degree of lattice distortion caused by the pre-
Structure consisted of uniform distribution of precipitates
cipitate. The variation in velocity values with aging treat-
ments were very well correlated with hardness and electrical throughout the matrix; however individual precipitates were
conductivity and are in close agreement with the findings of on very fine scale and therefore not resolved by optical mi-
other researchers [19, 57]. croscope. After 4 h aging, GP zones were thought to be
Results of attenuation coefficient measurement showed completely dissolved and replaced by intermediate phases of
linear relationship with aging time i.e. attenuation in sound definite crystal structure. High density of precipitation was
waves increases with aging time up to 16 h (Fig. 5d). Atten- observed in the spotted structure after 12 h of aging; respon-
uation kept increasing without any drop; even in overaged sible for high hardness. Fine coherent and semi-coherent
condition. Similar behavior in attenuation coefficient was precipitates were uniformly distributed throughout the ma-
also found in AA 2014 grade, as shown in Fig. 1d. The rea- trix. Figure 7b corresponds to the microstructure after 14 h
son for this was already discussed in preceding paragraphs. aging. Precipitates were relatively coarser; this illustrated
It was also noted that the high frequency probe leads better the onset of over-aging. The fine precipitates dissolved (to
results than low frequency probe. The occurrence of con- lower total interfacial energy) in favor of coarse equilibrium
temporaneous peaks in both hardness and ultrasonic attenu- precipitates. These equilibrium precipitates are incoherent
ation provides the experimental evidence of the suitability of with the matrix and their formation always leads to soften-
using ultrasonic testing for characterizing precipitation pro- ing (also confirmed from hardness, electrical conductivity
cesses in Al–Cu alloys. However, the occurrence of peaks and sound velocity results), since coherency strains disap-
in attenuation coefficient curve depends also on the type, pear. Precipitation free zones (PFZ) were also observed in
volume fraction and average distribution of the precipitate the structure (Fig. 7b). These zones were formed as a con-
size in the structure. From the results, it was cleared that sequence of solute atom (Cu) depletion from the adjoining
the onset of over-aging can not be detected by the attenua- areas of the grain boundaries.
tion coefficient measurement for most cases. This continu- Detailed microstructural analysis by SEM also con-
ous increase in attenuation with aging of Al–Li and Al–Cu 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 tate out of the solution. Moreover, continuous change in lat-
(Fig. 8). Microstructure of 9 h aged sample is shown in tice distortion due to matrix/precipitate interface, precipitate
Fig. 8a. Even dispersion of fine precipitates (black dots sizes, morphology and distribution within the matrix also
shown with arrow) is visible in the structure. Microstruc- cause change in conductivity. Steps in conductivity curve
ture of sample aged for 14 h is shown in Fig. 8b. It was exhibited the stages of precipitation (i.e. formation and dis-
viewed that the precipitates grew on longer aging times i.e. solution of GP zones, precipitation of metastable transition
over-aging had occurred. Coarse precipitates (indicated with phases, and precipitation of equilibrium particles and their
arrow) were evident in the magnified view of the selected re- coarsening). Similar electrical conductivity response with
gion in Fig. 8b. aging time was also observed in AA 2024 grade (Fig. 5b).
Microstructural changes and occurrence of different pre- Figure 9c shows prominent variations in longitudinal
cipitation stages during aging were confirmed from both sound wave velocity with aging treatments and it was ob-
optical and scanning electron microscope results and these served that the sound velocity varies in the same manner
changes were very well correlated with the hardness, elec- as the hardness upon aging. Different stages of precipita-
trical conductivity and ultrasonic parameters. tion were distinguished from different peaks in sound veloc-
ity curve. Similar dependence of sound velocity on elastic
3.3 AA 2219 (Al–Cu–Mn) modulus and hardness (which in turns depends upon precip-
itation process) during aging of AA 2219 grade was stated
The effect of artificial aging time up to 16 h at fixed temper- by other researchers [20]. It was thus confirmed that good
ature (i.e. 185°C) on hardness, electrical conductivity and correlation exists between hardness and longitudinal sound
ultrasonic parameters of AA 2219 grade are graphically de- velocity for AA 2219 grade.
picted in Fig. 9. Increase in hardness was observed with in- Changes evolved during aging of AA 2219 grade were
creasing aging time, as seen in Fig. 9a. Hardness increment also monitored in terms of attenuation coefficient as shown
with aging time in AA 2219 grade was almost similar to that in Fig. 9d. It was observed in Fig. 9d that attenuation co-
observed in AA 2024 grade (Fig. 5a) because both grades efficient measured with 4 MHz probe varied linearly with
were very close in chemical composition except Cu con- aging time. Similar tendency in attenuation coefficient (i.e.
tent (about 5.35% in AA 2219 grade as compare to 3.50% increase with increasing aging time) was already seen in
in AA 2024 grade). Initially, aging up to 4–5 h resulted in Fig. 5d for AA 2024 grade. However, results obtained from
marked rise in hardness up to 128 HV. The hardness was al- 2 MHz probe showed large scatter in the readings and were
most stable in between 5–12 h and then again increase upon therefore not meaningful.
aging to 12–14 h. Peak hardness of about 138 HV was at- Relationship of hardness data with electrical conductiv-
tained after 14 h of aging. Decline in hardness curve was ity, sound velocity and attenuation coefficient was plotted
registered for aging above 14 h owing to overaging. and linear as well as 2nd order polynomial regression was
Electrical conductivity results showed continuous in- calculated using least square fit method, as shown in Fig. 10.
crease in conductivity with increasing aging duration up to From Fig. 10a, it was clearly seen that the data was quite
14 h and then drops on further aging (Fig. 9b). It was ob- scattered and relatively weak relationship existed among
served that electrical conductivity values were not stable in hardness and electrical conductivity (R 2 of about 0.73). It
between 5–12 h aging as in hardness curve; instead they was observed that towards the highest values of hardness,
keep increasing and this trend was attributed to continu- the electrical conductivity shows rapid increase without any
ous depletion of solute elements from the Al matrix with appreciable increase in hardness. This trend was obvious in
subsequent formation of precipitates. This causes purifica- all three alloys (Figs. 2a and 6a). This is in the regime where
tion of Al-rich matrix. It is well known fact that all metallic the incoherent precipitates are forming. Precipitates of such
additions to Al reduce its electrical conductivity, and elec- phases do not increase the hardness but increase the elec-
trical conductivity increases when these elements precipi- trical conductivity. Distinct positive correlation was existed
J Nondestruct Eval

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 of transition phases. Precipitation of transition phases was
velocity (Fig. 10b). Correlation coefficient R 2 of about 0.85 also confirmed from hardness value i.e. 128 HV. Moreover,
was obtained between hardness and attenuation coefficient precipitates were seen segregated at various locations. Sol-
through 2nd order polynomial fit, as seen in Fig. 10c. The uble CuAl2 particles (white outlined) were also visible in
analysis of results suggested a rational correlation between Fig. 11b. Prolonged aging (up to 16 h) resulted in over-aging
hardness and ultrasound velocity, whereas other parameters of the structure; precipitates become incoherent and coarse.
are weakly related with hardness. Scanning electron micrographs of AA 2219 grade sam-
Figure 11 shows the optical micrographs of AA 2219 ples in aged conditions are displayed in Fig. 12. Change
grade taken after different thermal treatments. The basic in microstructure after 5 h of aging is shown in Fig. 12a.
trend in microstructural evolution during aging treatments This change in structure was attributed to precipitation of
was almost same as that observed in AA 2024 grade. Fig- intermediate phases responsible for significant increase in
ure 11a shows typical structure in solution treated condi- hardness. High magnification micrograph of 13 h aged sam-
tion containing large amount of insoluble intermetallics dis- ple revealed high density of precipitates evenly distributed
tributed all over the matrix. Grain boundaries were not re- throughout the matrix, as shown in Fig. 12b. This struc-
vealed in the micrograph (Fig. 11a). Significant alteration in ture corresponds to peak hardness condition (138 HV). Rela-
microstructure was observed in 5 h aged sample (Fig. 11b). tively large volume fraction of precipitates (probably coher-
Darkish mottled appearance was indicative of precipitations 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. set of over-aging could not be detected from attenuation
Aging above 14 h caused particle growth and coarsening change. The change in hardness with aging time was also
with subsequent decrease in hardness (about 127 HV in 16 h confirmed from microstructural examination. Thus, progress
aged sample), as seen in Fig. 12c. Coarse precipitates (prob- of aging treatments and resulting material properties (mainly
ably semi-coherent θ  and equilibrium θ ) are clearly visible hardness) could be successfully and non-destructively mon-
(shown with arrow) in magnified view in Fig. 12c. The mi- itored and assessed by simultaneous combination of eddy
crostructural modifications during aging examined by mi- current and ultrasonic nondestructive evaluation techniques.
croscopy are in conformance with the results of hardness
measurements, electrical conductivity and ultrasonic param-
eters.
Analysis of results and discussion firmly suggested that 4 Conclusions
excellent correlation existed between hardness and longi-
tudinal sound velocity obtained from 4 MHz probe for all The possibility and effectiveness of characterizing material
the three grades of 2xxx series investigated and the linear properties of 2xxx series Al-alloys as a result of age harden-
fit obtained show good promise in identifying any particu- ing treatments, by eddy current and ultrasonic nondestruc-
lar microstructure for a given ultrasonic velocity/hardness tive evaluation techniques, was evaluated in this study. The
(Table 3). Quite good relationship (using polynomial fit) results and discussion of this work can be summarized as
was found between hardness and electrical conductivity for follows:
AA 2014 and AA 2024 grades. However, relatively weak
relationship was existed between hardness and attenuation 1. Samples of three Al–Cu alloy grades were homogenized
coefficient for AA 2014 and AA 2219. But, electrical con- and solution treated followed by artificial aging at known
ductivity and attenuation coefficient could be helpful in pre- fixed temperature for varying time durations (1–16 h) to
dicting microstructural evolution during aging treatments; disclose different stages of precipitation.
since they can reveal different stages of precipitation. Fur- 2. Hardness measurements showed continuous, non-mono-
thermore, ultrasonic velocity was found to be more effective tonic increase in hardness in response to aging treatments
measure of hardness than attenuation coefficient because on- for all three Al-alloys. Upon initial aging, sudden rise in
J Nondestruct Eval

hardness was observed which was attributed to the for- and realistic results than any single technique for non-
mation of GP zones coherent with the matrix. Slight de- destructive detection and characterization of microstruc-
crease in hardness after few 2–4 h of aging was due to tures and material properties of 2xxx series Al-alloys
dissolution of GP zones. Hardness kept increasing till a when conventional testing techniques are difficult or not
peak value was attained at certain aging time. The peak suitable.
hardness condition is known to be due to precipitation of
coherent and semi-coherent metastable precipitates. Ag- Acknowledgements The authors wish to thank Mr. Muhammad
ing for longer times above 12–14 h resulted in decrease in Saraf (Deputy Chief Manager) and Dr. Sajid Mirza (Senior Chief Man-
ager) for their valuable suggestions and guidance and Mr. Ahmed Bilal
hardness due to dissolution and formation of incoherent (Chairman SUPARCO) for their approval and provision of facilities.
precipitates and their coarsening. Authors also like to acknowledge the technical assistance and mean-
3. Electrical conductivity measurement results of all three ingful discussions made by Mr. Badar-ul-Hassan (Technical Officer),
Al-alloys exhibited a linear trend that is conductivity Mr. Arsala Khan for his assistance and cooperation in ultrasonic test-
ing, Mr. Sajid Ali Asghar for providing eddy current testing facility,
increased with aging time up to peak hardness condi- and Mr. Yousuf Khan for SEM-EDS facility.
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-
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