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1 INTRODUCTION
When aluminum is solution heat treated at elevated temperatures, generally in the
range of 750^1000 F (400^540 C), some alloying elements are re-dissolved to pro-
duce a solute rich solid solution. The objective of the solution process is to maximize
the concentration of hardening elements including copper, zinc, magnesium, and (or)
silicon in the solid solution. The concentration and rate of dissolution of these
elements increases with temperature so solution treating temperatures are usually
near the liquidus temperature of the alloy.
If an alloy is slowly cooled from an elevated temperature, alloying elements are
precipitated and diffuse from the solid solution to concentrate at the grain
boundaries, small voids, on undissolved particles, at dislocations, and other
‘‘imperfections’’ in the aluminum lattice. To achieve optimal strength, toughness,
and corrosion resistance, it is desirable to retard this diffusion process and keep
the elements in solid solution until the alloy is age hardened. Elements are kept
in solution by quenching from the solution treating temperature. After quenching,
aluminum is aged and during this process, a ¢ne dispersion of elements and com-
pounds are precipitated that signi¢cantly increase the strength of the material. These
processes are illustrated in Fig. 1 [1].
Diffusion and precipitation kinetics are slower in some alloys than others, per-
mitting lower cooling rates while still allowing high strengths and corrosion resist-
ance to be obtained. Figure 1 illustrates that excessively slow cooling allows
excessive concentrations of alloying elements to develop on the grain boundaries.
Figure 2 shows that intergranular corrosion for 2024-T4 will be aggravated if cooling
rates are excessively slow during quenching. (See Sec. 2.5) Similar behavior has been
found for other aluminum alloys [2]. Therefore, it is important that cooling rates
during quenching be suf¢ciently fast to minimize precipitation during cooling.
The cooling process of age-hardenable aluminum alloys affects material
2 DISCUSSION
Cooling Rate
Quench Medium Quench Temp. ( C) ( C/sec @ 450^200 C)a
Vruggink examined the effect of cooling rate on the variation of yield stress as
an indicator of quench sensitivity using various commercially available aluminum
alloys [6]. The quench media included cold water, boiling water, and still air. These
media produced a range of cooling rates varying from 5000 F/sec to 3 F/sec.
Midplane cooling rates (750^550 F/sec) of various 12 12 in. test specimens of
7075-T6 with varying thicknesses are illustrated in Fig. 4 [6]. The data show that
the average mid-plane cooling rates of about 5000 F/sec, 40 F/sec and 3 F/sec
can be expected if 0.064, 3.0 and 10.0 in. thick test specimens are quenched into
water at 70 F. From these data, quench sensitivity of age-hardenable aluminum
alloys could be compared by quenching 12 12 0.064 in. test specimens in cold
water, boiling water and still air and aging to the desired temper. It was concluded
that quenchants providing lower cooling rates have the same effect as increasing
product thickness.
Figure 5 Effect of cooling rate on the properties of 2xxx series of aluminum alloy sheet in T6
temper.
The quench sensitivity of various 2xxx and 7xxx aluminum alloys have been
examined using this methodology, and the results are summarized in Fig. 5 and
6, respectively [6]. Although a wide range of strengths are achievable in the 2xxx
series when quenched at 5000 F/sec, signi¢cant variations in quench sensitivity were
observed only when decreasing the cooling rate from 40 F/sec to 3 F/sec (See Fig.
5). Alloy AA2618 exhibited the least quench sensitivity and AA2014 exhibited
the greatest sensitivity. The results of a similar study conducted on various 7xxx
series aluminum alloys are illustrated in Fig. 6. It was found that quench sensitivity
increased with increasing concentrations of Cu and Cr.
Vruggink also attempted to quantify quench sensitivity effects for thicker
cross-sections using a modi¢ed Jominy test commonly used for steel. A 3 in. dia
by 13 in. long cylindrical test specimen was used, as illustrated in Fig. 7 [6]. A
wedge-shaped specimen, illustrated in Fig. 8, was also used. Test specimens were
solution treated and quenched into 70 F water. Vruggink reported a poor corre-
lation between yield strengths in end-quench or wedge tests compared with results
from test specimens. The properties in plate were higher than in forged and quenched
specimens as illustrated in Fig. 9 [6]. Wedge specimens machined from plate
exhibited higher strengths than test specimens cooled at the same rate as illustrated
in Fig. 10 [6].
Hart, et al. used the Jominy end-quench test to evaluate the in£uence of quench
rates on corrosion properties of AA2024-T4 and -T6 and 7075-T73 [7]. Their
experimental apparatus is illustrated in Fig. 11, and tests were conducted according
to ASTM A255-48T. A summary of cooling rates as a function of section thickness
is provided in Fig. 12 [7]. Aluminum extrusions were used in this study because
the more pronounced grain structure would be expected to provide greater sensitivity
to stress corrosion and exfoliation corrosion. The water quenchant temperature was
286K; a metal screen was placed over the ori¢ce; and the transfer time from the
furnace to the quench was < 5 sec. Variations in water pressure produced no
measurable effect on cooling rate. The hardness and conductivity data obtained from
Jominy bars for different aluminum alloys are illustrated in Fig. 13 [7].
Specimens were removed from the Jominy bars for stress corrosion studies
using the cutting plan illustrated in Fig. 14. The results of the study are illustrated
in Fig. 15 [7], and the conclusions drawn from this study are summarized as follows:
The Jominy end-quench specimen was also used to compare the hardenability
of AA7075 and AA7050 using the alloy compositions shown in Table 3 [8,9].
A 13 mm dia. 100 mm long cylindrical bar of the desired alloy was
instrumented with Type K thermocouples at the positions shown in Fig. 16 and
quenched according to ASTM A255 [8]. A comparison of the hardness and conduc-
tivity data obtained as a function of distance from the quenched end illustrated
in Fig. 17 indicate that AA7050 is less sensitive to quench rate than AA7075 [8].
AA7050 was developed for use where thicker cross-section sizes are required [8].
Transmission electron micrographs of AA7075 and AA7050 at positions corre-
sponding to 7 mm, 24 mm, 56 mm, and 79 mm distances on the Jominy bar are shown
in Figs. 18 and 19, respectively [9]. These micrographs compare AA7075 and
AA7050 specimens that were quenched at different cooling rates but tempered under
identical conditions. This work suggests that the Jominy end-quench test may be
Figure 10 Effect of cooling rate on the properties of 7079 sheet and plate.
quite useful for aluminum alloy design and for determining the impact of quench
severity on aluminum properties and microstructure.
data [10]. Cylindrical bar probes were prepared as shown in Fig. 20. The bar length
was at least 4 times the diameter to approximate an in¢nite cylinder. A Type K
thermocouple was inserted to the geometric center of the bar. Thermocouple contact
with the probe material was maintained by using a spring loaded thermocouple or by
brazing. An aluminum tube was TIG welded to the bar probe to provide a handle and
protect the thermocouple from the quenchant.
Probes to measure the cooling rates of aluminum sheet stock were prepared as
illustrated in Fig. 21. The probe consisted of two 2 2 in. aluminum sheets with
a combined thickness equal to the thickness being simulated. The sheets and handle
were cleaned, thoroughly degreased, and the surface deoxidized. An intrinsic
thermocouple was prepared using 30 gage chromel-alumel wire by spot welding
the wire to the interior of the sheet [10]. A spacer was sandwiched between the sheets
to allow the thermocouple wire to exit. The assembly was placed on a notched handle
and TIG-welded water tight.
PROBE HEAT TRANSFER. Several material and quenchant characteristics in£u-
ence the rate of heat removal from a part during quenching. An in¢nite quench
is one that instantly decreases the skin of the part to the bath temperature. The
rate of cooling in the part is then a function of only the thermal diffusivity of
the metal, i.e. its ability to diffuse heat from the interior to the surface. In practice,
however, quenchants never provide the idealized ‘‘in¢nite’’ quench.
q ¼ hA ðT1 T2 Þ
where
q ¼ rate of heat transfer
A ¼ surface area of the part in contact with £uid
T1 ¼ surface temperature
Alloy Cu Fe Si Mn Mg Zn Ni Cr Ti Zr
7075-T6 1.36 0.20 0.10 0.04 2.62 5.77 0.003 0.20 0.0170 0.0115
7050-T7451 2.11 0.12 0.050 0.04 1.98 5.74 < 0.000 0.026 0.031 0.09
(a)
(b)
Figure 21 Aluminum sheet probe. Sheet edges must be TIG welded water tight before use.
q ¼ K . A . dT =dx
where
q ¼ amount of heat transferred
k ¼ thermal conductivity of the alloy
A ¼ area of the part
dT/dx ¼ thermal gradient in the part
The expression for heat transfer from a bar, neglecting axial heat £ow is:
d 2 T 1 dT 1 dT
þ . ¼ .
dr2 r dr a dt
where
r ¼ bar radius
a ¼ thermal diffusivity
dT/dr ¼ thermal gradient
The Grossman number, de¢ned in the equation below, is also used to describe
the rate of heat removal from metal parts and is the ratio of the interfacial heat
transfer coef¢cient divided by twice the metal conductivity:
H ¼ h=2K
The Grossman number has been reported to equal approximately one for 1 in.
sections of steel quenched in water. The ¢lm coef¢cient for various experimental
conditions evaluated can be determined by ¢rst solving the Fourier equation, using
a closed-form heat transfer program which allows speci¢c ¢lm coef¢cients to be
employed as input values.
Cooling curves at the center of various-sized bars and plates were calculated
and the cooling rate between 425 C and 150 C determined. A polynomial
least-squares ¢t was then obtained to relate the average cooling rate between 425 C
and 150 C from the cooling curve, and this value was put into the polynomial
expression relating the cooling rate to the imposed ¢lm coef¢cient.
The ¢lm coef¢cient, h, is then determined by recording a cooling curve using a
thermocouple located in the center of a test probe, determining the cooling rate
between 425 C and 150 C from the cooling curve, putting this value into the poly-
nomial expression relating the cooling rate to the ¢lm coef¢cient and solving for
the h value. This procedure provides an average or effective ¢lm coef¢cient over
this temperature range. Other investigators have described methods of determining
heat £ux as a function of time or surface temperature [11^13].
Figure 22 Effect of geometry of the probe shape on cooling rate when quenching into
70 water.
1 95 1000 10.5
2 23 106 4.6
3 15 41.5 2.8
4 12.5 23.0 1.8
5 10.0 17.4 1.7
6 7.5 13.5 1.8
l
a¼
r Cp
Where: Cp is the speci¢c heat capacity, l is the thermal conductivity and r is the
density.
Cooling curves recorded during quenching of an aluminum (AlMgSiCu) and a
silver specimen (Ag 99.5) in a water-soluble polymer are illustrated in Fig. 25 [16,17].
The aqueous polymer quenchant concentration was 10% by volume and the bath
temperature was 25 C. Both probes were cleaned with 600 grit abrasive paper before
each test, and the initial probe temperature was 520 C.
The polymer ¢lm surrounding the probe surface ruptured simultaneously
around the entire surface of both probes (a phenomena called ‘‘explosive’’
rewetting), and the rewetting times (tf t s ) were extremely short. However, a stable
¢lm-boiling stage lasting about 4 sec was observed around the silver probe which was
not observed for the aluminum probe. The centerline probe temperature at
‘‘rewetting’’ was about 440 C for silver and 500 C for aluminum. The reason that
the rewetting of the silver occurs about 4 sec later for the silver probe is probably
due to the higher heat capacity and mass of the silver. This means that it will take
longer for the surface temperature to drop to the nucleate boiling stage because
more heat must be removed.
When the quenching temperature of the silver probe is increased to 800 C,
considerable stabilization of the ¢lm-boiling occurs as illustrated in Fig. 26(A) [16].
Wetting now starts at about 260 C after 24 sec compared to the start of wetting
of the AlMgSiCu probe after 1 sec at about 500 C. The maximum cooling rate
of the silver probe is not reached until a centerline probe temperature of 200 C
as shown in Fig. 26(B) [16].
Figure 30 Time required for cooling a cylindrical AlMgSiCu probe (dia. 15 45 mm) from
solution treating temperature (temeerature at which the probe was immersed) to 180 C; (a)
Cooling in distilled water at varying bath temperatures; and (b) Cooling in a water-soluble
polymer quenchant at varying quenchant concentrations and 25 C.
concentration which means that ¢lm boiling persists for longer periods of time with
higher polymer concentrations. This behavior appears in Fig. 29 as a decrease in
the starting temperature for wetting (Ts ) measured at the geometric center of
the probe. The rewetting time increases by only about 2 sec with increased polymer
concentrations up to 30%.
The cooling time from the solution treating temperature where precipitation
begins is very important for age-hardenable aluminum alloys [4]. The effect of water
temperature and polymer concentration on cooling time has been compared and
some results are illustrated in Fig. 30. The cooling time varied between 2 sec and
16 sec but, the effect achieved by varying the polymer concentration in the water
was more favorable. (Note: The temperature was measured in the center of the
direct radiation. A fan was used to provide brisk air £ow for uniform heating. Sliding
doors on the furnace bottom provided a seal during soaking and allowed the panels
to be dropped at a controlled rate. The furnace was located approximately 5 ft above
the £oor and the quench system illustrated in Fig. 27 was placed directly underneath
the furnace.
where:
CT ¼ critical time required to precipitate a constant amount (the locus of the
critical line is the the C-curves). Coordinates for CT curves for different
aluminum alloys are provided in Table 6 [37,38].
k1 ¼ constant which equals the natural logarithm of the fraction
untransformed (1^fraction de¢ned by the C-curve).
k2 ¼ constant related to the reciprocal of the number of nucleation sites,
k3 ¼ constant related to the energy required to form a nucleus,
k4 ¼ constant related to the solvus temperature,
k5 ¼ constant related to the activation energy for diffusion,
R ¼ 8.3143 J.K.1 mol1 .
7050-T76 544 0.00501 2.2 1019 5190 850 1.8 105 425^150
7075-T6 485 0.00501 4.1 1013 1050 780 1.4 105 525^150
2024-T851 459 0.00501 1.721011 45 750 3.2 104 425^150
7075-T73 475 0.00501 1.371013 1069 737 1.37105 525^150
T ¼ temperature in K.
C-curves for different alloys and tempers are illustrated in Fig. 37, 38, 39 and 40.
From these C-curves and the mathematical parameters that describe them, it is
possible to rede¢ne the equation for the amount of solute precipitated during the
quench (x) which can be calculated [2]:
k1 t
z ¼ 1 exp ð3Þ
Ct
Cahn has shown that the transformation kinetics for non-isothermal con-
ditions, such as those that would be present during a typical quenching process,
may be described by [36,39]:
ðtf
1
t¼ dt ð4Þ
CT
t0
where:
CT ¼ critical time from the C-curve,
t ¼ time from the cooling curve,
D t1 D t2 D tn1 X n1 D tn
t¼ þ þ ¼ 1 ð5Þ
C1 C2 Cn1 Cn
Dt
q¼ ð6Þ
CT
Figure 43 Schematic illustration of the experimental method used for calculating a quench
factor.
To obtain the overall quench factor, Q, the incremental quench factor values
are summed progressively as the probe or part is cooled through the precipitation
range, normally about 800^300 F (425^150 C) as shown in Fig. 43 [37].
X
800
Q¼ q ð7Þ
300
Time
step, sec 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Quench
factor 1.19 1.19 1.17 1.14 1.30 1.52 1.53 1.33
a
The values were calculated for a cooling curve obtained by quenching an aluminum probe into 38 C water
£owing at 0.25 m/sec.
where:
sy ¼ predicted yield strength,
smax ¼ yield strength after an in¢nite quench (and aging cycle),
e ¼ base of the natural logarithm,
K1 ¼ In (0.995) ¼ -0.00501
Q ¼ quench factor
The relationship between quench factor and yield strength for 7075-T73 is
shown in Fig. 44. [37] Low values of Q are associated with high quench rates, mini-
mum precipitation during cooling and high yield strengths. Conversely, higher
Q-values are obtained with slower quench rates and are associated with lower
strength values.
An alloy with a low rate of precipitation will produce a lower quench factor (Q)
than an alloy with a high precipitation rate at the same cooling rate. Quench factors
calculated for different alloys might be different even if similar section sizes are
cooled in the same quenchant, because quench factors take into account individual
alloy precipitation kinetics by means of the equation describing the C-curve (CT
function) for each alloy.
Solute elements are precipitated during cooling from the solution treating tem-
perature at ‘‘high’’ Q-values. As a consequence, an improperly quenched alloy may
not properly harden during aging, and it may be susceptible to intergranular
corrosion, stress corrosion or exfoliation.
The relationship between quench factor and yield strength for 7075-T73 alumi-
num extrusions is illustrated in Fig. 44. Forty-¢ve tensile specimens were removed
from ¢ve lots of bar extrusions ranging in diameter from 12.7 mm to 127 mm
(0.5^5.0 in.). Sections of the bar stock were solution treated at 465 C and quenched
in water ranging in temperature between 25 C and 100 C. Additional quenching
media, including a polymer quenchant, fast oil, and a £uidized bed were also
employed.
The standard deviation in yield strength about the regression line was 2.1 MPa
and 3 standard deviations was 11.0 MPa. This implies that the yield strength in a
part can be predicted rather accurately if the C(T) expression for the alloy being
quenched is known and if a valid cooling curve is available. The coef¢cients
describing the C-curve for 7075-T73 are given in Table 6. [37]
Since there is a predictable functional relationship between the quench factor
and the yield strength of alloys where the C-curve is available, it is possible to select
an upper-limit value of Q, above which speci¢ed yield strength values can be
met statistically. Data relating the quench factor to predicted yield strength in
7075-T73 are given in Table 8 [37].
The minimum allowable properties for aluminum alloys quenched for use in
the aerospace industry in the United States are taken from Military Handbook
V [40]. Table 3.7.3.0 from this source, reproduced in part in Table 9, speci¢es mini-
mum longitudinal yield strength ‘‘A’’ and ‘‘B’’ design allowable values of 413.7 MPa
Quench Factor % Attainable Predicted Yield Quench Factor % Attainable Predicted Yield
(Q) Yield Strength Strength (MPa) (Q) Yield Strength Strength (MPa)
Mechanical L 469 496 483 510 483 503 483 503 476 510 469 490 448 483
Properties Ftu LT 495 483 469 496 462 483 455 476 427 462 400 421 386 414
Mpa L 400 421 414 434 414 434 414 434 407 448 393 427 379 414
Fty LT 386 407 393 414 393 414 386 403 352 386 317 345 303 331
Table 10 Quench Factors and Film Coef¢cients Obtained with a 25.4 mm diameter
7075-T73 Alloy Probe Quenched in Water Under Various Conditions
Effective Film
Water Temperature Water Velocity, Coef¢cient (h),
C m/s Quench Factor, Q W/cm2 K
7075 aluminum is about 1.70 W/cm2 K. Unagitated water at 25 C has a ¢lm
coef¢cient of about 3.9 W/cm2 K. The ¢lm coef¢cient increased to 4.22 and
5.53 W/cm2 K at velocities of 0.25 and 0.50 m/sec, respectively. With these high ¢lm
coef¢cient values, cold water quenching can create high thermal gradients from sur-
face to center of parts and high temperature differences between thick and thin
sections. The ¢lm coef¢cients generally decrease with increasing water temperature
until, at temperatures of 70^80 C, they were in the range of 0.35^1.3 W/cm2 K.
A more extensive listing of water quenching data is provided in the Appendices.
Similar data on polymer solutions under selected conditions are provided in
Table 11. Depending on section size, the 20% solution of a polymer quenchant pro-
duced quench factors of approximately 4^12 and ¢lm coef¢cients of approximately
1.2^1.4 W/cm2 K when the bath was operated at 30 C and with velocities of about
0.12 m/sec. (A more extensive listing of quenchant data for a polymer quenchant
is provided in the Appendices.)
If the effective heat transfer coef¢cient, h, between the part and the quenchant
is established, the quench factor in commercial parts can be calculated using ¢nite
element or ¢nite difference heat transfer programs. The results of calculations
on sheets and plates made using constant ¢lm coef¢cients are shown in Fig. 45
and 46, respectively. These diagrams illustrate the interrelationship between 7075
aluminum sheet or plate thickness, ¢lm coef¢cient and quench factor. The calcu-
lations for these graphs were performed using the ¢lm coef¢cients indicated at
the ends of the diagonal lines, each of which represent a line of constant ¢lm
coef¢cient.
Figure 46 Effect of plate thickness on ¢lm coef¢cient on the quench factor for AA7075-T73
alloy.
2.4.1 Water
When water is used to quench age-hardenable aluminum alloys, heat transfer from
the workpiece to the quenchant is controlled by events occurring in three stages:
¢lm boiling, nucleate boiling and convective heat transfer. Film boiling occurs upon
initial immersion. This is a slow cooling process because the hot surface is sur-
rounded by a vapor blanket. As the part cools, the vapor blanket collapses and
nucleate boiling begins. The transition temperature between ¢lm boiling and
nucleate boiling is called the ‘‘Leidenfrost temperature’’. Heat transfer is fastest
during nucleate boiling, and the heat transfer coef¢cient, a, for nucleate boiling
is about 100 times the value of a during ¢lm boiling [43,44]. When the part has cooled
below the boiling point of the quenchant, the rate is again reduced during the con-
vective heat transfer stage.
Since aluminum solution heat treatment temperatures are signi¢cantly higher
than the Leidenfrost temperature, ¢lm boiling is to be expected initially when
quenching into water [45,46]. If the surface temperature at any point on the
workpiece is less than the Leidenfrost temperature, stable wetting and nucleate
boiling will occur at that point [47^49]. Figure 24 illustrates a typical wetting
sequence during cooling of a cylindrical specimen quenched in distilled water at
40 C. The simultaneous presence of different boiling phases with the heat transfer
coef¢cient of one surface region greater than 100 times the other causes extremely
uneven workpiece cooling. This will strongly affect the wetting processes and result
in substantial thermal gradients and increased distortion during quenching. The
boiling mechanism is stabilized by increasing the water temperature and it is clearly
evident above about 55 C as illustrated in Fig. 47 [50,51].
The consequences of uneven cooling include [16,17]:
. Regions where the ¢lm boiling persists have more precipitate formation
during quenching, than regions of faster cooling (low ts ). During
age-hardening, these regions (high ts ) experience a smaller increase in
hardness and also exhibit greater potential for intergranular corrosion than
neighboring regions where the cooling rate was faster.
. Volume regions where ¢lm boiling persists exhibit a much lower yield point
during the cooling process than regions with shorter ¢lm-boiling phases.
The non-uniformity of this process can result in signi¢cant plastic
deformation and increased distortion due to increased thermal stresses.
States allow a water quenchant temperature range from 49 C to 60 C. The in£uence
of water temperature and velocity on the quench factor obtained for 7075-T73 alumi-
num alloy is illustrated in Fig. 50(A) and 50(B) for 25.4 mm and 38.1 mm sections.
The quench factor is relatively constant in 12.5 mm and 38.1 mm diameter
extrusions, irrespective of water velocity, so long as the water temperature is below
about 50 C. However, at low velocities when quenching in 70 C water, which is
allowed by AMS 2770, the quench factor may vary by 300% depending on the water
velocity around the part.
Thus, the attainable properties are highly dependent on both the localized
circulation velocity and temperature, especially in the range 0^0.25 m/sec. Many
quench tanks use relatively low quenchant velocities and the result may be erratic
and uncontrolled aging response. Furthermore, it may also be noted by comparing
Fig. 50(A) and 50(B) that the quench factor variation increases as the section size
increases. These data show that it is insuf¢cient to specify only water temperature
to assure meeting minimum properties. The circulation velocities required must also
be speci¢ed.
It has been shown that water does not effectively wet the surface of aluminum
during quenching [16,17]. Figure 24 shows that three distinctly different cooling
regimes, with dramatically different heat transfer characteristics, are present on
the surface of aluminum simultaneously during the quenching process, these cooling
regimes can produce suf¢cient thermal gradients to increase distortion [17].
PAG copolymer quenchants form a surface ¢lm which surrounds the alumi-
num surface during quenching, as illustrated in Fig. 52 [57]. The ¢lm mediates heat
transfer and enhances wetting uniformity, thus minimizing distortion. The improved
wetting process is evident by comparing ‘‘rewetting’’ times of aluminum quenched in
water and a PAG copolymer quenchant solution [8]. Rewetting times (tf -ts ) are the
difference in the time when ¢lm boiling begins (ts ) and when nucleate boiling ends
(tf ) and data are presented in Figs 28 and 29 for water and polymer quenchant
respectively [17].
A study conducted on A356-T6 and A357-T6 castings showed that it was poss-
ible to achieve similar, but more uniform, mechanical properties with a PAG poly-
mer quenchant than with hot water [58]. The relationship between cooling rate
and thickness for A356 aluminum quenched in water and a polymer quenchant
is shown in Fig. 53 [58,59].
Heat transfer rates decrease as the thickness of the polymer ¢lm increases, and
the polymer ¢lm thickness is dependent on both agitation and quenchant con-
centration. Agitation induced ¢lm breakage as a function of the polymer structure,
concentration, and bath temperature. Cooling curves as a function of polymer con-
centration are illustrated in Fig. 54 [51]. In general, the duration of the ¢lm boiling
region increases and cooling rates in the critical region decrease with increasing poly-
mer concentrations.
AMS Speci¢cations
The most common PAG quenchants used in the aerospace industry today are des-
ignated as ‘‘Type I’’ quenchants [24]. Type I quenchants are de¢ned by the physical
properties that they exhibit in aqueous solution. These physical properties are speci-
¢ed in AMS 3025A and are summarized in Table 12 [60].
There has been some discussion in the industry regarding the meaning of the
values in Table 12. Taken together, they do reasonably specify the composition
of the quenchant being evaluated. For example:
1. Viscosity, at constant water content, is indicative of the copolymer mol-
ecular weight (size).
2. Refractive index, while a very old characterization method, has tradition-
ally been related to the molar refractance values (structure) of chemical
compounds and their concentrations.
3. Speci¢c gravity, while not a critical parameter, is often used in chemical
engineering processes as an indicator of composition and concentration.
Figure 54 Cooling curves for 1 in. 7075 aluminum alloy plate quenched into different con-
centrations of a Type I polymer quenchant.
Water 45^48%
Speci¢c Gravity (20 C/68 F) 1.094 .005%
Refractive Index (20 C/68 F) 1.4140 0.005%
Viscosity (cS @100 F) 535 70
20% Dilution with water (cS @100 F) 5.5 0.5
Separation Temp. 165 F 5
2024-T6 0.010^0.249 47 60
2024-T6 0.063^0.249 49 62
2024-T6 0.250^0.499 49 62
7075-T73 0.250^0.499 63 72
7075-T73 < 3.0 56 66
7075-T73 3^4 55 64
7075-T73 4^5 53 62
7075-T6 0.750^1.000 65 75
7050 2.001^3.00 65 74
thermal stresses and the potential for increased distortion. Thermal gradients are
reduced by reducing the cooling rate and by increasing the duration of the ¢lm
boiling region up to, but not past, the ‘‘nose’’ of the C-curve. (This is why ‘‘hot’’
or boiling water is used.)
There is a cooling rate ‘‘window’’ that must be identi¢ed to obtain both optimal
physical properties and minimum residual stress and distortion. The position and
width of the window is a function of the speci¢c hardenability of the alloy and
the geometry of the part. This concept is illustrated by Fig. 56 which shows [63]:
1. Curve A is the maximum cooling rate for obtaining speci¢c structural
characteristics.
2. Curve B is the cooling rate beyond which the alloy undergoes plastic
deformation resulting in residual stresses.
3. Curve 1 does not introduce residual stresses but does not produce the des-
ired mechanical characteristics such as boiling water.
4. Curve 2 produces the desired mechanical properties but also produces
unacceptable residual stresses such as cold water.
5. Curve 3 is an optimized cooling process where the cooling rate is controlled
to optimize mechanical properties with minimum residual stresses.
[65], and 7075-T6 and T73 [65] have been reported and are illustrated in Fig. 57 [66].
The recommended concentration range for the Type I polymer quenchants varies
signi¢cantly with hardenability of the particular alloy.
The contour plot shown in Fig. 58 for the 2024-T851 model (0.063 in.) shows
that increasing polymer concentration has the expected effect of decreasing the
quench factor. Variations in quenchant velocity had no effect on quench factor
at this sheet thickness [67]. A similar study was performed on 7075-T73 aluminum
sheet except three sheet thicknesses were examined: 0.063, 0.126 and 0.25 in. Contour
plots for these quench factors are provided in Fig. 59 [67]. In this case, quenchant
velocity had an effect, especially as the sheet thickness increased.
The quenching data for 7075-T73 bar stock with diameters of 0.5, 1.0 and 1.5
in. were also modeled. Contour plots, holding bar diameter and bath temperature
constant, are shown in Fig. 60 [67]. These results show that agitation rate had
no signi¢cant effect on quench factor under these experimental conditions.
The regression equations developed from this work along with standard
deviations and R2 values are shown in Table 15. Since only one sheet thickness
of 2024 was evaluated, sheet thickness does not appear in the statistical model.
Thickness, agitation rate and bath temperature factors were modeled for both 7075
sheet and bar and these variables do appear in the statistical model. The statistical
¢t of the data to the model was better for the 7075 than for 2024 which is due
to the larger data set used.
T ¼ Temperature ( F)
st ¼ Sheet Thickness (in.)
D ¼ Bar Diameter (in.)
CR ¼ Agitation Rate (ft/min)
C ¼ Concentration (%)
Q ¼ Quench Factor
YS ¼ Yield Strength (ksi)
* ¼ Multiply
The initial quenchant solution is called the ‘‘feed solution’’. This solution is
passed through a pressurized membrane as illustrated in Fig. 64. The £uid that passes
through the membrane, called the ‘‘permeate’’, is typically pure water. The permeate
passes into the core of the membrane assembly where it is either released from the
system or delivered to a storage tank for further use. The concentrated solution
which does not pass through the membrane is either recycled through the membrane
assembly for further concentration or delivered to a storage tank for reuse.
Table 17 Relationship Between the Membrane Separation Method, System Pressures and
Size of Molecules Separated
Membrane Type Size of Solute Separated Pressure (psig)
The rate of permeate separation, QP , is equal to the rate of puri¢ed water pass-
ing through the membrane. This is usually expressed as volume/min at 25 C. The
£ow of the concentrate, QC , is equal to the £ow of the retained polymer. The £ow
rate of the feed stream of the incoming quenchant, QF , is equal to the permeate
rate plus the concentrate rate.
In membrane separation technology, the recovery rate is used to characterize
the separation system. Recovery rate (%) is de¢ned as:
CC ¼ Concentrate concentration,
CAVE ¼ Average concentration.
Cf þ Cc
Cave ¼
2
Cc
Passage G ¼
Cave
Cf
Retention ¼
Cave
Oil can be separated from the feed stream by coalescing technology which
permits the removal of the micron size oil droplets by coalescing them into larger
particles which are then separated by density differences. This process is illustrated
in Fig. 66 [73]. The primary driving force affecting oil separation by coalescence
is the excess free energy at the interface of the dispersed oil droplet caused by
unbalanced forces at the droplet surface. The relatively small interfacial tension
values are suf¢cient to permit oil coalescence in a contaminated quenchant solution.
Thus, the dispersed oil can be collected in a settling tank where it is separated from
the quenchant solution based on speci¢c gravity.
BLISTERING DUE TO LUBRICANT/QUENCHANT POLYMER CONTAMINATION. Instances
have been reported where residual polymer quenchants, die lubricants, and other
hydrocarbon materials are present on the surface of the aluminum during tempering.
This may lead to the formation of surface blisters and voids after quenching. This
effect may be observed metallographically by the presence of ‘‘water marks’’ on
AA7075 as illustrated in Fig. 67 [5]. Cleaning the parts with a caustic etch and nitric
acid accentuated the appearance of the blisters and produced a ‘‘smutty’’ residue in
the area of the blisters. Sectioning showed that the blisters and voids were present
to a depth of 0.050 in. with no indications of stringers, laps, etc.
Schuler reported that such blisters were due to high temperature oxidation of
the residual hydrocarbon material during solution heat treating which produced
hydrogen or water vapor which may have migrated into the grain boundaries.
Similarly, residual poly(alkylene glycol) polymer after quenching due to incomplete
rinsing may produce the same effect during tempering.
High temperature oxidation may be controlled or eliminated by more effective
precleaning or rinsing. A volatile £uoride atmosphere, such as that produced by
Magnesium
Magnesium Alloys
Zinc
Aluminum 2S
Cadmium
Aluminum 17ST
Steel or Iron
Cast Iron
Chromium^iron (active)
Ni^resist
18^8 Chromium^nickel^iron
18^8^3 Chromium^nickel^molybdenum^iron (active)
Lead^tin Solder
Lead
Tin
Nickel (active)
Iconel (active)
Hart alloy C (active)
Brass
Copper
Bronzes
Copper^nickel alloys
Monell
Silver Solder
Nickel (passive)
Iconel (passive)
Chromium (non-passive)
18^8 Chromium^nickel^iron (passive)
Hastelloy C (passive)
Silver
Graphite
Gold
Platinum
Protected end (Cathode)
Figure 70 Comparison of the cooling pro¢le of cold water, warm water, a single concen-
tration of a Type 1 polymer quenchant and carbonated water.
cathodic [88]. An aluminum alloy containing 4% copper in solid solution will exhibit
an electrochemical potential of 0.69 V. However, copper concentrations in grain
boundaries may reduce the electrochemical potential to -0.84 V making it more
anodic. Grain boundary corrosion may also occur when the grain boundary
precipitates are either more anodic than the adjacent solid solution (Mg2 Al3 ,
MgZn2 , and Alx -Znx Mg) or more cathodic (CuAl2 and Alx Cux Mg) [89].
The degree of intergranular corrosion may be controlled by selection of the
temper and maximizing the cooling rate permissible to still provide distortion con-
trol. For example, the T4 and T6 temper conditions are typically selected when
optimum resistance to intergranular corrosion is required [90]. Schuler reported that
the critical cooling rates (cooling rates between 750^550 F) for the 7xxx series to be
< 400 F/sec and 1000 F/sec for the 2xxx series for optimal resistance to
intergranular corrosion [90]. However, insuf¢cient quench rates are not the only
cause of intergranular corrosion. Other factors include transfer rate from the furnace
to the quench, air entrainment in the quench tank, and the ratio of section
mass/surface area [90]. The data in Table 20 show the effect of cooling rate on
increasing intergranular corrosion in AA7075 cylindrical bar [91]. The depth of
attack was consistently higher toward the center of quenched bars when the cooling
rate was slower.
A 53 Surface 0.46
Center 0.56
B 50 Surface 0.30
Center 0.86
C 30 Surface 0.46
Center 0.61
D 17 Surface 0.74
Center 1.09
a
SurfaceLwithin 3.2 mm of cylinder surface
CenterLwithin 3.2 mm of cylinder centerline.
20 106 . 500 ¼ 1:0%
The strains are at least ten times the yield strain, as illustrated in Fig. 74 [93], and
exceed the elastic limit which may lead to cracking during quenching.
Measured centerline quench rates for a 20 mm bar are illustrated in Fig. 75 [93].
The modulus is determined from its volume/surface area (area/circumference ratio)
and is determined to be 5 mm. From this estimation and Fig. 75, it is possible to
determine the cooling rate where distortion and cracking problems may occur.
Using the thermal properties from Table 21, which relate to aluminum at
approximately 250 C and steel at 500 C, the thermal diffusivity (d) of aluminum
is calculated. The diffusivity for different thicknesses (x) where heat can diffuse,
may be estimated from:
x ¼ ðdtÞ1=2
Figure 75 Cooling rate for a 5 mm modulus aluminum plate subjected to various quench
severities.
If x ¼ 10 mm, t ¼ 1 sec, the cooling rate upon cooling from 500 C to 250 C is:
DT 250
Cooling Rate ðCRÞ ¼ ¼ ¼ 250 K=sec
d 1
Using this process, the relationship between average diffusion distance at different
cooling rates may be determined as shown in Fig. 76.
If the following relationship is used [93]:
DT
t¼
CR
Figure 76 Rate of quench versus diffusion distance for heat during the critical time of the
quench showing the extent of safe and dangerous regimes for aluminum castings and test
bars. Area 1 was the regime for test bars quenched in water. Area 2 was quenched in
35% of a polymer quench.
Where the critical value of DDT for aluminum alloys is: 2.5 102 for aluminum
alloys and 2.5 103 for steel. Therefore, if the value for X or Q is suf¢cient to
meet the critical parameter, then there will be a high probability of quench stresses
in excess of the yield stress in the casting.
Table 22 Comparison of the Effectiveness of Various Cooling and Heating Media for
Uphill Quenching (AA7049 Aluminum Alloy)a
METHOD
Cooling Medium Heating Medium &T % Stress Relief
Table 23 Effect of Delay in Uphill Quenching from the Initial Quench on Stress Reduction
(AA7049 Aluminum Alloy)
Delay After Quench (hr) Measured Residual Stress (psi) Stress Reduction (%)
1 4000 83
3 7000 71
8 10000 58
24 14000 42
Figure 82 Cooling curves and temperature difference across a 76.3 mm diameter AA7075
probe quenched into 32 C water £owing at 0.25 mm/sec.
as a function of the center temperature (on the ordinate) [4]. It is observed that the
maximum temperature difference across the bar was approximately 110 C and
the maximum value occurred shortly after the start of quenching while the center
temperature was approximately 425 C.
Similar temperature-time histories and the temperature differences across the
probe when quenching in 60 C water and 20% Type I Polymer Quenchant £owing
at 0.25 m/sec past the probe are illustrated in Figs. 83 and 84 respectively. The data
in both cases are superimposed on the 32 C water data previously shown in Fig.
82. The higher water temperature of 60 C reduced the maximum temperature dif-
ference to 60 C and the 20% solution of Type I Polymer Quenchant reduced the
difference to a value of 69 C. The ¢lm coef¢cients associated with these quenchants
Figure 84 Cooling curves and temperature difference across a 76.3 mm diameter AA7075
probe quenched into water and a 20% solution of a Type 1 polymer quenchant solution
at 32 C £owing at 0.25 mm/sec.
were presented in Tables 10 and 11. The temperature difference across the section
decreased as the ¢lm coef¢cient decreased.
High ¢lm coef¢cients can produce even larger differences in temperature
between thick and thin sections of a part. Cooling curves associated with a 76.2 mm
section and a 12.7 mm section quenched in 32 C water £owing over the part at a
velocity of 0.25 m/sec are illustrated in Fig. 85. Water at this temperature and vel-
ocity had a ¢lm coef¢cient of about 4.78 W/cm2 K and produced a maximum tem-
perature difference between the two sections of approximately 290 C.
The thermal stress in a part, which causes distortion during quenching, is a
function of the alloy thermal expansion coef¢cient, elastic modulus and temperature
difference within the part. Minimizing the thermal stress requires that the tempera-
ture difference be minimized since no control can be exercised over either of the
physical properties.
The temperature differences across plates up to 76 mm thick were calculated
using a ¢nite difference heat transfer program in which the ¢lm coef¢cient was used
as an input value. The results are illustrated in Fig. 86 where the temperature dif-
ference is the maximum calculated value between the plate center and a location
1.60 mm beneath the surface. The temperature difference across a given section
thickness increased progressively as the ¢lm coef¢cients increased. In order to mini-
mize the temperature across a part to reduce the thermal stress, the ¢lm coef¢cient
must be minimized while cooling fast enough to guarantee the minimum yield
strength can be met. This can be done by selecting and using the most appropriate
quenchant and operating conditions.
Archambault et al. have suggested an alternative technique involving computer
control of quenchant spray heads aimed at different areas of a part [101]. This
approach can be used to control cooling rates and minimize thermal gradients.
Additional control can be exercised, as a function of time, on the heat transfer
coef¢cient by these means [4,102,103]. More precision in the calculated results
can undoubtedly be obtained using ¢lm coef¢cients that vary with the probe
temperature. Several investigators have shown how a functional relationship can
be established between ¢lm coef¢cient or heat £ux and the probe temperature
[104^107], but these methods were not used in the current study which assumed
a constant effective ¢lm coef¢cient.
Quenching real parts is usually more complicated than quenching sheets, bars
and plates because most real parts do not have a uniform cross-section. Many air-
craft structural members consist of £anges reinforced by thin web sections. When
such a part is quenched in water, the web section temperature drops far more quickly
than the temperature in the heavier £ange. The large temperature difference creates a
high thermal stress which often causes plastic deformation in the web. When the
heavy £ange cools, it contracts onto the thin web and often causes buckling or
2.7.2 Racking
One of the major causes of distortion is non-uniform heat removal from the parts
being quenched. To minimize distortion, the placement of the parts, commonly
known as ‘‘racking’’, in the quench tray is critical. The most important factors
to be considered in this regard are [108^111].
1. Part Spacing.
2. Part Con¢guration.
3. Agitation.
4. Immersion Rate.
5. Thickness Variation within the Part.
6. Quench Medium.
7. Part SpacingLPerhaps the most important consideration is part spacing.
It is essential that suf¢cient space be provided around the part to optimize
quenchantLsurface area contact. This enhances heat extraction from the
hot surface while minimizing the formation of hot spots or localized tem-
perature increases within the quenchant due to poor £uid £ow (agitation)
[109].
8. To achieve optimal £ow, parts must be properly ‘‘racked’’ with the use of
‘‘¢xtures’’ [97]. Fixtures may be a basket or a rack with places to hang or
place small parts so that they will not move when immersed in the
quenchant. Larger parts, although relatively heavy, must be racked prop-
erly to assure uniform heat removal during the quench. Such parts should
not be indiscriminately dumped into a basket and quenched. Instead, the
parts must be placed in the tank so that adequate £uid £ow around all of
the surfaces is assured.
9. The amount of space between the parts must be increased with increasing
mass. For water quenching, the distance between part surfaces must
increase with with higher quenchant temperatures. Water temperatures
greater than 160 F should not be used for larger cross-sections [110].
10. Part Con¢guration ^ Croucher’s rule of thumb is to place parts in a bas-
ket so that they will offer least resistance to £uid £ow [111].
11. AgitationLFigure 87 shows that the directional placement of a complex
part in the quenchant is often important if distortion and cracking
are to be prevented. A simple analysis is often suf¢cient to assure that
reasonable £uid £ow around the part is obtained. For example, situations
where the part would be placed to block £uid £ow may create hot spots
leading to more distortion [110]. An illustration of such a part is provided
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