Materials and Design 32 (2011) 38183822

Contents lists available at ScienceDirect

Materials and Design

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

Investigation of quench sensitivity and transformation kinetics during isothermal treatment in 6082 aluminum alloy
B.C. Shang a, Z.M. Yin a,, G. Wang a, B. Liu a, Z.Q. Huang a,b
a b

School of Materials Science and Engineering, Central South University, Changsha 410083, China Foshan Sanshui Fenglv Aluminium Co. Ltd., Foshan 528133, China

a r t i c l e

i n f o

a b s t r a c t
The quench sensitivity of 6082 aluminum alloy was investigated by timetemperatureproperty (TTP) curves. The sensitive temperature of quenching ranges from 250 C to 440 C in 6082 Al-alloy, and the nose temperature is about 360 C. During isothermal treatment process, the Mg2Si particles precipitate from the supersaturated solid solution, and the precipitation rate is the highest at the nose temperature. A number of rod-shaped b0 and b particles precipitate in the early stage of isothermal treatment at 360 C. Prolonging the holding time leads to more and coarser b particles in the matrix. Both the precipitation of b0 and b particles results in loss of solute and decreasing of the subsequent age hardening effect. Also, the important coefcients k2k5 and critical cooling rate for 6082 Al-alloy are identied, and the properties after different rates of cooling were predicted using quench factor analysis. 2011 Elsevier Ltd. All rights reserved.

Article history: Received 11 November 2010 Accepted 8 March 2011 Available online 17 March 2011 Keywords: C. Heat treatment F. Microstructure H. Value analysis

1. Introduction 6000 series alloys are widely used because of their benets such as medium strength, formability, weldability, corrosion resistance and low cost. And these AlMgSi alloys are mostly used in extruded aluminum products in Western Europe, as well as for construction and automotive purposes [1,2]. For the heat treatable alloys which can be heat treated to produce precipitation to various degrees, such as 6082 alloy, a proper process of heat treatment is important. When the alloy is given a solution heat treatment and then quenched to a temperature lower or equal to room temperature, it will be supersaturated with respect to the dissolved elements. Consequently, a precipitation reaction occurs during slow cooling. As mentioned above, a rapid quench from the solution heat treatment temperature is required to achieve optimal mechanical properties. But in industrial production, the quench rates should be controlled at a low level to reduce the residual stress and warping. An ideal quench will minimize residual stresses while maximizing the mechanical properties of the alloy. To achieve these, the quench sensitivity of heat treatable alloys should be studied carefully. Timetemperature-property (TTP) and timetemperature transformation (TTT) curves are both effective approach to evaluate quench sensitivity. Much work about quench sensitivity of aluminum alloys has been done in the present investigation. Dolan et al. [3,4] investigated the quench sensitivity of some typical alloys using TTP curves which were obtained by an interrupted quench tech Corresponding author. Tel./fax: +86 731 88830262.
E-mail addresses: shangbaochuan@163.com (B.C. Shang), zmyin@163.com, yin-grp@csu.edu.cn (Z.M. Yin). 0261-3069/$ - see front matter 2011 Elsevier Ltd. All rights reserved. doi:10.1016/j.matdes.2011.03.016

nique, the coefcients k2k5 for three kinds of alloys are identied. Liu et al. [57] mainly investigated the quench sensitivity of high strength AlZnMgCu alloys by TTP diagrams, and the inuence of quenching rate on the drop in the properties was studied by quench factor analysis method. And also many properties of alloy, such as hardness, strength, fracture toughness and corrosion resistance, were investigated using quench factor analysis method [810]. It is generally accepted that the TTP curves can be described mathematically as tc(T) shown in Eq. (1). tc(T) function with the following form is used to determine the incubation time for alloy of interest [11].

" tc T k1 k2 exp

k3 k4 RT k4 T 2

  k5 exp RT

where tc(T) is the critical time for precipitation of a constant amount of solute, k1 is the natural logarithm of the untransformed fraction during quenching, k2 is the constant related to the reciprocal of the number of nucleation sites, k3 is the constant related to the energy required to form a nucleus, k4 is the constant related to the solvus temperature, k5 is the constant related to the activation energy for diffusion, R is the universal gas constant, and T is the absolute temperature (K). With TTP curves, the effect of quenching rate on properties can be predicted by quench factor analysis method. Quench factors can be calculated according to the equation [11]:

tf t0

1 dt t c T

B.C. Shang et al. / Materials and Design 32 (2011) 38183822

3819

where s is the quench factor, tc(T) is the critical time as a function of temperature, t0 and tf are the upper and lower temperature of the quench sensitive temperature zone. The mechanical properties of the alloy can then be predicted from the quench factor using:

r rmax expk1 s

where r is the predicted property, rmax is the maximum property that can be attained after a fast quench. However, little quantitative data has been published to study the quench sensitivity of 6000 series alloys. In this paper, the TTP curves of 6082 aluminum alloy were obtained by an interrupted quench technique, the important constants k2k5 and critical temperature region for 6082 Al-alloy were identied, quench sensitivity was investigated and analyzed in view of the transformation kinetics. 2. Experimental The 6082 aluminum alloys were supplied by Foshan Sanshui Fenglv Aluminium Co. Ltd. in the form of as-extruded bars with a diameter of 16 mm, and the chemical composition is given in Table 1. Some disc samples of U16 mm 6 mm were cut down along the extruding direction. All the samples were given a solution treatment at 545 C for 50 min, then immediately transferred to a salt bath and held isothermally at temperatures ranging from 300 to 440 C for set periods of time, subsequent quenching was done in water at room temperature, nally aged at 170 C for 8 h. The differential scanning calorimetry (DSC) analyses were carried out in a puried argon atmosphere using Netzsch STA 449C instrument. Three millimeter diameter disc samples with mass about 15 mg cut down from the extruded bars were heated to 545 C at a rate of 40 K/min, held for 50 min, and cooled to room temperature with the scanning rate of 10 K/min. Hardness measurement after aging was performed on HBE3000 Brinell hardmeter, and three hardness data were taken for each sample while the average value was used. Microstructures of the specimens were examined with a transmission electron microscope (TEM), TECNAIG2 20, operated at 200 kV. The TEM specimens were prepared by cutting a small piece from the samples, mechanically grinding to about 80 lm thickness and then jet polishing in 30% HNO3 and 70% CH3OH at 25 C. 3. Results and discussion 3.1. The TTT curves of 6082 alloy The information of chemical composition and heat-treatment of 6082 aluminum alloy was inputted to the JMatPro 5.1 which is produced by the Sente Software Ltd., the TTT curves were created shown in Fig. 1. The nose temperature of b00 and b0 phases is about 350 C, while the nose temperature of the b phase is higher. 3.2. The DSC experiment The DSC curve during the cooling (Fig. 2) reveals the presence of two exothermic peaks A and B with a maximum situated at 350 C and 490 C, respectively. According to the related research [12,13] and the TTT curves of 6082 alloy created by JMatPro 5.1 (Fig. 1), the

Fig. 1. TTT curves of 6082 alloy created by the JMatPro 5.1.

Exo
DSC
w/mg

200

10
250

300

350

400

450

500

Temperature / C
Fig. 2. DSC curve of 6082 at cooling rate of 10 K/min after solution treatment.

high temperature peak (B) is ascribed to the precipitation of b phase, and the low temperature peak (A) is attributed to the precipitation of b00 and b0 phases. Because the precipitation of b phase needs more time and higher temperature, the quench sensitivity at 490 C is much lower than 350 C. The research in this paper is mainly about the peak A at the temperature from 300 to 440 C. The precipitate rate of b00 and b0 phases reaches the maximum value at about 350 C, consequently, the nose temperature of TTP curves of 6082 alloy should be about 350 C.

3.3. TTP curves of 6082 alloy Fig. 3 represents the inuence of isothermal treatment on mechanical properties of 6082 Al-alloy. Isothermal holding leads to decrease of hardness, the changes can be grouped under two situations: at moderate temperature, such as 340 C, its hardness drops rapidly to HB 45 within 200 s and then roughly maintains

Table 1 Composition analysis of experimental alloy (wt%). Mg 0.600.80 Si 0.851.15 Fe 0.40 Cu 0.10 Mn 0.400.60 Cr 0.10 Ti 0.05 Zn 0.10 Al Bal.

3820

B.C. Shang et al. / Materials and Design 32 (2011) 38183822 Table 2 Coefcients of TTP curve for aluminum alloy 6082 by tting. k2 3.2E9 k3 (J mol1) 2422 k4 (K) 896 k5 (J mol1) 103,683

100 90 80 70

440 410 380 360 340 320 300

550 500

HB

60 50 40 30 0 100 200 300 400 500 600 700 800 900

Temperature / C

450 400 350 300 250 200 -1 10 10

0

Fitted
99.5% 95% 90% 80% 70%

Measured
95% 90% 80% 70%

Time / s
Fig. 3. The curves of inuence of holding time at different temperature on hardness.

stable; at lower and higher temperature, such as 300 C and 440 C, the hardness declines in a much slower rate with time. Take the hardness of peak-aging condition (T6) as 0 transformation of Mg2Si. Choose the 70% of the hardness to be tted by Eq. (1). Using the iterative non-linear tting procedure of the Origin 7.5 software, the tted curve and k2k5 constants can be determined shown in Fig. 4 and Table 2. And the Table 2 enables the k2k5 constants to be varied to minimize the mist between the predicted and measured hardness values. The values in Table 2 were substituted in tc(T) function (Eq. (1)) and TTP curves were shown in Fig. 5. Fig. 5 compares the experimental and tted TTP curves for 6082 aluminum alloy, the gure shows clearly that there is a good agreement between them. The TTP curves of 6082 alloy are C shape, and the nose of C curves is at about 360 C. It is consistent with the results of Figs. 1 and 2. According to the location of the TTP curve of 99.5% of the highest property shown in Fig. 5, when the transformation time is 10 s, the critical temperature range is determined. The high quench sensitivity temperature zone is 250440 C, and in this zone the incubation period is short. With TTP curves, the effect of quenching rate on properties can be predicted by quench factor analysis method which is shown in the section 1. In order to attain accurate predicted results, the time

10

10

10

10

10

Time / s
Fig. 5. TTP curves of aluminum alloy 6082.

step interval should be selected so that an average drop in the critical temperature range is less than 25 C [6,11], so Dt = 0.3 s is used, the range of 250440 C is considered, and k1 = ln(0.995) is used. The inuence of average quenching rates from 0.5 to 100 C/s through the temperature range of 250440 C was investigated, and the results calculated according to the Eqs. (2) and (3) were shown in Fig. 6. From Fig. 6, it can be seen that the greater the cooling rate, the bigger the hardness, and the smaller the quench factor. With quenching rate higher than a certain rate Qc, the hardness increases slowly, while below the rate Qc, the hardness increases rapidly with increase in the quenching rate. According to Fig. 6, the rate Qc is estimated as about 15 C/s. When the quenching rate is more than 15 C/s, the hardness of the alloy reaches more than 95% of the maximum property. During the quenching, at intermediate temperatures, where the cooling rate has a signicant impact on the mechanical properties of the alloy, the cooling rate should be high (more than 15 C/s) to

550 500

200

100 90 80 70
HB

70% measured 70% fitted

180 160 140 120 100 80 60 40 20 0 0.1

Temperature / C

400 350 300 250

Quench factor

450

HB

60 50 40

10

10

10

10

10

30 100

Cooling rate (C /s)

Fig. 6. Effect of average cooling rate on quench factor and predicted hardness of alloy.

Time / s
Fig. 4. The TTP curve for the 70% of highest property by measured and tting.

B.C. Shang et al. / Materials and Design 32 (2011) 38183822

3821

ensure a supersaturated solid solution is retained, while at higher and lower temperatures, decreasing the cooling rate is helpful to relieve the effect of residual stress. 3.4. TEM microstructure observation Fig. 7 is TEM micrographs of the 6082 Al-alloy after holding for different times at 360 C and then quenched. After solution treatment there are many irregular and polygonal particles, by the analyzing of the X-ray Energy Dispersive Spectroscopy (XEDS), the particles mainly contain Mn, Si and Fe (Fig. 7a). After 120 s of isothermal treatment, a number of rod-shaped b0 and b particles with several hundred nanometers in length appear. The rod-shaped particles precipitate along the [0 1 0] and [1 0 0] directions in the Al matrix (Fig. 7b). In the 48 h isothermal treated specimen, the rod-shaped particles have grown up, formed the coarse plate-like b phases (Fig. 7c). 3.5. General Avrami kinetics The kinetics of phase transformations, including diffusion-controlled precipitation, are frequently well described by the Avrami equation w = 1 exp( ktn), where w is the volume fraction transformed at time t, k is the Avrami constant depending on the nucleation rate and the growth rate and very sensitive to temperature, n is the Avrami exponent which is dependent on the nucleation mechanism [14]. The volume fraction transformed w at the time t can be got from the TTP curves (the points in Fig. 8), these points are tted by the Avrami equation using the iterative non-linear tting procedure of

the Origin 7.5 software. Fig. 8 illustrates the time-dependent relative crystallinity function w(t) for three different crystallization temperatures ranging from 300 to 440 C. The most reliable results for the Avrami parameters are shown in Table 3. It is reported that rapid transformations are associated with large values of k [15]. The result k(360 C) > k(300 C) > k(440 C) shows that, the isothermal transformation at 360 C is fastest, and the isothermal transformation at 300 C is slower than 360 C, but faster than 440 C, the isothermal transformation at 440 C is slowest. In other words, at moderate temperature zone about 360 C, the transformation needs short time, and the alloy has very high quench sensitivity, while the quench sensitivity at low temperature and high temperature is lower than the moderate temperature. For diffusion-controlled growth transformation, when n = 0.5, it means thickening of very large plates, and when n = 1, it means thickening of long cylinders or needles [14,16]. And the precipitation sequence of AlMgSi alloys during aging is generally accepted: supersaturated solid solution ? atomic clusters ? spherical GP zones ? needle like metastable b00 phase ? rod like metastable b0 phase ? platelets of equilibrium b phase (Mg2Si) [17,18]. For 6082 aluminum alloy, the n value got by tting is about 1, the phase transformation of 6082 alloy is mainly the thickening of rods or needles during the isothermal holding process. In other words, it is mainly the process of forming of b00 and b0 phases, and only at last it becomes the thickening of plate-like b phase. These processes can be seen in the TEM micrographs (Fig. 7). The nose of C curves of 6082 Al-alloy has the fastest rate of precipitation, both the high phase transformation driving force and the high diffusion rate of solute atoms lead to the primary

(a)

(b)

[010]Al

[100]Al

(c)

Fig. 7. TEM micrographs of the 6082 Al-alloy after holding for different times at 360 C: (a) 0 s, (b) 120 s, (c) 48 h.

3822

B.C. Shang et al. / Materials and Design 32 (2011) 38183822

500
1.0

450

Temperature / C

0.8

400 350 300

360
95% 90% 80% 70%

300

440

inhibits the precipitate of strengthening phase b00 in subsequent aging. It was possible to slowly cool the alloys from the solution heat treatment temperature to temperatures above the critical temperature region and then enhance quench rate to more than 15 C/s at the moderate temperature zone (250440 C) to get optimal mechanical properties. Acknowledgement

0.6 0.4 0.2

This work was funded by the State Key Fundamental Research Program of China (Grant No. 2009A080205001). References
[1] Marioara CD, Andersen SJ, Jansen J, Zandbergen HW. The inuence of temperature and storage time at RT on nucleation of the b00 phase in a 6082 AlMgSi alloy. Acta Mater 2003;51:78996. [2] Jin Man, Li Jing, Shao Guang Jie. The effects of Cu addition on the microstructure and thermal stability of an AlMgSi alloy. J Alloys Compd 2007;437:14650. [3] Dolan GP, Flynn RJ, Tanner DA. Quench factor analysis of Aluminum alloys using the Jominy end quench technique. Mater Sci Technol 2005;21:68792. [4] Dolan GP, Robinson JS. Residual stress reduction in 7175-T73, 6061-T6 and 2017A-T4 aluminum alloys using quench factor analysis. J Mater Process Technol 2004;153154:34651. [5] Liu Shengdan, Zhang Xinming, You Jianghai, Huang Zhenbao, Zhang Chong, Zhang Xiaoyan. TTP curve of 7055 aluminum alloy and its application. Trans Nonferrous Met Soc China 2006;16:20349. [6] Liu Shengdan, Zhong Qimin, Zhang Yong, Liu Wenjun, Zhang Xinming, Deng Yunlai. Investigation of quench sensitivity of high strength AlZnMgCu alloys by timetemperatureproperties diagrams. Mater Des 2010;31:311620. [7] Zhang Xinming, Liu Wenjun, Liu Shengdan, Yuan Yubao, Deng Yunlai. TTP curve of 7050 aluminum alloy. Trans Nonferrous Met Soc China 2009;19:8618. [8] Staley JT. Quench factor analysis of aluminum alloys. Mater Sci Technol 1987;3(11):92335. [9] Robinson JS, Cudd RL, Tanner DA, Dolan GP. Quench sensitivity and tensile property in homogeneity in 7010 forgings. J Mater Process Technol 2001;119:2617. [10] Rometsch PA, Starink MJ, Gregson PJ. Improvements in quench factor modeling. Mater Sci Eng A 2003;339:25564. [11] Totten GE, MacKenzie DS. Handbook of aluminum. Physical metallurgy and processes, vol. 1. New York: Marcel Dekker; 2003. p. 10018. [12] Benjamin Milkereit, Olaf Kessler, Christoph Schick. Recording of continuous cooling precipitation diagrams of aluminum alloys. Thermochim Acta 2009;492:738. [13] Bratland DH, Grong O, Shercliff H, Myhr OR, Tjotta S. Overview No. 124 modelling of precipitation reactions in industrial processing. Acta Mater 1997;45:122. [14] Ziqiao Zheng. Materials science and engineering. Changsha: Central South University Press; 2005. p. 400401. [15] Porter DA, Easterling KE. Phase transformations in metals and alloys. London: Chapman & Hall Press; 1992. p. 263381. [16] Christian JW. The theory of transformations in metals and alloys, PART I. Oxford: Pergamon Press; 2002. p. 546. [17] Marioara CD, Andersen SJ, Jansen J, Zandbergen HW. The inuence of temperature and storage time at RT on nucleation of the b00 phase in a 6082 AlMgSi alloy. Acta Mater 2003;51:78996. [18] Vedani M, Angella G, Bassani P, Ripamonti D, Tuissi A. DSC analysis of strengthening precipitates in ultrane AlMgSi alloys. J Therm Anal Calorim 2007;87:27784.

250
0.0

200 -1 10

10

10

10

10

10

10

Time / s
Fig. 8. The curves of TTP and the time-dependent relative crystallinity function w(t).

Table 3 k and n value at different temperature through tting. Temperature (C) k n 300 0.00217 1.00207 360 0.00413 0.99937 440 0.00041 0.99792

precipitating of Mg2Si particles. The large particles do not have much effect in improving the strength of the alloy, what is worse, both the precipitation of b0 and b particles lead to a low level concentration of solute elements, and inhibit the precipitate of strengthening phase b00 in aging, resulting in decreasing of subsequent aging hardening effect. These are consistent with the results of hardness tests and the TEM micrographs. 4. Conclusions The TTP curves have been constructed for 6082 Al-alloy. Using the TTP curves, the critical temperature range and the important coefcients k2k5 and critical cooling rate for 6082 alloy are identied, and the curves got by JMatPro 5.1 and DSC experiments are well matched with the data got from the TTP curves, they are also good methods to investigate the quench sensitivity of aluminum alloys. During the isothermal holding of 6082 Al-alloy, the Mg2Si particles precipitate from supersaturated solid solution, and the transformation rate is fastest at about 360 C. The number of Mg2Si particles increases and the size becomes larger, it leads to a low level concentration of solute elements, and at the same time it also